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Sample records for esi-ms applications dans

  1. Contribution to the development of new analytical methods by the coupling between capillary electrophoresis and mass spectrometry (ICP-MS and ESI-MS): applications to the nuclear and biological fields; Contribution au developpement de nouvelles methodes analytiques par le couplage entre l'electrophorese capillaire et la spectrometrie de masse (ICP-MS et ESI-MS): applications dans les domaines nucleaires et biologiques

    Energy Technology Data Exchange (ETDEWEB)

    Pitois, A

    2006-04-15

    The coupling between chromatographic and electrophoretic separation techniques and mass spectrometry is used to combine the efficiency of the separation technique to the selectivity and sensitivity of the detectors. In this work, the number of applications of the CE-MS couplings has been increased. New analytical methods have been set up in the nuclear and biological fields. New analytical methods for the determination of fission products (cesium and lanthanides) have been developed by CE-ICP-MS. They enable to determine both concentration and isotopic composition of the fission products for very low detection limits (ng/mL by CE-Q-ICPMS, pg/mL by CE-HR-ICP-MS), since all the isobaric interferences are resolved. Moreover, only some nano-liters of sample are necessary to perform the analysis. These method have been applied with success to a simulated sample of spent fuel, to a nuclear sample from PUREX process and to a leaching of MOX fuel. Then, lanthanides have been analysed by CE-ESI-MS and the capability of ESI-MS to provide structural information has been studied. Elementary information has been obtained for strong potentials. Structural information has been obtained for low potentials. Finally, a new analytical method by CE-ESI-MS for the determination of 10B-boronophenylalanine (10B-BPA) has been developed for Boron Neutron Capture Therapy (BNCT). It has been applied to the cellular lines F98 and HUVEC. This CE-ESI-MS method has been validated by HR-ICP-MS. It enables a direct quantification of the chemical form 10B-BPA in samples of limited size (some nano-liters) and for low concentrations (ng/mL). As a consequence, this CE-ESI-MS method has enabled the study of the kinetics of 10B-BPA release and uptake for the F98 cells. (author)

  2. Application of LC-ESI-MS-MS for detection of synthetic adulterants in herbal remedies.

    Science.gov (United States)

    Bogusz, Maciej J; Hassan, Huda; Al-Enazi, Eid; Ibrahim, Zuhour; Al-Tufail, Mohammed

    2006-05-03

    Adulteration of allegedly "natural herbal medicines" with undeclared synthetic drugs is a common and dangerous phenomenon of alternative medicine. The purpose of the study was to develop a procedure for detection of most common synthetic adulterants in herbal remedies, using high-pressure liquid chromatography-electrospray tandem mass spectrometry (LC-ESI-MS-MS). Eighty drugs belonging to various pharmacological classes were included in the study. For most drugs two transitions were monitored, using protonated or deprotonated molecules as precursor ions. The drugs were isolated from herbal remedies using simple methanol extraction. Chromatographic separation was done in gradient of acetonitrile-10 mM ammonium formate buffer (pH 3.0). Drugs tested were grouped in suites, comprising analgesic drugs, antibiotics, antidiabetic drugs, antiepileptic drugs, aphrodisiacs, hormones and anabolic drugs, psychotropic drugs, and weight reducing compounds. These suites were used according to the declared benefits of examined preparations. Limits of detection ranged from 5 pg to 1 ng per injected sample. Drug-free herbal remedy spiked with eight various pharmaceuticals occurring in adulterated herbal preparations was used for internal proficiency testing. The recoveries of spiked drugs ranged from 63 to 100%. The procedure was applied in everyday casework. Several undeclared drugs were identified in "herbal" remedies, like e.g. sildenafil, tadalafil, testosterone, or glibenclamide. Pharmacological properties of detected drugs always corresponded with the claims of the "natural" remedies. The method presents a valuable extension of standard GC-MS screening used for this purpose.

  3. Establish an automated flow injection ESI-MS method for the screening of fragment based libraries: Application to Hsp90.

    Science.gov (United States)

    Riccardi Sirtori, Federico; Caronni, Dannica; Colombo, Maristella; Dalvit, Claudio; Paolucci, Mauro; Regazzoni, Luca; Visco, Carlo; Fogliatto, Gianpaolo

    2015-08-30

    ESI-MS is a well established technique for the study of biopolymers (nucleic acids, proteins) and their non covalent adducts, due to its capacity to detect ligand-target complexes in the gas phase and allows inference of ligand-target binding in solution. In this article we used this approach to investigate the interaction of ligands to the Heat Shock Protein 90 (Hsp90). This enzyme is a molecular chaperone involved in the folding and maturation of several proteins which has been subjected in the last years to intensive drug discovery efforts due to its key role in cancer. In particular, reference compounds, with a broad range of dissociation constants from 40pM to 100μM, were tested to assess the reliability of ESI-MS for the study of protein-ligand complexes. A good agreement was found between the values measured with a fluorescence polarization displacement assay and those determined by mass spectrometry. After this validation step we describe the setup of a medium throughput screening method, based on ESI-MS, suitable to explore interactions of therapeutic relevance biopolymers with chemical libraries. Our approach is based on an automated flow injection ESI-MS method (AFI-MS) and has been applied to screen the Nerviano Medical Sciences proprietary fragment library of about 2000 fragments against Hsp90. In order to discard false positive hits and to discriminate those of them interacting with the N-terminal ATP binding site, competition experiments were performed using a reference inhibitor. Gratifyingly, this group of hits matches with the ligands previously identified by NMR FAXS techniques and confirmed by X-ray co-crystallization experiments. These results support the use of AFI-MS for the screening of medium size libraries, including libraries of small molecules with low affinity typically used in fragment based drug discovery. AFI-MS is a valid alternative to other techniques with the additional opportunities to identify compounds interacting with

  4. Electro-spray ionization - mass spectrometry (ESI/MS) and molecular modelling, two complementary approaches. Application to calixarenes; Electrospray - spectrometrie de masse (ESI/MS) et modelisation moleculaire, deux approches complementaires. Application aux calixarenes

    Energy Technology Data Exchange (ETDEWEB)

    Allain, F.; Virelizier, H.; Moulin, Ch. [CEA Saclay, Dept. des Procedes d' Enrichissement, 91 - Gif-sur-Yvette (France); Lamare, V.; Dozol, J.F. [CEA Cadarache, Dept. d' Entreposage et de Stockage des Dechets, 13 - Saint-Paul-lez-Durance (France)

    2001-07-01

    The molecular dynamics simulation and the experimental results obtained by the ESI/MS technique have shown that the stability of the calixarene - alkaline cation complexes is dependent of the medium. Indeed, in solution, the calixarene presents a strong affinity for cesium whereas in gaseous phase, the strong affinity is for sodium. The stability of the [calixarene+Na]{sup +} complexes depends of the nature of the medium too; these two techniques having shown that the presence of a small quantity of water in the dilution solvent stabilizes the complex. At last, calixarenes with benzo groups on their crown have an affinity for sodium which is weak in solution but strong in gaseous phase. These different results show the excellent complementarity between the two techniques. (O.M.)

  5. Electro-spray ionization - mass spectrometry (ESI/MS) and molecular modelling, two complementary approaches. Application to calixarenes

    International Nuclear Information System (INIS)

    Allain, F.; Virelizier, H.; Moulin, Ch.; Lamare, V.; Dozol, J.F.

    2001-01-01

    The molecular dynamics simulation and the experimental results obtained by the ESI/MS technique have shown that the stability of the calixarene - alkaline cation complexes is dependent of the medium. Indeed, in solution, the calixarene presents a strong affinity for cesium whereas in gaseous phase, the strong affinity is for sodium. The stability of the [calixarene+Na] + complexes depends of the nature of the medium too; these two techniques having shown that the presence of a small quantity of water in the dilution solvent stabilizes the complex. At last, calixarenes with benzo groups on their crown have an affinity for sodium which is weak in solution but strong in gaseous phase. These different results show the excellent complementarity between the two techniques. (O.M.)

  6. Measurement of caffeine and its three primary metabolites in human plasma by HPLC-ESI-MS/MS and clinical application.

    Science.gov (United States)

    Chen, Feng; Hu, Zhe-Yi; Parker, Robert B; Laizure, S Casey

    2017-06-01

    Caffeine is a mild stimulant with significant potential for abuse, being consumed in larger doses with the widespread availability of energy drinks and by novel routes of administration such as inspired powder, oral sprays and electronic cigarettes. How these recent changes in caffeine consumption affecting caffeine disposition and abuse potential is of growing concern. In the study of caffeine disposition in humans, it is common to only measure the caffeine concentration; however, caffeine's three major metabolites (paraxanthine, theobromine and theophylline) retain central nervous system stimulant activity that may contribute to the overall pharmacological activity and toxicity. Therefore, it would be scientifically more rigorous to measure caffeine and its major metabolites in the evaluation of caffeine disposition in human subjects. Herein, we report a method for the simultaneous quantification of caffeine and its three major metabolites in human plasma by high-performance liquid chromatography coupled to electrospray tandem mass spectrometry (HPLC-ESI-MS/MS). Human plasma samples were treated by simple protein precipitation and the analytes were separated using a 6 min gradient program. Precision and accuracy were well within in the 15% acceptance range. The simple sample preparation, short runtime, sensitivity and the inclusion of caffeine's major metabolites make this assay methodology optimal for the study of caffeine's pharmacokinetics and pharmacodynamics in human subjects. Copyright © 2016 John Wiley & Sons, Ltd.

  7. An UPLC-ESI-MS/MS Assay Using 6-Aminoquinolyl-N-Hydroxysuccinimidyl Carbamate Derivatization for Targeted Amino Acid Analysis: Application to Screening of Arabidopsis thaliana Mutants.

    Science.gov (United States)

    Salazar, Carolina; Armenta, Jenny M; Shulaev, Vladimir

    2012-07-06

    In spite of the large arsenal of methodologies developed for amino acid assessment in complex matrices, their implementation in metabolomics studies involving wide-ranging mutant screening is hampered by their lack of high-throughput, sensitivity, reproducibility, and/or wide dynamic range. In response to the challenge of developing amino acid analysis methods that satisfy the criteria required for metabolomic studies, improved reverse-phase high-performance liquid chromatography-mass spectrometry (RPHPLC-MS) methods have been recently reported for large-scale screening of metabolic phenotypes. However, these methods focus on the direct analysis of underivatized amino acids and, therefore, problems associated with insufficient retention and resolution are observed due to the hydrophilic nature of amino acids. It is well known that derivatization methods render amino acids more amenable for reverse phase chromatographic analysis by introducing highly-hydrophobic tags in their carboxylic acid or amino functional group. Therefore, an analytical platform that combines the 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC) pre-column derivatization method with ultra performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-ESI-MS/MS) is presented in this article. For numerous reasons typical amino acid derivatization methods would be inadequate for large scale metabolic projects. However, AQC derivatization is a simple, rapid and reproducible way of obtaining stable amino acid adducts amenable for UPLC-ESI-MS/MS and the applicability of the method for high-throughput metabolomic analysis in Arabidopsis thaliana is demonstrated in this study. Overall, the major advantages offered by this amino acid analysis method include high-throughput, enhanced sensitivity and selectivity; characteristics that showcase its utility for the rapid screening of the preselected plant metabolites without compromising the quality of the metabolic data. The

  8. An UPLC-ESI-MS/MS Assay Using 6-Aminoquinolyl-N-Hydroxysuccinimidyl Carbamate Derivatization for Targeted Amino Acid Analysis: Application to Screening of Arabidopsis thaliana Mutants

    Directory of Open Access Journals (Sweden)

    Carolina Salazar

    2012-07-01

    Full Text Available In spite of the large arsenal of methodologies developed for amino acid assessment in complex matrices, their implementation in metabolomics studies involving wide-ranging mutant screening is hampered by their lack of high-throughput, sensitivity, reproducibility, and/or wide dynamic range. In response to the challenge of developing amino acid analysis methods that satisfy the criteria required for metabolomic studies, improved reverse-phase high-performance liquid chromatography-mass spectrometry (RPHPLC-MS methods have been recently reported for large-scale screening of metabolic phenotypes. However, these methods focus on the direct analysis of underivatized amino acids and, therefore, problems associated with insufficient retention and resolution are observed due to the hydrophilic nature of amino acids. It is well known that derivatization methods render amino acids more amenable for reverse phase chromatographic analysis by introducing highly-hydrophobic tags in their carboxylic acid or amino functional group. Therefore, an analytical platform that combines the 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC pre-column derivatization method with ultra performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-ESI-MS/MS is presented in this article. For numerous reasons typical amino acid derivatization methods would be inadequate for large scale metabolic projects. However, AQC derivatization is a simple, rapid and reproducible way of obtaining stable amino acid adducts amenable for UPLC-ESI-MS/MS and the applicability of the method for high-throughput metabolomic analysis in Arabidopsis thaliana is demonstrated in this study. Overall, the major advantages offered by this amino acid analysis method include high-throughput, enhanced sensitivity and selectivity; characteristics that showcase its utility for the rapid screening of the preselected plant metabolites without compromising the quality of the

  9. Contribution to the development of new analytical methods by the coupling between capillary electrophoresis and mass spectrometry (ICP-MS and ESI-MS): applications to the nuclear and biological fields

    International Nuclear Information System (INIS)

    Pitois, A.

    2006-04-01

    The coupling between chromatographic and electrophoretic separation techniques and mass spectrometry is used to combine the efficiency of the separation technique to the selectivity and sensitivity of the detectors. In this work, the number of applications of the CE-MS couplings has been increased. New analytical methods have been set up in the nuclear and biological fields. New analytical methods for the determination of fission products (cesium and lanthanides) have been developed by CE-ICP-MS. They enable to determine both concentration and isotopic composition of the fission products for very low detection limits (ng/mL by CE-Q-ICPMS, pg/mL by CE-HR-ICP-MS), since all the isobaric interferences are resolved. Moreover, only some nano-liters of sample are necessary to perform the analysis. These method have been applied with success to a simulated sample of spent fuel, to a nuclear sample from PUREX process and to a leaching of MOX fuel. Then, lanthanides have been analysed by CE-ESI-MS and the capability of ESI-MS to provide structural information has been studied. Elementary information has been obtained for strong potentials. Structural information has been obtained for low potentials. Finally, a new analytical method by CE-ESI-MS for the determination of 10B-boronophenylalanine (10B-BPA) has been developed for Boron Neutron Capture Therapy (BNCT). It has been applied to the cellular lines F98 and HUVEC. This CE-ESI-MS method has been validated by HR-ICP-MS. It enables a direct quantification of the chemical form 10B-BPA in samples of limited size (some nano-liters) and for low concentrations (ng/mL). As a consequence, this CE-ESI-MS method has enabled the study of the kinetics of 10B-BPA release and uptake for the F98 cells. (author)

  10. Application of CE-ICP-MS and CE-ESI-MS/MS for identification of Zn-binding ligands in Goji berries extracts.

    Science.gov (United States)

    Ruzik, Lena; Kwiatkowski, Piotr

    2018-06-01

    The identification of groups of ligands binding metals is a crucial issue for the better understanding of their bioaccessibility. In the current study, we have intended an approach for identification of Zn-binding ligands based on using capillary electrophoresis combined with inductively coupled plasma mass spectrometry (CE-ICP-MS) and tandem electrospray ionization mass spectrometry (CE-ESI-MS/MS). The approach, which featured the use of the coupling of capillary electrophoresis with inductively coupled plasma mass spectrometry allows to separate and observe zinc ions present in complexes with respect to their size and charge and to identify nine compounds with zinc isotopic profile. CE-ICP-MS provides us with information about presence of zinc species and elemental information about zinc distribution. CE-ESI-MS/MS provide us with information about the most favorable Zn binding ligands: amino acids, flavonols, stilbenoids, fenolic acids and carotenoids. The presented work is the continuation of previous studies based on using LC-ESI-MS/MS, though, now we presented a new solutions with the possibility of changing detectors without changing the separation techniques, what is important without re-optimizing the method. The new presented method allows to identify the zinc-binding ligands in shorter time. Copyright © 2018 Elsevier B.V. All rights reserved.

  11. High-throughput and rapid quantification of lipids by nanoflow UPLC-ESI-MS/MS: application to the hepatic lipids of rabbits with nonalcoholic fatty liver disease.

    Science.gov (United States)

    Byeon, Seul Kee; Lee, Jong Cheol; Chung, Bong Chul; Seo, Hong Seog; Moon, Myeong Hee

    2016-07-01

    A rapid and high-throughput quantification method (approximately 300 lipids within 20 min) was established using nanoflow ultrahigh-pressure liquid chromatography-tandem mass spectrometry (nUPLC-ESI-MS/MS) with selective reaction monitoring (SRM) and applied to the quantitative profiling of the hepatic lipids of rabbits with different metabolic conditions that stimulate the development of nonalcoholic fatty liver disease (NAFLD). Among the metabolic conditions of rabbits in this study [inflammation (I), high-cholesterol diet (HC), and high-cholesterol diet combined with inflammation (HCI)], significant perturbation in hepatic lipidome (>3-fold and p groups, while no single lipid showed a significant change in group I. In addition, this study revealed a dramatic increase (>2-fold) in relatively high-abundant monohexosylceramides (MHCs), sphingomyelins (SMs), and triacylglycerols (TGs) in both the HC and HCI groups, especially in MHCs as all 11 MHCs increased by larger than 3- to 12-fold. As the levels of the relatively high-abundant lipids in the above classes increased, the total lipidome level of each class increased significantly by approximately 2-fold to 5-fold. Other classes of lipids also generally increased, which was likely induced by the increase in mitogenic and nonapoptotic MHCs and SMs, as they promote cell proliferation. On the other hand, a slight decrease in the level of apoptotic ceramides (Cers) was observed, which agreed with the general increase in total lipid level. As distinct changes in hepatic lipidome were observed from HC groups, this suggests that HC or HCI is highly associated with NAFLD but not inflammation alone itself. Graphical Abstract Schematic of lipidomic analysis from hepatic tissue using nanoflow LC-ESI-MS/MS and nUPLC-ESI-MS/MS.

  12. Natural chlorate in the environment: application of a new IC-ESI/MS/MS method with a Cl¹⁸O₃-internal standard.

    Science.gov (United States)

    Balaji Rao, Balaji Rao; Hatzinger, Paul B; Böhlke, John Karl; Sturchio, Neil C; Andraski, Brian J; Eckardt, Frank D; Jackson, W Andrew

    2010-11-15

    A new ion chromatography electrospray tandem mass spectrometry (IC-ESI/MS/MS) method has been developed for quantification and confirmation of chlorate (ClO₃⁻) in environmental samples. The method involves the electrochemical generation of isotopically labeled chlorate internal standard (Cl¹⁸O₃⁻) using ¹⁸O water (H₂¹⁸O) he standard was added to all samples prior to analysis thereby minimizing the matrix effects that are associated with common ions without the need for expensive sample pretreatments. The method detection limit (MDL) for ClO₃⁻ was 2 ng L⁻¹ for a 1 mL volume sample injection. The proposed method was successfully applied to analyze ClO₃⁻ in difficult environmental samples including soil and plant leachates. The IC-ESI/MS/MS method described here was also compared to established EPA method 317.0 for ClO₃⁻ analysis. Samples collected from a variety of environments previously shown to contain natural perchlorate (ClO₄⁻) occurrence were analyzed using the proposed method and ClO₃⁻ was found to co-occur with ClO₄⁻ at concentrations ranging from 500 mg kg⁻¹ in caliche salt deposits from the Atacama Desert in Chile. Relatively low concentrations of ClO₃⁻ in some natural groundwater samples (0.1 µg L⁻¹) analyzed in this work may indicate lower stability when compared to ClO₄⁻ in the subsurface. The high concentrations ClO₃⁻ in caliches and soils (3-6 orders of magnitude greater) as compared to precipitation samples indicate that ClO₃⁻, like ClO₄⁻, may be atmospherically produced and deposited, then concentrated in dry soils, and is possibly a minor component in the biogeochemical cycle of chlorine.

  13. Natural chlorate in the environment: Application of a new IC-ESI/MS/MS method with a Cl18O3- internal standard

    Science.gov (United States)

    Rao, Balaji; Hatzinger, Paul B.; Böhlke, John Karl; Sturchio, Neil C.; Andraski, Brian J.; Eckardt, Frank D.; Jackson, W. Andrew

    2010-01-01

    A new ion chromatography electrospray tandem mass spectrometry (IC-ESI/MS/MS) method has been developed for quantification and confirmation of chlorate (ClO3−) in environmental samples. The method involves the electro-chemical generation of isotopically labeled chlorate internal standard (Cl18O3−) using 18O water (H218O). The standard was added to all samples prior to analysis thereby minimizing the matrix effects that are associated with common ions without the need for expensive sample pretreatments. The method detection limit (MDL) for ClO3− was 2 ng L−1 for a 1 mL volume sample injection. The proposed method was successfully applied to analyze ClO3− in difficult environmental samples including soil and plant leachates. The IC-ESI/MS/MS method described here was also compared to established EPA method 317.0 for ClO3− analysis. Samples collected from a variety of environments previously shown to contain natural perchlorate (ClO4−) occurrence were analyzed using the proposed method and ClO3− was found to co-occur with ClO4− at concentrations ranging from 500 mg kg−1 in caliche salt deposits from the Atacama Desert in Chile. Relatively low concentrations of ClO3− in some natural groundwater samples (<0.1 μg L−1) analyzed in this work may indicate lower stability when compared to ClO4− in the subsurface. The high concentrations of ClO3− in caliches and soils (3−6 orders of magnitude greater) as compared to precipitation samples indicate that ClO3−, like ClO4−, may be atmospherically produced and deposited, then concentrated in dry soils, and is possibly a minor component in the biogeochemical cycle of chlorine.

  14. LC-ESI-MS/MS determination of 4-methylpyrazole in dog plasma and its application to a pharmacokinetic study in dogs.

    Science.gov (United States)

    Chandrasekhar, Devaraj V; Suresh, Ponnayyan Sulochana; Dittakavi, Sreekanth; Hiremath, Rakesh A; Bhamidipati, Ravi Kanth; Richter, Wolfgang; Srinivas, Nuggehally R; Mullangi, Ramesh

    2018-02-01

    A simple, specific, sensitive and rapid LC-ESI-MS/MS method has been developed and validated for the quantification of 4-methylpyrazole in dog plasma using N-methylnicotinamide-d 4 as an internal standard (IS) as per regulatory guidelines. Sample preparation was accomplished through a simple protein precipitation. Chromatographic separation of 4-methylpyrazole and the IS was performed on a monolithic (Chromolith RP 18e ) column using an isocratic mobile phase comprising 0.2% formic acid in water and acetonitrile (20:80, v/v) at a flow rate of 1.0 mL/min. Elution of 4-methylpyrazole and the IS occurred at ~1.60 and 1.56 min, respectively. The total chromatographic run time was 3.2 min. A linear response function was established in the concentration range of 4.96-4955 ng/mL. The intra- and inter-day accuracy and precision were in the ranges 1.81-12.9 and 3.80-11.1%, respectively. This novel method has been applied to a pharmacokinetic study in dogs. Copyright © 2017 John Wiley & Sons, Ltd.

  15. Development of a UPLC-ESI-MS/MS method for the determination of larotaxel in beagle dog plasma: application to the pharmacokinetic study.

    Science.gov (United States)

    Liu, Zhenzhen; Zhang, Bo; Liu, Zhihong; Li, Song; Li, Guofei; Geng, Lulu; Zhao, Xu; Bi, Kaishun; Tang, Xing; Chen, Xiaohui

    2012-04-01

    A UPLC-ESI-MS/MS method has been developed and validated for the determination of larotaxel in beagle dog plasma. After addition of the internal standard, plasma samples were extracted by liquid-liquid extraction with methyl tert-butyl ether and separated on a 50×2.1 mm ACQUITY 1.7 μm C18 column (Waters, USA), with acetonitrile and 5 mM ammonium acetate as mobile phase, within a runtime of 3.0 min. The analytes were detected without interference in Multiple Reaction Monitoring mode with positive electrospray ionization. The linear range was 2.5-5,000 ng/mL. The intra-day and inter-day precisions (relative standard deviation, RSD, %) were within 9.3% and 10.2%, respectively, and the accuracy (relative error, RE, %) was less than 11.5%. The validated method was successfully applied to a pharmacokinetic study of larotaxel in beagle dogs after intravenous administration of larotaxel-loaded lipid microsphere with different doses of 0.4, 0.8, and 1.6 mg/kg. The area under the concentration-time curve and the peak concentration of larotaxel seemed to increase with increasing dose proportionally, suggesting linear pharmacokinetics.

  16. Pyrrolizidine alkaloids in the food chain: development, validation, and application of a new HPLC-ESI-MS/MS sum parameter method.

    Science.gov (United States)

    Cramer, Luise; Schiebel, Hans-Martin; Ernst, Ludger; Beuerle, Till

    2013-11-27

    Contamination of food and feed with pyrrolizidine alkaloids is currently discussed as a potential health risk. Here, we report the development of a new HPLC-ESI-MS/MS sum parameter method to quantitate the pyrrolizidine alkaloid content in complex food matrices. The procedure was validated for honey and culinary herbs. Isotopically labeled 7-O-9-O-dibutyroyl-[9,9-(2)H2]-retronecine was synthesized and utilized as an internal standard for validation and quantitation. The total pyrrolizidine alkaloid content of a sample is expressed as a single sum parameter: retronecine equivalents (RE). Ld/Lq for honey was 0.1 μg RE/kg/0.3 μg RE/kg. For culinary herbs, 1.0 μg RE/kg/3.0 μg RE/kg (dry weight, dw) and 0.1 μg RE/kg/0.3 μg RE/kg (fresh weight, fw) were determined, respectively. The new method was applied to analyze 21 herbal convenience products. Fifteen products (71%) were pyrrolizidine alkaloid positive showing pyrrolizidine alkaloid concentrations ranging from 0.9 to 74 μg RE/kg fw.

  17. Determination of Mycophenolic acid in the vitreous humor using the HPLC-ESI-MS/MS method: application of intraocular pharmacokinetics study in rabbit eyes with ophthalmic implantable device.

    Science.gov (United States)

    Martins Duarte Byrro, Ricardo; de Oliveira Fulgêncio, Gustavo; Rocha Chellini, Paula; da Silva Cunha, Armando; Pianetti, Gerson Antônio

    2013-10-01

    Mycophenolic acid (MPA) is an immunosuppressive agent widely used in the treatment of solid organ transplant rejection. The success of MPA in the treatment of inflammatory intraocular diseases has been reported in recent literature. The treatment of inflammatory eye diseases in the posterior chamber is a challenge due to the anatomy of the eye, which presents certain barriers to drug access. Thus, the bioavailability of drugs in the eye is quite low, and successful drug delivery may well represent a key limiting factor to attaining a successful therapeutic strategy. Ophthalmic controlled drug delivery offers the potential to enhance the efficacy of treatment for pathological conditions. Thus, a novel delivery system based on a biodegradable polymeric device, which can be implanted inside the eye and deliver MPA directly to the target, is being developed. Specific analytical methods to determine the use of effective drugs within the eye are needed to characterize this device. A liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI-MS/MS) method for the quantitation of MPA in the vitreous humor of rabbits was developed and validated. The vitreous was collected from rabbits, extracted by a protein precipitation extraction procedure and then separated on a C18 column with a mobile phase comprised of 0.15% aqueous acetic acid and methanol (60:40, v/v). The calibration curve was constructed within the range of 3-10,000 ng/mL for MPA. The mean R.S.D. values for the intra-run and inter-run precision were 5.15% and 4.35%. The mean accuracy value was 100.16%. The validated method was successfully applied to determine the MPA concentration in the vitreous humor of rabbits treated with an ocular implantable device. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. Quantification of sibutramine and its two metabolites in human plasma by LC–ESI-MS/MS and its application in a bioequivalence study

    Directory of Open Access Journals (Sweden)

    Venkata Suresh Ponnuru

    2012-08-01

    Full Text Available Obesity can be considered as a chronic illness of epidemic proportion and its incidents have increased exponentially in recent years. The use of anti-obesity drugs such as sibutramine is somewhat helpful. There is a need to quantify such drugs in biological samples, which is generally quite difficult. In this report, we developed and validated a simple, sensitive and specific liquid chromatography–tandem mass spectrometry (LC–MS/MS method for the quantification of sibutramine (SB and its two metabolites N-des methyl sibutramine (DSB and N-di desmethyl sibutramine (DDSB in human plasma. Zorbax SB-C18 (4.6 mm×75 mm, 3.5 μm, 80 Å analytical column and 5 mM ammonium formate:acetonitrile (10:90, v/v mobile phase were used for chromatographic separation of SB, DSB and DDSB. Multiple reaction monitoring (MRM in the positive mode was used to detect SB, DSB and DDSB at m/z 280.3/124.9, 266.3/125.3 and 252.2/124.9, respectively. Liquid–liquid extraction was used for the extraction of analytes and internal standard from human plasma. This method was validated over a linear concentration range of 10.0–10,000.0 pg/mL for SB, DSB and DDSB with correlation coefficients (r of ≥0.9997. The drug and the two metabolites were stable in plasma samples. The validated method was successfully applied in a bioequivalence and pharmacokinetic study with human volunteers under fasting condition. Keywords: LC–ESI-MS/MS, Sibutramine, Human plasma, Bioequivalence, Pharmacokinetic study

  19. Application of HPLC and ESI-MS techniques in the analysis of phenolic acids and flavonoids from green leafy vegetables (GLVs

    Directory of Open Access Journals (Sweden)

    B. Ramesh Kumar

    2017-12-01

    Full Text Available Diets containing high proportions of fruits and vegetables reduce the risk of onset of chronic diseases. The role of herbal medicines in improving human health is gaining popularity over the years, which also increases the need for safety and efficiency of these products. Green leafy vegetables (GLVs are the richest source of phenolic compounds with excellent antioxidant properties. Increased consumption of diets containing phenolic compounds may give positive and better results to human health and significantly improves the immune system. Highly selective, susceptible and versatile analytical techniques are necessary for extraction, identification, and quantification of phenolic compounds from plant extracts, which helps to utilize their important biological properties. Recent advances in the pre-treatment procedures, separation techniques and spectrometry methods are used for qualitative and quantitative analysis of phenolic compounds. The online coupling of liquid chromatography with mass spectrometry (LC–MS has become a useful tool in the metabolic profiling of plant samples. In this review, the separation and identification of phenolic acids and flavonoids from GLVs by LC–MS have been discussed along with the general extraction procedures and other sources of mass spectrometer used. The review is devoted to the understanding of the structural configuration, nature and accumulation pattern of phenolic acids and flavonoids in plants and to highlighting the recent developments in the chemical investigation of these compounds by chromatographic and spectroscopic techniques. It concludes with the advantages of the combination of these two methods and prospects. Keywords: Green leafy vegetables, Phenolic acids, Flavonoids, HPLC, ESI-MS

  20. Effective application of freezing lipid precipitation and SCX-SPE for determination of pyrrolizidine alkaloids in high lipid foodstuffs by LC-ESI-MS/MS.

    Science.gov (United States)

    Yoon, Soo Hwan; Kim, Min-Sun; Kim, Sang Hoon; Park, Hyun Mee; Pyo, Heesoo; Lee, Yong Moon; Lee, Kyung-Tae; Hong, Jongki

    2015-06-15

    Pyrrolizidine alkaloids (PAs) are naturally occurring plant toxins associated with serious hepatic disease in humans and animals. In this study, rapid and sensitive analytical method was developed for the determination of 9 toxic PAs in popularly high lipid foodstuffs by liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS). PAs in lipid foodstuff were effectively purified by freezing lipid precipitation (FLP) and strong cation exchange (SCX)-solid-phase extraction (SPE). Especially, FLP could easily remove the large amounts of triacylglycerols in the lipid sample extract and effectively combine with SPE cleanup. During the FLP procedure, over 77% of the lipids in the foodstuff extracts were rapidly eliminated without any significant loss of the PAs with over 81% recovery. The elimination efficiency of lipids by FLP was tested with LC-atmospheric chemical ionization (APCI)-MS. For further purification, SCX-SPE cartridge could successfully purify PAs from the remaining interfering substances by the variation pH with 5% NH4OH in methanol. For precise quantification and confirmation of PAs in complicate sample matrices, appropriate transition ions in LC-MS/MS-multiple-ion reaction monitoring (MRM) mode were selected on the basis of MS/MS fragmentation pathways of PAs. The established analytical method was validated in terms of the linearity, limits of detection (LOD), and quantification (LOQ), precision, and accuracy. The method was deemed satisfactory by inter- and intra-day validation and exhibited both high accuracy and precision (relative standard deviation<11.06%). Overall limits of detection and quantitation of PAs were approximately 0.06-0.60ng/mL at a signal-to-noise ratio (S/N) of 3 and were about 0.20-1.99ng/mL at a S/N of 10 for all foodstuffs. The established method was successfully applied for the monitoring of toxic PAs in several types of high lipid foodstuffs such as soybeans, seed oil, milk, and margarine. Copyright

  1. Development of a chromatographic separation method hyphenated to electro-spray ionization mass spectrometry (ESI-MS) and inductively coupled plasma mass spectrometry (ICP-MS): application to the lanthanides speciation analysis

    International Nuclear Information System (INIS)

    Beuvier, Ludovic

    2015-01-01

    This work focuses on the development of a chromatographic separation method coupled to both ESI-MS and ICP-MS in order to achieve the comprehensive speciation analysis of lanthanides in aqueous phase representative of back-extraction phases of advanced spent nuclear fuel treatment processes. This analytical method allowed the separation, the characterization and the quantitation of lanthanides complexes holding poly-aminocarboxylic ligands, such as DTPA and EDTA, used as complexing agents in these processes. A HILIC separation method of lanthanides complexes has been developed with an amide bonded stationary phase. A screening of a wide range of mobile phase compositions demonstrated that the adsorption mechanism was predominant. This screening allowed also obtaining optimized separation conditions. Faster analysis conditions with shorter amide column packed with sub 2 μm particles reduced analysis time by 2.5 and 25% solvent consumption. Isotopic and structural characterization by HILIC ESI-MS was performed as well as the development of external calibration quantitation method. Analytical performances of quantitation method were determined. Finally, the development of the HILIC coupling to ESI-MS and ICP-MS was achieved. A simultaneous quantitation method by ESI-MS and ICP-MS was performed to determine the species quantitative distribution in solution. Analytical performances of quantitation method were also determined. (author) [fr

  2. Simultaneous quantification of tafetinib (SIM010603), a novel potent inhibitor of receptor tyrosine kinase, and its major metabolite in dog plasma by HPLC-ESI/MS/MS and its application to a pharmacokinetic study.

    Science.gov (United States)

    Shao, Feng; Zhu, Tian; Tang, Feng; Liu, Xin

    2013-01-01

    This study presents a high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (HPLC-ESI/MS/MS) technique for the simultaneous determination of tafetinib (SIM010603) and its main metabolite (M1) in dog plasma by using Prazosin hydrochloric acid as the internal standard (IS). Both compounds were extracted from dog plasma with ethyl acetate and were separated by HPLC on a reversed phase C₁₈ column with a mobile phase of 10 mM ammonium acetate buffer containing 0.1% formic acid-acetonitrile (40:60, v/v) at a flow rate of 0.2 mL/min. For quantification, the triple-quadruple MS was used in selected reaction monitoring (SRM) mode. The monitored transitions were m/z 425.3 → 309.2 for tafetinib, m/z 397.2 → 309.2 for M1 and m/z 384.2 → 247.1 for IS. The developed method had a short run time of 4 min and good linearity was observed over a wide range of 1-1000 ng/mL for the two compounds. The method was successfully applied in the pharmacokinetic study of tafetinib and M1 in dog. Copyright © 2013 Elsevier B.V. All rights reserved.

  3. Characterization, stoichiometry, and stability of salivary protein-tannin complexes by ESI-MS and ESI-MS/MS.

    Science.gov (United States)

    Canon, Francis; Paté, Franck; Meudec, Emmanuelle; Marlin, Thérèse; Cheynier, Véronique; Giuliani, Alexandre; Sarni-Manchado, Pascale

    2009-12-01

    Numerous protein-polyphenol interactions occur in biological and food domains particularly involving proline-rich proteins, which are representative of the intrinsically unstructured protein group (IUP). Noncovalent protein-ligand complexes are readily detected by electrospray ionization mass spectrometry (ESI-MS), which also gives access to ligand binding stoichiometry. Surprisingly, the study of interactions between polyphenolic molecules and proteins is still an area where ESI-MS has poorly benefited, whereas it has been extensively applied to the detection of noncovalent complexes. Electrospray ionization mass spectrometry has been applied to the detection and the characterization of the complexes formed between tannins and a human salivary proline-rich protein (PRP), namely IB5. The study of the complex stability was achieved by low-energy collision-induced dissociation (CID) measurements, which are commonly implemented using triple quadrupole, hybrid quadrupole time-of-flight, or ion trap instruments. Complexes composed of IB5 bound to a model polyphenol EgCG have been detected by ESI-MS and further analyzed by MS/MS. Mild ESI interface conditions allowed us to observe intact noncovalent PRP-tannin complexes with stoichiometries ranging from 1:1 to 1:5. Thus, ESI-MS shows its efficiency for (1) the study of PRP-tannin interactions, (2) the determination of stoichiometry, and (3) the study of complex stability. We were able to establish unambiguously both their stoichiometries and their overall subunit architecture via tandem mass spectrometry and solution disruption experiments. Our results prove that IB5.EgCG complexes are maintained intact in the gas phase.

  4. Quantitative analysis of the major constituents of St John's wort with HPLC-ESI-MS.

    Science.gov (United States)

    Chandrasekera, Dhammitha H; Welham, Kevin J; Ashton, David; Middleton, Richard; Heinrich, Michael

    2005-12-01

    A method was developed to profile the major constituents of St John's wort extracts using high-performance liquid chromatography-electrospray mass spectrometry (HPLC-ESI-MS). The objective was to simultaneously separate, identify and quantify hyperforin, hypericin, pseudohypericin, rutin, hyperoside, isoquercetrin, quercitrin and chlorogenic acid using HPLC-MS. Quantification was performed using an external standardisation method with reference standards. The method consisted of two protocols: one for the analysis of flavonoids and glycosides and the other for the analysis of the more lipophilic hypericins and hyperforin. Both protocols used a reverse phase Luna phenyl hexyl column. The separation of the flavonoids and glycosides was achieved within 35 min and that of the hypericins and hyperforin within 9 min. The linear response range in ESI-MS was established for each compound and all had linear regression coefficient values greater than 0.97. Both protocols proved to be very specific for the constituents analysed. MS analysis showed no other signals within the analyte peaks. The method was robust and applicable to alcoholic tinctures, tablet/capsule extracts in various solvents and herb extracts. The method was applied to evaluate the phytopharmaceutical quality of St John's wort preparations available in the UK in order to test the method and investigate if they contain at least the main constituents and at what concentrations.

  5. Phytochemical Analysis of Pfaffia glomerata Inflorescences by LC-ESI-MS/MS

    Directory of Open Access Journals (Sweden)

    Daniele F. Felipe

    2014-09-01

    Full Text Available Pfaffia glomerata contains high levels of β-ecdysone, which has shown a range of beneficial pharmacological effects. The present study demonstrated that inflorescences of P. glomerata contain other important bioactive compounds in addition to β-ecdysone. The identification of compounds from inflorescences using liquid chromatography coupled with electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS was performed for the first time. The eight compounds identified were β-ecdysone, flavonoid glycosides such as quercetin-3-O-glucoside, kaempferol-3-O-glucoside and kaempferol-3-O-(6-p-coumaroyl-glucoside, oleanane-type triterpenoid saponins such as ginsenoside Ro and chikusetsusaponin IV, in addition to oleanonic acid and gluconic acid. This study provided information on the phytochemicals contained in P. glomerata inflorescences revealing the potential application of this plant part as raw material for the phytotherapeutic and cosmetic industries.

  6. UFLC-ESI-MS/MS analysis of multiple mycotoxins in medicinal and edible Areca catechu.

    Science.gov (United States)

    Liu, Hongmei; Luo, Jiaoyang; Kong, Weijun; Liu, Qiutao; Hu, Yichen; Yang, Meihua

    2016-05-01

    A robust, sensitive and reliable ultra fast liquid chromatography combined with electrospray ionization tandem mass spectrometry (UFLC-ESI-MS/MS) was optimized and validated for simultaneous identification and quantification of eleven mycotoxins in medicinal and edible Areca catechu, based on one-step extraction without any further clean-up. Separation and quantification were performed in both positive and negative modes under multiple reaction monitoring (MRM) in a single run with zearalanone (ZAN) as internal standard. The chromatographic conditions and MS/MS parameters were carefully optimized. Matrix-matched calibration was recommended to reduce matrix effects and improve accuracy, showing good linearity within wide concentration ranges. Limits of quantification (LOQ) were lower than 50 μg kg(-1), while limits of detection (LOD) were in the range of 0.1-20 μg kg(-1). The accuracy of the developed method was validated for recoveries, ranging from 85% to 115% with relative standard deviation (RSD) ≤14.87% at low level, from 75% to 119% with RSD ≤ 14.43% at medium level and from 61% to 120% with RSD ≤ 13.18% at high level, respectively. Finally, the developed multi-mycotoxin method was applied for screening of these mycotoxins in 24 commercial samples. Only aflatoxin B2 and zearalenone were found in 2 samples. This is the first report on the application of UFLC-ESI(+/-)-MS/MS for multi-class mycotoxins in A. catechu. The developed method with many advantages of simple pretreatment, rapid determination and high sensitivity is a proposed candidate for large-scale detection and quantification of multiple mycotoxins in other complex matrixes. Copyright © 2016 Elsevier Ltd. All rights reserved.

  7. Validated analytical methodology for the simultaneous determination of a wide range of pesticides in human blood using GC-MS/MS and LC-ESI/MS/MS and its application in two poisoning cases.

    Science.gov (United States)

    Luzardo, Octavio P; Almeida-González, Maira; Ruiz-Suárez, Norberto; Zumbado, Manuel; Henríquez-Hernández, Luis A; Meilán, María José; Camacho, María; Boada, Luis D

    2015-09-01

    Pesticides are frequently responsible for human poisoning and often the information on the involved substance is lacking. The great variety of pesticides that could be responsible for intoxication makes necessary the development of powerful and versatile analytical methodologies, which allows the identification of the unknown toxic substance. Here we developed a methodology for simultaneous identification and quantification in human blood of 109 highly toxic pesticides. The application of this analytical scheme would help in minimizing the cost of this type of chemical identification, maximizing the chances of identifying the pesticide involved. In the methodology that we present here, we use a liquid-liquid extraction, followed by one single purification step, and quantitation of analytes by a combination of liquid and gas chromatography, both coupled to triple quadrupole mass spectrometry, which is operated in the mode of multiple reaction monitoring. The methodology has been fully validated, and its applicability has been demonstrated in two recent cases involving one self-poisoning fatality and one non-fatal homicidal attempt. Copyright © 2015 The Chartered Society of Forensic Sciences. Published by Elsevier Ireland Ltd. All rights reserved.

  8. Experimental variability and data pre-processing as factors affecting the discrimination power of some chemometric approaches (PCA, CA and a new algorithm based on linear regression) applied to (+/-)ESI/MS and RPLC/UV data: Application on green tea extracts.

    Science.gov (United States)

    Iorgulescu, E; Voicu, V A; Sârbu, C; Tache, F; Albu, F; Medvedovici, A

    2016-08-01

    The influence of the experimental variability (instrumental repeatability, instrumental intermediate precision and sample preparation variability) and data pre-processing (normalization, peak alignment, background subtraction) on the discrimination power of multivariate data analysis methods (Principal Component Analysis -PCA- and Cluster Analysis -CA-) as well as a new algorithm based on linear regression was studied. Data used in the study were obtained through positive or negative ion monitoring electrospray mass spectrometry (+/-ESI/MS) and reversed phase liquid chromatography/UV spectrometric detection (RPLC/UV) applied to green tea extracts. Extractions in ethanol and heated water infusion were used as sample preparation procedures. The multivariate methods were directly applied to mass spectra and chromatograms, involving strictly a holistic comparison of shapes, without assignment of any structural identity to compounds. An alternative data interpretation based on linear regression analysis mutually applied to data series is also discussed. Slopes, intercepts and correlation coefficients produced by the linear regression analysis applied on pairs of very large experimental data series successfully retain information resulting from high frequency instrumental acquisition rates, obviously better defining the profiles being compared. Consequently, each type of sample or comparison between samples produces in the Cartesian space an ellipsoidal volume defined by the normal variation intervals of the slope, intercept and correlation coefficient. Distances between volumes graphically illustrates (dis)similarities between compared data. The instrumental intermediate precision had the major effect on the discrimination power of the multivariate data analysis methods. Mass spectra produced through ionization from liquid state in atmospheric pressure conditions of bulk complex mixtures resulting from extracted materials of natural origins provided an excellent data

  9. Determining the degradation efficiency and mechanisms of ethyl violet using HPLC-PDA-ESI-MS and GC-MS

    Directory of Open Access Journals (Sweden)

    Chung Wen-Hsin

    2012-06-01

    Full Text Available Abstract Background The discharge of wastewater that contains high concentrations of reactive dyes is a well-known problem associated with dyestuff activities. In recent years, semiconductor photocatalysis has become more and more attractive and important since it has a great potential to contribute to such environmental problems. One of the most important aspects of environmental photocatalysis is in the selection of semiconductor materials like ZnO and TiO2, which are close to being two of the ideal photocatalysts in several respects. For example, they are relatively inexpensive, and they provide photo-generated holes with high oxidizing power due to their wide band gap energy. In this work, nanostructural ZnO film on the Zn foil of the Alkaline-Manganese Dioxide-Zinc Cell was fabricated to degrade EV dye. The major innovation of this paper is to obtain the degradation mechanism of ethyl violet dyes resulting from the HPLC-PDA-ESI-MS analyses. Results The fabrication of ZnO nanostructures on zinc foils with a simple solution-based corrosion strategy and the synthesis, characterization, application, and implication of Zn would be reported in this study. Other objectives of this research are to identify the reaction intermediates and to understand the detailed degradation mechanism of EV dye, as model compound of triphenylmethane dye, with active Zn metal, by HPLC-ESI-MS and GC-MS. Conclusions ZnO nanostructure/Zn-foils had an excellent potential for future applications on the photocatalytic degradation of the organic dye in the environmental remediation. The intermediates of the degradation process were separated and characterized by the HPLC-PDA-ESI-MS and GC-MS, and twenty-six intermediates were characterized in this study. Based on the variation of the amount of intermediates, possible degradation pathways for the decolorization of dyes are also proposed and discussed.

  10. A simple, rapid and stability indicating validated method for quantification of lamotrigine in human plasma and dry plasma spot using LC-ESI-MS/MS: Application in clinical study.

    Science.gov (United States)

    Namdev, Kuldeep Kumar; Dwivedi, Jaya; Chilkoti, Deepak Chandra; Sharma, Swapnil

    2018-01-01

    Lamotrigine (LTZ) is a phenyltriazine derivative which belongs to anti-epileptic drugs (AEDs) class and prescribed as mono- or adjunctive-therapy in treatment of epilepsy. Therapeutic drug monitoring (TDM) of AEDs provides a valid clinical tool in optimization of overall therapy. However, TDM is challenging due to the high biological samples (plasma/blood) storage/shipment costs and the limited availability of laboratories providing TDM services. Sampling in the form of dry plasma spot (DPS) or dry blood spot (DBS) are suitable alternative to overcome these issues. We developed and validated a new method for quantification of LTZ in human plasma and DPS. The extraction of LTZ from plasma and DPS was performed using liquid-liquid extraction with diethyl ether and an extraction solution composed of diethyl ether- methyl tert-butyl ether- acetone (50:30:20, v/v/v), respectively. Lamotrigine- 13C3, d3 was used as internal standard (ISTD) and the chromatographic separation was achieved on Hypurity Advance C18 column (150×4.6mm, 5μm). Quantitative estimation of LTZ and ISTD was performed on a liquid chromatography tandem mass spectrometer coupled with electrospray ionization interface operated under positive mode of ionization. Calibration curves were linear (r 2 >0.99) over the concentration range of 10-3020ng/mL for both plasma and DPS. Statistical analysis provides insignificant difference between LTZ concentration extracted from plasma and DPS samples. The method is found suitable for application in clinical study and in therapeutic monitoring of LTZ. To the best of our knowledge this is the first report which describing a validated stability indicating assay for quantification of LTZ in dry plasma spot. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Metabolic profiling of roots of liquorice (Glycyrrhiza glabra) from different geographical areas by ESI/MS/MS and determination of major metabolites by LC-ESI/MS and LC-ESI/MS/MS.

    Science.gov (United States)

    Montoro, Paola; Maldini, Mariateresa; Russo, Mariateresa; Postorino, Santo; Piacente, Sonia; Pizza, Cosimo

    2011-02-20

    Liquid chromatography electrospray mass spectrometry (LC-ESI/MS) has been applied to the full characterization of saponins and phenolics in hydroalcoholic extracts of roots of liquorice (Glycyrrhiza glabra). Relative quantitative analyses of the samples with respect to the phenolic constituents and to a group of saponins related to glycyrrhizic acid were performed using LC-ESI/MS. For the saponin constituents, full scan LC-MS/MS fragmentation of the protonated (positive ion mode) or deprotonated (negative ion mode) molecular species generated diagnostic fragment ions that provided information concerning the triterpene skeleton and the number and nature of the substituents. On the basis of the specific fragmentation of glycyrrhizic acid, an LC-MS/MS method was developed in order to quantify the analyte in the liquorice root samples. Chinese G. glabra roots contained the highest levels of glycyrrhizic acid, followed by those from Italy (Calabria). Copyright © 2010 Elsevier B.V. All rights reserved.

  12. Screening natural libraries of human milk oligosaccharides against lectins using CaR-ESI-MS.

    Science.gov (United States)

    El-Hawiet, Amr; Chen, Yajie; Shams-Ud-Doha, Km; Kitova, Elena N; Kitov, Pavel I; Bode, Lars; Hage, Naim; Falcone, Franco H; Klassen, John S

    2018-01-15

    Human milk oligosaccharides (HMOs) afford many health benefits to breast-fed infants, such as protection against infection and regulation of the immune system, through the formation of non-covalent interactions with protein receptors. However, the molecular details of these interactions are poorly understood. Here, we describe the application of catch-and-release electrospray ionization mass spectrometry (CaR-ESI-MS) for screening natural libraries of HMOs against lectins. The HMOs in the libraries were first identified based on molecular weights (MWs), ion mobility separation arrival times (IMS-ATs) and collision-induced dissociation (CID) fingerprints of their deprotonated anions. The libraries were then screened against lectins and the ligands identified from the MWs, IMS-ATs and CID fingerprints of HMOs released from the lectin in the gas phase. To demonstrate the assay, four fractions, extracted from pooled human milk and containing ≥35 different HMOs, were screened against a C-terminal fragment of human galectin-3 (hGal-3C), for which the HMOs specificities have been previously investigated, and a fragment of the blood group antigen-binding adhesin (BabA) from Helicobacter pylori, for which the HMO specificities have not been previously established. The structures of twenty-one ligands, corresponding to both neutral and acidic HMOs, of hGal-3C were identified; all twenty-one were previously shown to be ligands for this lectin. The presence of HMO ligands at six other MWs was also ascertained. Application of the assay to BabA revealed nineteen specific HMO structures that are recognized by the protein and HMO ligands at two other MWs. Notably, it was found that BabA exhibits broad specificity for HMOs, and recognizes both neutral HMOs, including non-fucosylated ones, and acidic HMOs. The results of competitive binding experiments indicate that HMOs can interact with BabA at previously unknown binding sites. The affinities of eight purified HMOs for BabA were

  13. Practical approaches to the ESI-MS analysis of catalytic reactions.

    Science.gov (United States)

    Yunker, Lars P E; Stoddard, Rhonda L; McIndoe, J Scott

    2014-01-01

    Electrospray ionization mass spectrometry (ESI-MS) is a soft ionization technique commonly coupled with liquid or gas chromatography for the identification of compounds in a one-time view of a mixture (for example, the resulting mixture generated by a synthesis). Over the past decade, Scott McIndoe and his research group at the University of Victoria have developed various methodologies to enhance the ability of ESI-MS to continuously monitor catalytic reactions as they proceed. The power, sensitivity and large dynamic range of ESI-MS have allowed for the refinement of several homogenous catalytic mechanisms and could potentially be applied to a wide range of reactions (catalytic or otherwise) for the determination of their mechanistic pathways. In this special feature article, some of the key challenges encountered and the adaptations employed to counter them are briefly reviewed. Copyright © 2014 John Wiley & Sons, Ltd.

  14. Real-time ESI-MS of enzymatic conversion: impact of organic solvents and multiplexing.

    Science.gov (United States)

    Scheerle, Romy K; Grassmann, Johanna; Letzel, Thomas

    2012-01-01

    Different enzymatic assays were characterized systematically by real-time electrospray ionization mass spectrometry (ESI-MS) in the presence of organic solvents as well as in multiplex approaches and in a combination of both. Typically, biological enzymatic reactions are studied in aqueous solutions, since most enzymes show their full activity solely in aqueous solutions. However, in recent years, the use of organic solvents in combination with enzymatic reactions has gained increasing interest due to biotechnological advantages in chemical synthesis, development of online coupled setups screening for enzyme regulatory compounds, advantages regarding mass spectrometric detection and others. In the current study, the influence of several common organic solvents (methanol, ethanol, isopropanol, acetone, acetonitrile) on enzymatic activity (hen egg white lysozyme, chitinase, α-chymotrypsin, elastase from human neutrophils and porcine pancreas, acetylcholinesterase) was tested. Moreover, multiplexing is a promising approach enabling fast and cost-efficient screening methods, e.g. for determination of inhibitors in complex mixtures or in the field of biomedical research. Although in multiplexed setups the enzymatic activity may be affected by the presence of other substrates and/or enzymes, the expected advantages possibly will predominate. To investigate those effects, we measured multiple enzymatic assays simultaneously. For all conducted measurements, the conversion rate of the substrate(s) was calculated, which reflects the enzymatic activity. The results provide an overview about the susceptibility of the selected enzymes towards diverse factors and a reference point for many applications in analytical chemistry and biotechnology.

  15. Molecular diagnosis of bloodstream infections in onco-haematology patients with PCR/ESI-MS technology.

    Science.gov (United States)

    Jordana-Lluch, Elena; Rivaya, Belén; Marcó, Clara; Giménez, Montserrat; Quesada, Mª Dolores; Escobedo, Agustín; Batlle, Montserrat; Martró, Elisa; Ausina, Vicente

    2017-02-01

    Onco-haematological patients are prone to develop infections, and antibiotic prophylaxis may lead to negative blood cultures. Thus, the microbiological diagnosis and subsequent administration of a targeted antimicrobial therapy is often difficult. The goal of this study was to evaluate the usefulness of IRIDICA (PCR/ESI-MS technology) for the molecular diagnosis of bloodstream infections in this patient group. A total of 463 whole blood specimens from different sepsis episodes in 429 patients were analysed using the PCR/ESI-MS platform, comparing the results with those of blood culture and other clinically relevant information. The sensitivity of PCR/ESI-MS by specimen (excluding polymicrobial infections, n = 25) in comparison with blood culture was 64.3% overall, 69.0% in oncological patients, and 59.3% in haematological patients. When comparing with a clinical infection criterion, overall sensitivity rose to 74.7%, being higher in oncological patients (80.0%) than in haematological patients (67.7%). Thirty-one microorganisms isolated by culture were not detected by IRIDICA, whereas 42 clinically relevant pathogens not isolated by culture were detected moleculary. PCR/ESI-MS offers a reliable identification of pathogens directly from whole blood. While additional studies are needed to confirm our findings, the system showed a lower sensitivity in onco-haematological patients in comparison with previously reported results in patients from the Intensive Care Unit. Copyright © 2016 The British Infection Association. Published by Elsevier Ltd. All rights reserved.

  16. Analysis of triglyceride degradation products in drying oils and oil paints using LC–ESI-MS

    NARCIS (Netherlands)

    van Dam, E.P.; van den Berg, K.J.; Proaño Gaibor, A.N.; van Bommel, M.

    An LC–ESI-MS method is presented as a novel approach for the study of aged drying oils and oil paints invarious stages of oxidation and hydrolysis. The method involves separation and detection of glyceridesand fatty acids on a reversed phase column using a polar gradient ranging from methanol/water

  17. Lanthanide and actinide inorganic complexes in natural waters. TRLFS and ESI-MS studies

    Energy Technology Data Exchange (ETDEWEB)

    Vercouter, T.; Amekraz, B.; Moulin, C.; Vitorge, P

    2004-07-01

    Aqueous complexes of M(III) f-element ions with the inorganic ligands CO{sub 3}{sup 2-} and SO{sub 4}{sup 2-} have been investigated using the highly-sensitive speciation techniques TRLFS and ESI-MS. The Eu(CO{sub 3}){sub i}{sup 3-2i} (i=1-3) species have been characterized by TRLFS, and the stoichiometry of the limiting complex Eu(CO{sub 3}){sub 3}{sup 3-} have been confirmed by solubility measurements of NaEu(CO{sub 3}){sub 2}(s) at high ionic strength. Temperature effect on Cm(III) carbonate complexes is evidenced by the TRLFS technique. Investigation on sulphate complexation has been done at various ionic strengths by TRLFS on Eu(III) and by ESI-MS on La(III). New thermodynamic data are obtained by both techniques, which are consistent with literature data. (authors)

  18. LC/ESI-MS method applied to characterization of flavonoids glycosides in B. forficata subsp. pruinosa

    Directory of Open Access Journals (Sweden)

    Lidiane da Silveira Farias

    2014-06-01

    Full Text Available Bauhinia forficata is used in folk medicine for its hypoglycemiant effect. In the south of Brazil, the subspecies pruinosa is found in a region with the characteristic flora, pampa biome. This species has been consumed by the local population as a tea for diabetes treatment. We studied the chemical composition of hydroethanolic extracts using LC/ESI-MS. The leaf extracts were prepared by percolation with 50% (v/v ethanol. The chromatographic analyses were performed using a reverse-phase system, gradient elution with acetonitrile:phosphoric acid 0.05%, and ESI-MS in the positive ion mode. The chemical profile of the flavonoids was suggested to involve four quercetin and kaempferol glycosides.

  19. Ellagitannin composition of blackberry as determined by HPLC-ESI-MS and MALDI-TOF-MS.

    Science.gov (United States)

    Hager, Tiffany J; Howard, Luke R; Liyanage, Rohana; Lay, Jackson O; Prior, Ronald L

    2008-02-13

    Blackberries ( Rubus sp.) were evaluated by high-performance liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS) and matrix-assisted laser desorption/ionization-time-of-flight mass spectrometry (MALDI-TOF-MS) to identify the ellagitannins present in flesh, torus (receptacle tissue), and seeds. Most ellagitannins were present (or detectable) only in seed tissues. Ellagitannins identified by HPLC-ESI-MS in the seeds included pedunculagin, casuarictin/potentillin, castalagin/vescalagin, lambertianin A/sanguiin H-6, lambertianin C, and lambertianin D. For several of the ellagitannins, isomeric separation was also obtained. The MALDI-TOF-MS analysis was primarily utilized to evaluate and identify high molecular mass (>1000 Da) ellagitannins. The MALDI analysis verified the presence of the ellagitannins identified by HPLC-ESI-MS including lambertianin A/sanguiin H-6, lambertianin C, and lambertianin D, but the analysis also indicated the presence of several other compounds that were most likely ellagitannins based on the patterns observed in the masses (i.e., loss or addition of a gallic acid moiety to a known ellagitannin). This study determined the presence of several possible isomeric forms of ellagitannins previously unidentified in fruit and presents a possible analytical HPLC method for the analysis of the major ellagitannins present in the fruit.

  20. Comparison of LC-ESI-MS and GC-MS for the Analysis of a Synthetic Tabun Sample

    National Research Council Canada - National Science Library

    D'Agostino, Paul

    2003-01-01

    Packed capillary LC-ESI-MS and capillary column GC-MS were compared for the analysis of a synthetic tabun sample as each method has advantages for the analysis of samples containing chemical warfare...

  1. Comparison of piracetam measured with HPLC-DAD, HPLC-ESI-MS, DIP-APCI-MS, and a newly developed and optimized DIP-ESI-MS.

    Science.gov (United States)

    Lenzen, Claudia; Winterfeld, Gottfried A; Schmitz, Oliver J

    2016-06-01

    The direct inlet probe-electrospray ionization (DIP-ESI) presented here was based on the direct inlet probe-atmospheric pressure chemical ionization (DIP-APCI) developed by our group. It was coupled to an ion trap mass spectrometer (MS) for the detection of more polar compounds such as degradation products from pharmaceuticals. First, the position of the ESI tip, the gas and solvent flow rates, as well as the gas temperature were optimized with the help of the statistic program Minitab® 17 and a caffeine standard. The ability to perform quantitative analyses was also tested by using different concentrations of caffeine and camphor. Calibration curves with a quadratic calibration regression of R (2) = 0.9997 and 0.9998 for caffeine and camphor, respectively, were obtained. The limit of detection of 2.5 and 1.7 ng per injection for caffeine and camphor were determined, respectively. Furthermore, a solution of piracetam was used to compare established analytical methods for this drug and its impurities such as HPLC-diode array detector (DAD) and HPLC-ESI-MS with the DIP-APCI and the developed DIP-ESI. With HPLC-DAD and 10 μg piracetam on column, no impurity could be detected. With HPLC-ESI-MS, two impurities (A and B) were identified with only 4.6 μg piracetam on column, while with DIP-ESI, an amount of 1.6 μg piracetam was sufficient. In the case of the DIP-ESI measurements, all detected impurities could be identified by MS/MS studies. Graphical Abstract Scheme of the DIP-ESI principle.

  2. ESI MS/MS Study of Calix[4]arene Derivatives and their Metal Complexes

    OpenAIRE

    Benković, Tomislav; Tomišić, Vladislav; Frkanec, Leo; Galić, Nives

    2012-01-01

    The peptidocalixarenes 1–3 bearing tryptophan, phenylglycine and leucil units at the lower rim and their complexes with alkali-metal (Li+, Na+, K+, Rb+, Cs+) and selected lanthanide cations (La3+, Ce3+, Eu3+, Yb3+) were analyzed by ESI MS. The influences of the solvent (acetonitrile, methanol, addition of formic acid or sodium acetate) and the calixarene:cation molar ratio on signal intensities were investigated. Comprehensive MS/MS analyses were performed of all singly and doubly charged ion...

  3. LC/PDA/ESI-MS Profiling and Radical Scavenging Activity of Anthocyanins in Various Berries

    Directory of Open Access Journals (Sweden)

    Jun-ichiro Nakajima

    2004-01-01

    Full Text Available Anthocyanin extracts of two blueberries, Vaccinium myrtillus (bilberry and Vaccinium ashei (rabbiteye blueberry, and of three other berries, Ribes nigrum (black currant, Aronia melanocarpa (chokeberry, and Sambucus nigra (elderberry, were analyzed by high-performance liquid chromatography coupled with photodiode array detection and electrospray ionization - mass spectrometry (LC/PDA/ESI-MS. Both bilberry and rabbiteye blueberry contained 15 identical anthocyanins with different distribution patterns. Black currant, chokeberry, and elderberry contained 6, 4, and 4 kinds of anthocyanins, respectively. The radical scavenging activities of these berry extracts were analyzed by using 2,2-diphenyl-1-picrylhydrazyl (DPPH. All these extracts showed potent antiradical activities.

  4. Detecting Protein-Glycolipid Interactions Using Glycomicelles and CaR-ESI-MS.

    Science.gov (United States)

    Han, Ling; Kitova, Elena N; Klassen, John S

    2016-11-01

    This study reports on the use of the catch-and-release electrospray ionization mass spectrometry (CaR-ESI-MS) assay, combined with glycomicelles, as a method for detecting specific interactions between water-soluble proteins and glycolipids (GLs) in aqueous solution. The B subunit homopentamers of cholera toxin (CTB 5 ) and Shiga toxin type 1 B (Stx1B 5 ) and the gangliosides GM1, GM2, GM3, GD1a, GD1b, GT1b, and GD2 served as model systems for this study. The CTB 5 exhibits broad specificity for gangliosides and binds to GM1, GM2, GM3, GD1a, GD1b, and GT1b; Stx1B 5 does not recognize gangliosides. The CaR-ESI-MS assay was used to analyze solutions of CTB 5 or Stx1B 5 and individual gangliosides (GM1, GM2, GM3, GD1a, GD1b, GT1b, and GD2) or mixtures thereof. The high affinity interaction of CTB 5 with GM1 was successfully detected. However, the apparent affinity, as determined from the mass spectra, is significantly lower than that of the corresponding pentasaccharide or when GM1 is presented in model membranes such as nanodiscs. Interactions between CTB 5 and the low affinity gangliosides GD1a, GD1b, and GT1b, as well as GD2, which served as a negative control, were detected; no binding of CTB 5 to GM2 or GM3 was observed. The CaR-ESI-MS results obtained for Stx1B 5 reveal that nonspecific protein-ganglioside binding can occur during the ESI process, although the extent of binding varies between gangliosides. Consequently, interactions detected for CTB 5 with GD1a, GD1b, and GT1b are likely nonspecific in origin. Taken together, these results reveal that the CaR-ESI-MS/glycomicelle approach for detecting protein-GL interactions is prone to false positives and false negatives and must be used with caution. Graphical Abstract GRAPHICAL ABSTRACT TEXT HERE] -->.

  5. Characterization of foot-and-mouth disease virus's viral peptides with LC-ESI-MS

    International Nuclear Information System (INIS)

    Pzdemir, Z.O.; Bulut, E.K.; Mustafeva, Z.; Karahan, M.

    2010-01-01

    Peptides and proteins play a central role in numerous biological and physiological processes in living organisms. Viral capsid peptides are part of the viruses' outer shell of genetic materials. Viruses are recognized by immune system via capsid peptides. Depending on this property of capsid peptides, prototypes synthetic peptide-based vaccine can be developed. In this work, we synthesized three different viral peptide sequences of foot-and-mouth disease virus with microwave enhanced solid phase synthesis method. These peptides were characterized by using liquid chromatography electro spray interface mass spectrometry (LC-ESI-MS) with electro spray ionization. We briefly describe the essential facts for peptide characterization. (author)

  6. Simultaneous quantification of the organophosphorus pesticides dimethoate and omethoate in porcine plasma and urine by LC-ESI-MS/MS and flow-injection-ESI-MS/MS.

    Science.gov (United States)

    John, Harald; Eddleston, Michael; Clutton, R Eddie; Worek, Franz; Thiermann, Horst

    2010-05-15

    Dimethoate is an organophosphorus toxicant used in agri- and horticulture as a systemic broad-spectrum insecticide. It also exhibits toxic activity towards mammalian organism provoked by catalytic desulfuration in the liver producing its oxon-derivative omethoate thus inhibiting acetylcholinesterase, initiating cholinergic crisis and ultimately leading to death by respiratory paralysis and cardiovascular collapse. Pharmaco- and toxicokinetic studies in animal models help to broaden basic understanding of medical intervention by antidotes and supportive care. Therefore, we developed and validated a LC-ESI-MS/MS method suitable for the simultaneous, selective, precise (RSD(intra-day) 1-8%; RSD(inter-day) 5-14%), accurate (intra-day: 95-107%; inter-day: 90-115%), and robust quantification of both pesticides from porcine urine and plasma after deproteinization by precipitation and extensive dilution (1:11,250 for plasma and 1:40,000 for urine). Accordingly, lower limits of quantification (0.24-0.49 microg/ml plasma and 0.78-1.56 microg/ml urine) and lower limits of detection (0.12-0.24 microg/ml plasma and 0.39-0.78 microg/ml urine) were equivalent to quite low absolute on-column amounts (1.1-2.1 pg for plasma and 2.0-3.9 pg for urine). The calibration range (0.24-250 microg/ml plasma and 0.78-200 microg/ml urine) was subdivided into two linear ranges (r(2)>or=0.998) each covering nearly two orders of magnitude. The lack of any interfering peak in 6 individual blank specimens from plasma and urine demonstrated the high selectivity of the method. Furthermore, extensive sample dilution causing lowest concentration of potentially interfering matrix ingredients prompted us to develop and validate an additional flow-injection method (FI-ESI-MS/MS). Validation characteristics were as good as for the chromatographic method but sample throughput was enhanced by a factor of 6. Effects on ionization provoked by plasma and urine matrix from 6 individuals as well as in the

  7. Proanthocyanidin screening by LC-ESI-MS of Portuguese red wines made with teinturier grapes.

    Science.gov (United States)

    Teixeira, Natércia; Azevedo, Joana; Mateus, Nuno; de Freitas, Victor

    2016-01-01

    Proanthocyanidins (PAs) are one of the most important polyphenolic compounds in wine. Among PAs, prodelphinidin (PD) dimers and trimers have not been widely detected in wines due to the lack of available commercial standards and the difficulty to detect and isolate them from natural sources. LC-ESI-MS (liquid chromatography-electrospray ionization-mass spectrometry) with the right chromatographic conditions has proven to be a powerful tool for PAs detection and identification in complex samples. This technique has been applied to an exhaustive study of PA composition of two Portuguese red wines made with teinturier grapes, especially for the identification of PD dimers and trimers. Tandem mass spectrometry (MS/MS) with ion trap provided additional information about the structures of these compounds through the fragmentation patterns of the pseudomolecular ions. A LC-ESI-MS method was optimized and 41 different compounds were found. Among them are included 8 PD dimers and 13 PD trimers. Copyright © 2015 Elsevier Ltd. All rights reserved.

  8. ANALYSIS OF SULFONATES IN AQUEOUS SAMPLES BY ION-PAIR LC/ESI-MS/MS WITH IN-SOURCE CID FOR ADDUCT PEAK ELIMINATION

    Energy Technology Data Exchange (ETDEWEB)

    OUYANG,S.; VAIRAVAMURTHY,M.A.

    1999-06-13

    Determination of low-molecular-weight organic sulfonates (e.g. taurine and cysteic acid) in aqueous solutions is important in many applications of biological, environmental and pharmaceutical sciences. These compounds are difficult to be determined by commonly used reversed-phase liquid chromatographic separation combined with UV-Visible detection because of their high solubility and the lack chromophoric moieties. Here the authors report a method combining ion-pair liquid chromatography and electrospray ionization tandem mass spectrometry (IPLC/ESI-MS/MS)for determining sulfonates. The ability of low-molecular-weight sulfonates to form ion-pairs with quaternary ammonium cations in aqueous solutions allowed LC separation with a C{sub 18} column. Detection of the sulfonates was accomplished with ESI-MS that lends a universal mode of mass detection for polar, water soluble compounds. An in-source collision induced dissociation (CID) was applied to eliminate the adduct peaks in mass spectra. Characteristic marker ions showed in the second stage mass spectra lent a method for identifying sulfonates.

  9. A novel multidimensional protein identification technology approach combining protein size exclusion prefractionation, peptide zwitterion-ion hydrophilic interaction chromatography, and nano-ultraperformance RP chromatography/nESI-MS2 for the in-depth analysis of the serum proteome and phosphoproteome: application to clinical sera derived from humans with benign prostate hyperplasia.

    Science.gov (United States)

    Garbis, Spiros D; Roumeliotis, Theodoros I; Tyritzis, Stavros I; Zorpas, Kostas M; Pavlakis, Kitty; Constantinides, Constantinos A

    2011-02-01

    was made with the proteomes resulting from the immunodepletion of the high abundant albumin and IgG proteins with offline first dimensional tryptic peptide separation with both ZIC-HILIC and strong cation exchange (SCX) chromatography and their subsequent online RP-nUPLC-nESI-MS(2) analysis.

  10. Measurement of methionine level with the LC-ESI-MS/MS method in schizophrenic patients.

    Science.gov (United States)

    Kulaksizoglu, S; Kulaksizoglu, B; Ellidag, H Y; Eren, E; Yilmaz, N; Baykal, A

    2016-01-01

    The purpose of this study was to evaluate plasma methionine levels by using liquid chromatography electrospray ionization-tandem mass spectroscopy (LC-ESI-MS/MS) in schizophrenic patients. A twelve-point standard graph was drawn, and the recovery rate, the intra-day and inter-day coefficients of variation (CV), the limit of detection (LOD), and the limit of quantification (LOQ) were evaluated. The y and R2 values of the standard graph equation were determined as 0.011x + 0.0179 and 0.9989, respectively, and the graph remained linear until the 200 µmol/l level. The intra-day coefficients of variation of the samples (n = 10) containing 8, 28, and 58 µmol/l methionine were determined as 2.68, 3.10, and 3.79%, respectively; while their inter-day coefficients of variation were determined as 2.98, 3.19, and 3.84%. The LOD and LOQ values were determined as 0.04 and 0.1 µmol/l, respectively, while the mean recovery rates were determined as 101.7 and 99.3%. Plasma methionine values were measured as 21.5 (19.5-24,6) µmol/l for the patient group, 17.8 (16.3-20.1) µmol/l for the control group, and the difference between the two groups was statistically significant (p = 0.03). LC-ESI-MS/MS method represents a fairly sensitive, economic, and rapid analysis that requires very little sample and is suitable for measuring methionine levels in schizophrenic patients.

  11. In vivo Phosphoproteome of Human Skeletal Muscle Revealed by Phosphopeptide Enrichment and HPLC-ESI-MS/MS

    DEFF Research Database (Denmark)

    Højlund, Kurt; Bowen, Benjamin P; Hwang, Hyonson

    2009-01-01

    volunteers. Trypsin digestion of 3-5 mg human skeletal muscle protein was followed by phosphopeptide enrichment using SCX and TiO2. The resulting phosphopeptides were analyzed by HPLC-ESI-MS/MS. Using this unbiased approach, we identified 306 distinct in vivo phosphorylation sites in 127 proteins, including...

  12. Simultaneous quantitation of sphingoid bases by UPLC-ESI-MS/MS with identical (13)C-encoded internal standards

    NARCIS (Netherlands)

    Mirzaian, M.; Wisse, P.; Ferraz, M. J.; Marques, A. R. A.; Gaspar, P.; Oussoren, S. V.; Kytidou, K.; Codée, J. D. C.; van der Marel, G.; Overkleeft, H. S.; Aerts, J. M.

    2017-01-01

    Free sphingoid bases (lysosphingolipids) of primary storage sphingolipids are increased in tissues and plasma of several sphingolipidoses. As shown earlier by us, sphingoid bases can be accurately quantified using UPLC-ESI-MS/MS, particularly in combination with identical (13)C-encoded internal

  13. Analysis of peptide mixtures for proteomics research using LC–ESI-MS with a simple microgradient device

    Czech Academy of Sciences Publication Activity Database

    Lenobel, R.; Řehulková, H.; Šebela, M.; Franc, V.; Kahle, Vladislav; Moravcová, Dana; Řehulka, P.

    2015-01-01

    Roč. 33, č. 6 (2015), s. 420-428 ISSN 1527-5949 R&D Projects: GA MV VG20112015021 Institutional support: RVO:68081715 Keywords : LC-ESI-MS * proteomics * peptide Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 0.519, year: 2014 http://hdl.handle.net/11104/0249120

  14. Selenium speciation analysis of Misgurnus anguillicaudatus selenoprotein by HPLC-ICP-MS and HPLC-ESI-MS/MS

    Science.gov (United States)

    Analytical methods for selenium (Se) speciation were developed using high performance liquid chromatography (HPLC) coupled to either inductively coupled plasma mass spectrometry (ICP-MS) or electrospray ionization tandem mass spectrometry (ESI-MS/MS). Separations of selenomethionine (Se-Met) and sel...

  15. Substitution pattern elucidation of hydroxypropyl Pinus pinaster (Ait.) bark polyflavonoid derivatives by ESI(-)-MS/MS.

    Science.gov (United States)

    García Marrero, Danny E; Glasser, Wolfgang G; Pizzi, Antonio; Paczkowski, Sebastian; Laborie, Marie-Pierre G

    2014-10-01

    The structure of condensed tannins (CTs) from Pinus pinaster bark extract and their hydroxypropylated derivatives with four degrees of substitution (DS 1, 2, 3 and 4) has been characterized for the first time using negative-ion mode electrospray ionization tandem mass spectrometry (ESI(-)-MS/MS). The results showed that P. pinaster bark CTs possess structural homogeneity in terms of monomeric units (C(15), catechin). The oligomer sizes were detected to be dimers to heptamers. The derivatives showed typical phenyl-propyl ether mass fragmentation by substituent elimination (58 amu) and inherent C(15) flavonoid fissions. The relative abundance of the product ions revealed a preferential triple, tetra-/penta- and octa- hydroxypropylation substitution pattern in the monomer, dimer and trimer derivatives, respectively. A defined order of -OH reactivity towards propylene oxide was established by means of multistage experiments (A-ring ≥ B-ring > C-ring). A high structural heterogeneity of the modified oligomers was detected. Copyright © 2014 John Wiley & Sons, Ltd.

  16. HPLC-DAD-ESI-MS Analysis of Flavonoids from Leaves of Different Cultivars of Sweet Osmanthus.

    Science.gov (United States)

    Wang, Yiguang; Fu, Jianxin; Zhang, Chao; Zhao, Hongbo

    2016-09-14

    Osmanthus fragrans Lour. has traditionally been a popular ornamental plant in China. In this study, ethanol extracts of the leaves of four cultivar groups of O. fragrans were analyzed by high-performance liquid chromatography coupled with diode array detection (HPLC-DAD) and high-performance liquid chromatography with electrospray ionization and mass spectrometry (HPLC-ESI-MS). The results suggest that variation in flavonoids among O. fragrans cultivars is quantitative, rather than qualitative. Fifteen components were detected and separated, among which, the structures of 11 flavonoids and two coumarins were identified or tentatively identified. According to principal component analysis (PCA) and hierarchical cluster analysis (HCA) based on the abundance of these components (expressed as rutin equivalents), 22 selected cultivars were classified into four clusters. The seven cultivars from Cluster III ('Xiaoye Sugui', 'Boye Jingui', 'Wuyi Dangui', 'Yingye Dangui', 'Danzhuang', 'Foding Zhu', and 'Tianxiang Taige'), which are enriched in rutin and total flavonoids, and 'Sijigui' from Cluster II which contained the highest amounts of kaempferol glycosides and apigenin 7-O-glucoside, could be selected as potential pharmaceutical resources. However, the chemotaxonomy in this paper does not correlate with the distribution of the existing cultivar groups, demonstrating that the distribution of flavonoids in O. fragrans leaves does not provide an effective means of classification for O. fragrans cultivars based on flower color.

  17. Determination of the major phenolic compounds in pomegranate juices by HPLC−DAD−ESI-MS.

    Science.gov (United States)

    Gómez-Caravaca, Ana María; Verardo, Vito; Toselli, Moreno; Segura-Carretero, Antonio; Fernández-Gutiérrez, Alberto; Caboni, Maria Fiorenza

    2013-06-05

    Traditionally, pomegranate (Punica granatum L.) has been consumed as fresh fruit or as pomegranate juice. In this study, the main phenolic compounds of 12 pomegranate varieties and 5 pomegranate clones were determined by HPLC−DAD−ESI-MS. Two chromatographic methods with a fused-core C18 column and a classical HPLC system were developed. Thirteen anthocyanins and fourteen other phenolic compounds were determined in the pomegranate juices. As far as we are concerned, a new flavonol-glycoside, phellatin or its isomer amurensin, has been tentatively identified for the first time in pomegranate juices. Total phenolic content ranged from 580.8 to 2551.3 mg/L of pomegranate juice. Anthocyanins varied between 20 to 82% of total phenolic content. Flavonoids were 1.6-23.6% of total phenolic compounds, while phenolic acids and ellagitannins were in the range 16.4-65.8%. The five clones reported a phenolic content comparable with that of the other pomegranate samples.

  18. Sensitivity of GC-EI/MS, GC-EI/MS/MS, LC-ESI/MS/MS, LC-Ag(+) CIS/MS/MS, and GC-ESI/MS/MS for analysis of anabolic steroids in doping control.

    Science.gov (United States)

    Cha, Eunju; Kim, Sohee; Kim, Ho Jun; Lee, Kang Mi; Kim, Ki Hun; Kwon, Oh-Seung; Lee, Jaeick

    2015-01-01

    This study compared the sensitivity of various separation and ionization methods, including gas chromatography with an electron ionization source (GC-EI), liquid chromatography with an electrospray ionization source (LC-ESI), and liquid chromatography with a silver ion coordination ion spray source (LC-Ag(+) CIS), coupled to a mass spectrometer (MS) for steroid analysis. Chromatographic conditions, mass spectrometric transitions, and ion source parameters were optimized. The majority of steroids in GC-EI/MS/MS and LC-Ag(+) CIS/MS/MS analysis showed higher sensitivities than those obtained with other analytical methods. The limits of detection (LODs) of 65 steroids by GC-EI/MS/MS, 68 steroids by LC-Ag(+) CIS/MS/MS, 56 steroids by GC-EI/MS, 54 steroids by LC-ESI/MS/MS, and 27 steroids by GC-ESI/MS/MS were below cut-off value of 2.0 ng/mL. LODs of steroids that formed protonated ions in LC-ESI/MS/MS analysis were all lower than the cut-off value. Several steroids such as unconjugated C3-hydroxyl with C17-hydroxyl structure showed higher sensitivities in GC-EI/MS/MS analysis relative to those obtained using the LC-based methods. The steroids containing 4, 9, 11-triene structures showed relatively poor sensitivities in GC-EI/MS and GC-ESI/MS/MS analysis. The results of this study provide information that may be useful for selecting suitable analytical methods for confirmatory analysis of steroids. Copyright © 2015 John Wiley & Sons, Ltd.

  19. Unambiguous metabolite identification in high-throughput metabolomics by hybrid 1D 1 H NMR/ESI MS 1 approach: Hybrid 1D 1 H NMR/ESI MS 1 metabolomics method

    Energy Technology Data Exchange (ETDEWEB)

    Walker, Lawrence R. [Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, Richland WA 99354 USA; Hoyt, David W. [Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, Richland WA 99354 USA; Walker, S. Michael [Department of Ecology and Evolutionary Biology, University of Kansas, Lawrence KS 66045 USA; Ward, Joy K. [Department of Ecology and Evolutionary Biology, University of Kansas, Lawrence KS 66045 USA; Nicora, Carrie D. [Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, Richland WA 99354 USA; Bingol, Kerem [Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, Richland WA 99354 USA

    2016-09-16

    We present a novel approach to improve accuracy of metabolite identification by combining direct infusion ESI MS1 with 1D 1H NMR spectroscopy. The new approach first applies standard 1D 1H NMR metabolite identification protocol by matching the chemical shift, J-coupling and intensity information of experimental NMR signals against the NMR signals of standard metabolites in metabolomics library. This generates a list of candidate metabolites. The list contains false positive and ambiguous identifications. Next, we constrained the list with the chemical formulas derived from high-resolution direct infusion ESI MS1 spectrum of the same sample. Detection of the signals of a metabolite both in NMR and MS significantly improves the confidence of identification and eliminates false positive identification. 1D 1H NMR and direct infusion ESI MS1 spectra of a sample can be acquired in parallel in several minutes. This is highly beneficial for rapid and accurate screening of hundreds of samples in high-throughput metabolomics studies. In order to make this approach practical, we developed a software tool, which is integrated to Chenomx NMR Suite. The approach is demonstrated on a model mixture, tomato and Arabidopsis thaliana metabolite extracts, and human urine.

  20. Dependence of matrix effect on ionization polarity during LC-ESI-MS analysis of derivatized amino acids in some natural samples.

    Science.gov (United States)

    Oldekop, Maarja-Liisa; Rebane, Riin; Herodes, Koit

    2017-10-01

    Matrix effect, the influence of co-eluting components on the ionization efficiency of the analyte, affects the trueness and precision of the LC-ESI-MS analysis. Derivatization can reduce or eliminate matrix effect, for example, diethyl ethoxymethylenemalonate (DEEMM) derivatives have shown less matrix effect compared to other derivatives. Moreover, the use of negative ion mode can further reduce matrix effect. In order to investigate the combination of derivatization and different ionization modes, an LC-ESI-MS/MS method using alternating positive/negative ion mode was developed and validated. The analyses in positive and negative ion modes had comparable limit of quantitation values. The influence of ESI polarity on matrix effect was investigated during the analysis of 22 DEEMM-derivatized amino acids in herbal extracts and honeys. Sample dilution approach was used for the evaluation of the presence of matrix effect. Altogether, 4 honeys and 11 herbal extracts were analyzed, and the concentrations of 22 amino acids in the samples are presented. In the positive ion mode, matrix effect was observed for several amino acid derivatives and the matrix effect was stronger in honey samples compared to the herbal extracts. The negative ion mode was free from matrix effect, with only few exceptions in honeys (average relative standard deviation over all analytes and matrices was 8%; SD = 7%). The matrix effect was eliminated in the positive ion mode by sample dilution and agreement between concentrations from the two ion modes was achieved for most amino acids. In conclusion, it was shown that the combination of derivatization and negative ion mode can be a powerful tool for minimizing matrix effect in more complicated applications.

  1. Measurement of O(6)-alkylguanine-DNA alkyltransferase activity in tumour cells using stable isotope dilution HPLC-ESI-MS/MS.

    Science.gov (United States)

    Sun, Guohui; Zhao, Lijiao; Fan, Tengjiao; Ren, Ting; Zhong, Rugang

    2016-10-15

    The repair of DNA mediated by O(6)-alkylguanine-DNA alkyltransferase (AGT) provides protection against DNA damage from endogenous or exogenous alkylation of the O(6) position of guanine. However, this repair acts as a double-edged sword in cancer treatment, as it not only protects normal cells from chemotherapy-associated toxicities, but also results in cancer cell resistance to guanine O(6)-alkylating antitumour agents. Thus, AGT plays an important role in predicting the individual susceptibility to guanine O(6)-alkylating carcinogens and chemotherapies. Accordingly, it is necessary to establish a quantitative method for determining AGT activity with high accuracy, sensitivity and practicality. Here, we describe a novel nonradioactive method for measuring AGT activity using stable isotope dilution high-performance liquid chromatography electrospray ionization tandem mass spectrometry (HPLC-ESI-MS/MS). This method is based on the irreversibility of the removal of the O(6)-alkyl group from guanine by AGT and on the high affinity of O(6)-benzylguanine (O(6)-BG) as an AGT substrate. HPLC-ESI-MS/MS was used to measure the AGT activities in cell protein extracts from eight tumour lines, demonstrating that AGT activity was quite variable among different cell lines, ranging from nondetectable to 1021 fmol/mg protein. The experiments performed in intact tumour cells yielded similar results but exhibited slightly higher activities than those observed in cell protein extracts. The accuracy of this method was confirmed by an examination of AGT expression levels using western blotting analysis. To our knowledge, this method is the first mass spectrometry-based AGT activity assay, and will likely provide assistance in the screening of cancer risk or the application of chemotherapies. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Quantitation of iothalamate in urine and plasma using liquid chromatography electrospray tandem mass spectrometry (HPLC-ESI-MS/MS).

    Science.gov (United States)

    Molinaro, Ross J; Ritchie, James C

    2010-01-01

    The following chapter describes a method to measure iothalamate in plasma and urine samples using high performance liquid chromatography combined with electrospray positive ionization tandem mass spectrometry (HPLC-ESI-MS/MS). Methanol and water are spiked with the internal standard (IS) iohexol. Iothalamate is isolated from plasma after IS spiked methanol extraction and from urine by IS spiked water addition and quick-spin filtration. The plasma extractions are dried under a stream of nitrogen. The residue is reconstituted in ammonium acetate-formic acid-water. The reconstituted plasma and filtered urine are injected into the HPLC-ESI-MS/MS. Iothalamate and iohexol show similar retention times in plasma and urine. Quantification of iothalamate in the samples is made by multiple reaction monitoring using the hydrogen adduct mass transitions, from a five-point calibration curve.

  3. HPLC-DAD-ESI/MS Identification of Light Harvesting and Light Screening Pigments in the Lake Sediments at Edmonson Point

    OpenAIRE

    Giovannetti, Rita; Alibabaei, Leila; Zannotti, Marco; Ferraro, Stefano; Petetta, Laura

    2013-01-01

    The composition of sedimentary pigments in the Antarctic lake at Edmonson Point has been investigated and compared with the aim to provide a useful analytical method for pigments separation and identification, providing reference data for future assessment of possible changes in environmental conditions. Reversed phase high performance liquid chromatography (HPLC) with electrospray-mass spectrometry (ESI-MS) detection and diode array detection (DAD) has been used to identify light screeni...

  4. Profiling the Oxylipin and Endocannabinoid Metabolome by UPLC-ESI-MS/MS in Human Plasma to Monitor Postprandial Inflammation.

    Science.gov (United States)

    Gouveia-Figueira, Sandra; Späth, Jana; Zivkovic, Angela M; Nording, Malin L

    2015-01-01

    Bioactive lipids, including oxylipins, endocannabinoids, and related compounds may function as specific biochemical markers of certain aspects of inflammation. However, the postprandial responsiveness of these compounds is largely unknown; therefore, changes in the circulating oxylipin and endocannabinoid metabolome in response to a challenge meal were investigated at six occasions in a subject who freely modified her usual diet. The dietary change, and especially the challenge meal itself, represented a modification of precursor fatty acid status, with expectedly subtle effects on bioactive lipid levels. To detect even the slightest alteration, highly sensitive ultra-performance liquid chromatography (UPLC) coupled to electrospray ionization (ESI) tandem mass spectrometry (MS/MS) methods for bioactive lipid profiling was employed. A previously validated UPLC-ESI-MS/MS method for profiling the endocannabinoid metabolome was used, while validation of an UPLC-ESI-MS/MS method for oxylipin analysis was performed with acceptable outcomes for a majority of the parameters according to the US Food and Drug Administration guidelines for linearity (0.9938 metabolome, caused by changes in diet and ii) responsiveness to a challenge meal for a subset of the oxylipin and endocannabinoid metabolome. To summarize, we have shown proof-of-concept of our UPLC-ESI-MS/MS bioactive lipid protocols for the purpose of monitoring subtle shifts, and thereby useful to address lipid-mediated postprandial inflammation.

  5. Quantum-chemical, NMR, FT IR, and ESI MS studies of complexes of colchicine with Zn(II).

    Science.gov (United States)

    Jankowski, Wojciech; Kurek, Joanna; Barczyński, Piotr; Hoffmann, Marcin

    2017-04-01

    Colchicine is a tropolone alkaloid from Colchicinum autumnale. It shows antifibrotic, antimitotic, and anti-inflammatory activities, and is used to treat gout and Mediterranean fever. In this work, complexes of colchicine with zinc(II) nitrate were synthesized and investigated using DFT, 1 H and 13 C NMR, FT IR, and ESI MS. The counterpoise-corrected and uncorrected interaction energies of these complexes were calculated. We also calculated their 1 H, 13 C NMR, and IR spectra and compared them with the corresponding experimentally obtained data. According to the ESI MS mass spectra, colchicine forms stable complexes with zinc(II) nitrate that have various stoichiometries: 2:1, 1:1:1, and 2:1:1 with respect to colchichine, Zn(II), and nitrate ion. All of the complexes were investigated using the quantum theory of atoms in molecules (QTAIM). The calculated and the measured spectra showed differences before and after the complexation process. Calculated electron densities and bond critical points indicated the presence of bonds between the ligands and the central cation in the investigated complexes that satisfied the quantum theory of atoms in molecules. Graphical Abstract DFT, NMR, FT IR, ESI MS, QTAIM and puckering studies of complexes of colchicine with Zn(II).

  6. Characterization of the Proteome of Theobroma cacao Beans by Nano-UHPLC-ESI MS/MS.

    Science.gov (United States)

    Scollo, Emanuele; Neville, David; Oruna-Concha, M Jose; Trotin, Martine; Cramer, Rainer

    2018-02-01

    Cocoa seed storage proteins play an important role in flavour development as aroma precursors are formed from their degradation during fermentation. Major proteins in the beans of Theobroma cacao are the storage proteins belonging to the vicilin and albumin classes. Although both these classes of proteins have been extensively characterized, there is still limited information on the expression and abundance of other proteins present in cocoa beans. This work is the first attempt to characterize the whole cocoa bean proteome by nano-UHPLC-ESI MS/MS analysis using tryptic digests of cocoa bean protein extracts. The results of this analysis show that >1000 proteins could be identified using a species-specific Theobroma cacao database. The majority of the identified proteins were involved with metabolism and energy. Additionally, a significant number of the identified proteins were linked to protein synthesis and processing. Several proteins were also involved with plant response to stress conditions and defence. Albumin and vicilin storage proteins showed the highest intensity values among all detected proteins, although only seven entries were identified as storage proteins. A comparison of MS/MS data searches carried out against larger non-specific databases confirmed that using a species-specific database can increase the number of identified proteins, and at the same time reduce the number of false positives. The results of this work will be useful in developing tools that can allow the comparison of the proteomic profile of cocoa beans from different genotypes and geographic origins. Data are available via ProteomeXchange with identifier PXD005586. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Separation and identification of Se-methylselenogalactosamine - a new metabolite in basal human urine - by HPLC-ICP-MS and CE-nano-ESI-(MS)(2)

    DEFF Research Database (Denmark)

    Bendahl, L.; Gammelgaard, Bente

    2004-01-01

    Three minor metabolites were isolated from human urine. Two of these were identified by nano electrospray ionisation mass spectrometry (nESI-MS) as Se-methylseleno-N-acetylglucosamine and Se-methylselenogalactosamine, respectively. A human urine pool was lyophilised and reconstituted in methanol......-chromatographed in the reversed phase system and further purified in different separation systems before analysis by nESI-MS. By CE-nESI-MS analysis of one of the fractions, the characteristic selenium pattern was recognized around m/z 285 and ( MS) 2 fragmentation resulted in a fragments at m/z 267, 173 and 155, respectively....... It was not possible to identify this selenium compound on basis of the available data. The selenium compound in the second fraction showed co-elution with a Se-methylseleno-N-acetylglucosamine standard. The identity of this compound was verified by nESI-MS after further purification by size exclusion chromatography...

  8. An analytical approach based on ESI-MS, LC-MS and PCA for the quali-quantitative analysis of cycloartane derivatives in Astragalus spp.

    Science.gov (United States)

    Napolitano, Assunta; Akay, Seref; Mari, Angela; Bedir, Erdal; Pizza, Cosimo; Piacente, Sonia

    2013-11-01

    Astragalus species are widely used as health foods and dietary supplements, as well as drugs in traditional medicine. To rapidly evaluate metabolite similarities and differences among the EtOH extracts of the roots of eight commercial Astragalus spp., an approach based on direct analyses by ESI-MS followed by PCA of ESI-MS data, was carried out. Successively, quali-quantitative analyses of cycloartane derivatives in the eight Astragalus spp. by LC-ESI-MS(n) and PCA of LC-ESI-MS data were performed. This approach allowed to promptly highlighting metabolite similarities and differences among the various Astragalus spp. PCA results from LC-ESI-MS data of Astragalus samples were in reasonable agreement with both PCA results of ESI-MS data and quantitative results. This study affords an analytical method for the quali-quantitative determination of cycloartane derivatives in herbal preparations used as health and food supplements. Copyright © 2013 Elsevier B.V. All rights reserved.

  9. Chemical characterisation of non-defective and defective green arabica and robusta coffees by electrospray ionization-mass spectrometry (ESI-MS).

    Science.gov (United States)

    Mendonça, Juliana C F; Franca, Adriana S; Oliveira, Leandro S; Nunes, Marcella

    2008-11-15

    The coffee roasted in Brazil is considered to be of low quality, due to the presence of defective coffee beans that depreciate the beverage quality. These beans, although being separated from the non-defective ones prior to roasting, are still commercialized in the coffee trading market. Thus, it was the aim of this work to verify the feasibility of employing ESI-MS to identify chemical characteristics that will allow the discrimination of Arabica and Robusta species and also of defective and non-defective coffees. Aqueous extracts of green (raw) defective and non-defective coffee beans were analyzed by direct infusion electrospray ionization mass spectrometry (ESI-MS) and this technique provided characteristic fingerprinting mass spectra that not only allowed for discrimination of species but also between defective and non-defective coffee beans. ESI-MS profiles in the positive mode (ESI(+)-MS) provided separation between defective and non-defective coffees within a given species, whereas ESI-MS profiles in the negative mode (ESI(-)-MS) provided separation between Arabica and Robusta coffees. Copyright © 2008 Elsevier Ltd. All rights reserved.

  10. Europium, uranyl, and thorium-phenanthroline amide complexes in acetonitrile solution: an ESI-MS and DFT combined investigation.

    Science.gov (United States)

    Xiao, Cheng-Liang; Wang, Cong-Zhi; Mei, Lei; Zhang, Xin-Rui; Wall, Nathalie; Zhao, Yu-Liang; Chai, Zhi-Fang; Shi, Wei-Qun

    2015-08-28

    The tetradentate N,N'-diethyl-N,N'-ditolyl-2,9-diamide-1,10-phenanthroline (Et-Tol-DAPhen) ligand with hard-soft donor atoms has been demonstrated to be promising for the group separation of actinides from highly acidic nuclear wastes. To identify the formed complexes of this ligand with actinides and lanthanides, electrospray ionization mass spectrometry (ESI-MS) combined with density functional theory (DFT) calculations was used to probe the possible complexation processes. The 1 : 2 Eu-L species ([EuL2(NO3)](2+)) can be observed in ESI-MS at low metal-to-ligand ([M]/[L]) ratios, whereas the 1 : 1 Eu-L species ([EuL(NO3)2](+)) can be observed when the [M]/[L] ratio is higher than 1.0. However, ([UO2L(NO3)](+)) is the only detected species for the uranyl complexes. The [ThL2(NO3)2](2+) species can be observed at low [M]/[L] ratios; the 1 : 2 species ([ThL2(NO3)](3+)) and a new 1 : 1 species ([ThL(NO3)3](+)) can be detected at high [M]/[L] ratios. Collision-induced dissociation (CID) results showed that Et-Tol-DAPhen ligands can coordinate strongly with metal ions, and the coordination moieties remain intact under CID conditions. Natural bond orbital (NBO), molecular electrostatic potential (MEP), electron localization function (ELF), atoms in molecules (AIM) and molecular orbital (MO) analyses indicated that the metal-ligand bonds of the actinide complexes exhibited more covalent character than those of the lanthanide complexes. In addition, according to thermodynamic analysis, the stable cationic M-L complexes in acetonitrile are found to be in good agreement with the ESI-MS results.

  11. HPLC-ESI-MS/MS analysis of oxidized di-caffeoylquinic acids generated by metalloporphyrin-catalyzed reactions

    Directory of Open Access Journals (Sweden)

    Michel D. Santos

    2008-01-01

    Full Text Available This paper reports an HPLC-ESI-MS/MS investigation on the oxidation of 3,5- and 4,5- dicaffeoylquinic acid using iron(III tetraphenylporphyrin chloride as catalyst. Two major mono-oxidised products of the quinic acid moiety have been identified for both compounds. However, only the 4,5-derivative afforded two different tri-oxo products. Thus, it seems that the oxidation pattern depends on the number and positions of the caffeic acid moieties present in caffeoylquinic acid molecules.

  12. HPLC-ESI-MS/MS analysis of oxidized di-caffeoylquinic acids generated by metalloporphyrin-catalyzed reactions

    International Nuclear Information System (INIS)

    Santos, Michel D.; Lopes, Norberto P.; Iamamoto, Yassuko

    2008-01-01

    This paper reports an HPLC-ESI-MS/MS investigation on the oxidation of 3,5- and 4,5- dicaffeoylquinic acid using iron(III) tetraphenylporphyrin chloride as catalyst. Two major mono-oxidised products of the quinic acid moiety have been identified for both compounds. However, only the 4,5-derivative afforded two different tri-oxo products. Thus, it seems that the oxidation pattern depends on the number and positions of the caffeic acid moieties present in caffeoylquinic acid molecules. (author)

  13. HPLC-ESI-MS/MS analysis of oxidized di-caffeoylquinic acids generated by metalloporphyrin-catalyzed reactions

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Michel D.; Lopes, Norberto P. [Universidade de Sao Paulo (USP), Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas. Dept. de Fisica e Quimica]. E-mail: npelopes@fcfrp.usp.br; Iamamoto, Yassuko [Universidade de Sao Paulo (USP), Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas. Dept. de Quimica

    2008-07-01

    This paper reports an HPLC-ESI-MS/MS investigation on the oxidation of 3,5- and 4,5- dicaffeoylquinic acid using iron(III) tetraphenylporphyrin chloride as catalyst. Two major mono-oxidised products of the quinic acid moiety have been identified for both compounds. However, only the 4,5-derivative afforded two different tri-oxo products. Thus, it seems that the oxidation pattern depends on the number and positions of the caffeic acid moieties present in caffeoylquinic acid molecules. (author)

  14. HPLC-DAD-ESI/MS identification of light harvesting and light screening pigments in the lake sediments at Edmonson Point.

    Science.gov (United States)

    Giovannetti, Rita; Alibabaei, Leila; Zannotti, Marco; Ferraro, Stefano; Petetta, Laura

    2013-01-01

    The composition of sedimentary pigments in the Antarctic lake at Edmonson Point has been investigated and compared with the aim to provide a useful analytical method for pigments separation and identification, providing reference data for future assessment of possible changes in environmental conditions. Reversed phase high performance liquid chromatography (HPLC) with electrospray-mass spectrometry (ESI-MS) detection and diode array detection (DAD) has been used to identify light screening and light harvesting pigments. The results are discussed in terms of local environmental conditions.

  15. HPLC-DAD-ESI/MS Identification of Light Harvesting and Light Screening Pigments in the Lake Sediments at Edmonson Point

    Directory of Open Access Journals (Sweden)

    Rita Giovannetti

    2013-01-01

    Full Text Available The composition of sedimentary pigments in the Antarctic lake at Edmonson Point has been investigated and compared with the aim to provide a useful analytical method for pigments separation and identification, providing reference data for future assessment of possible changes in environmental conditions. Reversed phase high performance liquid chromatography (HPLC with electrospray-mass spectrometry (ESI-MS detection and diode array detection (DAD has been used to identify light screening and light harvesting pigments. The results are discussed in terms of local environmental conditions.

  16. First characterisation of flavonoid- and diarylheptanoid-type antioxidant phenolics in Corylus maxima by HPLC-DAD-ESI-MS.

    Science.gov (United States)

    Riethmüller, Eszter; Tóth, Gergő; Alberti, Ágnes; Végh, Krisztina; Burlini, Ilaria; Könczöl, Árpád; Balogh, György Tibor; Kéry, Ágnes

    2015-03-25

    Corylus maxima Mill. (Betulaceae) leaves have been used in traditional medicine both internally and externally, nevertheless phytochemical exploration of the plant remains incomplete. In this study, the in vitro antioxidant activity and polyphenolic composition of the ethyl acetate and methanolic extracts of C. maxima leaves and bark are reported for the first time. The radical scavenging activities of the extracts were investigated by the ABTS and DPPH assays. All the extracts of C. maxima possessed notable antioxidant activity. By mean of a HPLC-DAD-ESI-TOF and a HPLC-DAD-ESI-MS/MS method, altogether twenty-two phenolics were tentatively characterised: one flavan derivative (1), seven flavonol derivatives (4, 6, 12, 13, 16, 20 and 21) and fourteen diarylheptanoids (2, 3, 5, 7-11, 14, 15, 17-19 and 22). The amount of the two main flavonoids - myricetin-3-O-rhamnoside (6) and quercetin-3-O-rhamnoside (13) - and two diarylheptanoids - oregonin (3) and hirsutenone (15) - in the extracts were determined by a validated HPLC-ESI-MS/MS method in multiple reaction monitoring (MRM) mode. Our results showed that C. maxima could be considered as a valuable source of pharmacologically important natural products that might contribute to the revaluation of the phytotherapeutical potential of the plant. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. Unambiguous Metabolite Identification in High-Throughput Metabolomics by Hybrid 1H-NMR/ESI-MS1 Approach

    Energy Technology Data Exchange (ETDEWEB)

    2016-10-18

    The invention improves accuracy of metabolite identification by combining direct infusion ESI-MS with one-dimensional 1H-NMR spectroscopy. First, we apply a standard 1H-NMR metabolite identification protocol by matching the chemical shift, J-coupling and intensity information of experimental NMR signals against the NMR signals of standard metabolites in a metabolomics reference libraries. This generates a list of candidate metabolites. The list contains both false positive and ambiguous identifications. The software tool (the invention) takes the list of candidate metabolites, generated from NMRbased metabolite identification, and then calculates, for each of the candidate metabolites, the monoisotopic mass-tocharge (m/z) ratios for each commonly observed ion, fragment and adduct feature. These are then used to assign m/z ratios in experimental ESI-MS spectra of the same sample. Detection of the signals of a given metabolite in both NMR and MS spectra resolves the ambiguities, and therefore, significantly improves the confidence of the identification.

  18. Phenolic Profiling of the South American “Baylahuen” Tea (Haplopappus spp., Asteraceae by HPLC-DAD-ESI-MS

    Directory of Open Access Journals (Sweden)

    Guillermo Schmeda-Hirschmann

    2015-01-01

    Full Text Available The aerial parts of several Haplopappus species (Asteraceae, known under the common name “baylahuen”, are used as herbal teas in Chile and Argentina. In Chile, “baylahuen” comprises H. multifolius, H. taeda, H. baylahuen and H. rigidus. Little is known about the chemical identity of the infusion constituents in spite of widespread consumption. The aim of the present work was the characterization of phenolics occurring in the infusions and methanol extracts of “baylahuen” by HPLC-DAD-ESI-MS. A simple HPLC-DAD-ESI-MS method was developed for the fast identification and differentiation of Haplopappus spp. used as a tea source, based on the phenolics from the tea and methanol extracts. Some 27 phenolics were tentatively identified in the infusions and methanol extract, including 10 caffeoyl quinic and feruloyl quinic acid derivatives and 17 flavonoids. The HPLC patterns of the Haplopappus tea and methanol extract allow a clear differentiation at the species level. The occurrence of hydroxycinnamic acid derivatives and flavonoids can explain the reputed nutraceutical and health beneficial properties of this herbal tea.

  19. Hibiscus sabdariffa L. and Its Bioactive Constituents Exhibit Antiviral Activity against HSV-2 and Anti-enzymatic Properties against Urease by an ESI-MS Based Assay

    Directory of Open Access Journals (Sweden)

    Sherif T. S. Hassan

    2017-04-01

    Full Text Available For decades, Hibiscus sabdariffa L. and its phytochemicals have been shown to possess a wide range of pharmacologic properties. In this study, aqueous extract of Hibiscus sabdariffa (AEHS and its bioactive constituent protocatechuic acid (PCA, have been evaluated in vitro for their antiviral activity against HSV-2 clinical isolates and anti-enzymatic activity against urease. Antiherpetic activity was evaluated by the titer reduction assay in infected Vero cells, and cytotoxicity was evaluated by the neutral red dye-uptake method. Anti-urease activity was determined by a developed Electrospray Ionization-Mass Spectrometry (ESI-MS-based assay. PCA showed potent anti-HSV-2 activity compared with that of acyclovir, with EC50 values of 0.92 and 1.43 µg∙mL−1, respectively, and selectivity indices > 217 and > 140, respectively. For the first time, AEHS was shown to exert anti-urease inhibition activity, with an IC50 value of 82.4 µg∙mL−1. This, combined with its safety, could facilitate its use in practical applications as a natural urease inhibitor. Our results present Hibiscus sabdariffa L. and its bioactive compound PCA as potential therapeutic agents in the treatment of HSV-2 infection and the treatment of diseases caused by urease-producing bacteria.

  20. Hibiscus sabdariffa L. and Its Bioactive Constituents Exhibit Antiviral Activity against HSV-2 and Anti-enzymatic Properties against Urease by an ESI-MS Based Assay.

    Science.gov (United States)

    Hassan, Sherif T S; Švajdlenka, Emil; Berchová-Bímová, Kateřina

    2017-04-30

    For decades, Hibiscus sabdariffa L. and its phytochemicals have been shown to possess a wide range of pharmacologic properties. In this study, aqueous extract of Hibiscus sabdariffa (AEHS) and its bioactive constituent protocatechuic acid (PCA), have been evaluated in vitro for their antiviral activity against HSV-2 clinical isolates and anti-enzymatic activity against urease. Antiherpetic activity was evaluated by the titer reduction assay in infected Vero cells, and cytotoxicity was evaluated by the neutral red dye-uptake method. Anti-urease activity was determined by a developed Electrospray Ionization-Mass Spectrometry (ESI-MS)-based assay. PCA showed potent anti-HSV-2 activity compared with that of acyclovir, with EC 50 values of 0.92 and 1.43 µg∙mL -1 , respectively, and selectivity indices > 217 and > 140, respectively. For the first time, AEHS was shown to exert anti-urease inhibition activity, with an IC 50 value of 82.4 µg∙mL -1 . This, combined with its safety, could facilitate its use in practical applications as a natural urease inhibitor. Our results present Hibiscus sabdariffa L. and its bioactive compound PCA as potential therapeutic agents in the treatment of HSV-2 infection and the treatment of diseases caused by urease-producing bacteria.

  1. The salivary proteome profile in patients affected by SAPHO syndrome characterized by a top-down RP-HPLC-ESI-MS platform.

    Science.gov (United States)

    Sanna, Monica; Firinu, Davide; Manconi, Paolo Emilio; Pisanu, Maria; Murgia, Giuseppe; Piras, Valentina; Castagnola, Massimo; Messana, Irene; del Giacco, Stefano Renato; Cabras, Tiziana

    2015-06-01

    SAPHO syndrome is a rare and often unrecognized disease with prominent inflammatory cutaneous and articular symptoms characterized by musculoskeletal manifestations (synovitis, hyperostosis, osteomyelitis) associated with dermatological conditions (severe acne and pustulosis). The acidic soluble fraction of whole saliva from 10 adult women affected by SAPHO syndrome and from a group of 28 healthy women was analysed by RP-HPLC-ESI-MS with the aim of discovering salivary biomarkers of the disorder. The levels of the oral proteins and peptides were correlated with clinical data. The following proteins showed a significant decreased concentration in saliva of SAPHO subjects with respect to controls: cystatin S1 and SN, histatins, the major acidic PRPs, P-C and P-B peptides. The cystatin SN abundance lowered according to the disease duration and histatins showed positive correlations with the C reactive protein. Statistical analysis performed excluding one patient with a different pattern of salivary proteins/peptides highlighted a positive relationship between cystatin S1, histatins 3, histatin 5, and the neutrophil count. Moreover, histatin 3 correlated positively with the total white cell count and negatively with the erythrocyte sedimentation rate. Levels and frequency of S100A12 protein showed a trend to increase in SAPHO patients. The high expression of this pro-inflammatory protein is probably related to the inflammatory response and to the altered neutrophil responses to functional stimuli that characterize SAPHO syndrome suggesting a possible application as a salivary biomarker.

  2. Use of ESI-MS to determine reaction pathway for hydrogen sulphide scavenging with 1,3,5-tri-(2-hydroxyethyl)-hexahydro-s-triazine

    DEFF Research Database (Denmark)

    Madsen, Henrik Tækker; Søgaard, Erik Gydesen

    2012-01-01

    To study the reaction between hydrogen sulphide and 1,3,5-tri-(2-hydroxyethyl)- hexahydro-s-triazine, which is an often used hydrogen sulphide scavenger, electro spray ionisation mass spectrometry (ESI-MS) was used. The investigation was carried out in positive mode, and tandem mass spectrometry...... the dithiazine species, hereby confirming previously obtained results and showing the ability of the ESI-MS method for studying the scavenging reaction. The final theoretical product s-trithiane was not detected. Furthermore, fragmentation products of thiadiazine and dithiazine were detected in the solution...

  3. Sulphur fertilization influences the sulphur species composition in Allium sativum: sulphomics using HPLC-ICPMS/MS-ESI-MS/MS.

    Science.gov (United States)

    Raab, Andrea; Ronzan, Marilena; Feldmann, Joerg

    2017-10-18

    Garlic (A. sativum) contains a large number of small sulphur (S)-containing metabolites, which are important for its taste and smell and vary with A. sativum variety and growth conditions. This study was designed to investigate the influence of different sulphur-fertilization regimes on low molecular weight S-species by attempting the first sulphur mass balance in A. sativum roots and bulbs using HPLC-ICPMS/MS-ESI-MS/MS. Species unspecific quantification of acid soluble S-containing metabolites was achieved using HPLC-ICP-MS/MS. For identification of the compounds, high resolution ESI-MS (Orbitrap LTQ and q-TOF) was used. The plants contained up to 54 separated sulphur-containing compounds, which constitute about 80% of the total sulphur present in A. sativum. The roots and bulbs of A. sativum contained the same compounds, but not necessarily the same amounts and proportions. The S-containing metabolites in the roots reacted more sensitively to manipulations of sulphur fertilization than those compounds in the bulbs. In addition to known compounds (e.g. γ-glutamyl-S-1-propenylcysteine) we were able to identify and partially quantify 31 compounds. Three as yet undescribed S-containing compounds were also identified and quantified for the first time. Putative structures were assigned to the oxidised forms of S-1-propenylmercaptoglutathione, S-2-propenylmercaptoglutathione, S-allyl/propenyl-containing PC-2 and 2-amino-3-[(2-carboxypropyl)sulfanyl]propanoic acid. The parallel use of ICP-MS/MS as a sulphur-specific detector and ESI-MS as a molecular detector simplifies the identification and quantification of sulphur containing metabolites without species specific standards. This non-target analysis approach enables a mass balance approach and identifies the occurrence of the so far unidentified organosulphur compounds. The experiments showed that the sulphur-fertilization regime does not influence sulphur-speciation, but the concentration of some S

  4. Analysis of perchlorate in foods and beverages by ion chromatography coupled with tandem mass spectrometry (IC-ESI-MS/MS)

    Energy Technology Data Exchange (ETDEWEB)

    El Aribi, Houssain [Applied Biosystems/MDS Sciex, 71 Four Valley Drive, Concord, Ont., L4K 4V8 (Canada)]. E-mail: houssain.aribi@sciex.com; Le Blanc, Yves J.C. [Applied Biosystems/MDS Sciex, 71 Four Valley Drive, Concord, Ont., L4K 4V8 (Canada); Antonsen, Stephen [Dionex Canada Ltd., 1540 Cornwall Road, Oakville, Ont., L6J 7W5 (Canada); Sakuma, Takeo [Applied Biosystems/MDS Sciex, 71 Four Valley Drive, Concord, Ont., L4K 4V8 (Canada)

    2006-05-10

    A new IC-ESI-MS/MS method, with simple sample preparation procedure, has been developed for quantification and confirmation of perchlorate (ClO{sub 4} {sup -}) anions in water, fresh and canned food, wine and beer samples at low part-per-trillion (ng l{sup -1}) levels. To the best of our knowledge, this is the first time an analytical method is used for determination of perchlorate in wine and beer samples. The IC-ESI-MS/MS instrumentation consisted of an ICS-2500 ion chromatography (IC) system coupled to either an API 2000{sup TM} or an API 3200{sup TM} mass spectrometer. The IC-ESI-MS/MS system was optimized to monitor two pairs of precursor and fragment ion transitions, i.e., multiple reaction monitoring (MRM). All samples had oxygen-18 isotope labeled perchlorate internal standard (ISTD) added prior to extraction. Chlorine isotope ratio ({sup 35}Cl/{sup 37}Cl) was used as a confirmation tool. The transition of {sup 35}Cl{sup 16}O{sub 4} {sup -} (m/z 98.9) into {sup 35}Cl{sup 16}O{sub 3} {sup -} (m/z 82.9) was monitored for quantifying the main analyte; the transition of {sup 37}Cl{sup 16}O{sub 4} {sup -} (m/z 100.9) into {sup 37}Cl{sup 16}O{sub 3} {sup -} (m/z 84.9) was monitored for examining a proper isotopic abundance ratio of {sup 35}Cl/{sup 37}Cl; and the transition of {sup 35}Cl{sup 18}O{sub 4} {sup -} (m/z 107.0) into {sup 35}Cl{sup 18}O{sub 3} {sup -} (m/z 89.0) was monitored for quantifying the internal standard. The minimum detection limit (MDL) for this method in de-ionized water is 5 ng l{sup -1} (ppt) using the API 2000{sup TM} mass spectrometer and 0.5 ng l{sup -1} using the API 3200{sup TM} mass spectrometer. Over 350 food and beverage samples were analyzed mostly in triplicate. Except for four, all samples were found to contain measurable amounts of perchlorate. The levels found ranged from 5 ng l{sup -1} to 463.5 {+-} 6.36 {mu}g kg{sup -1} using MRM 98.9 {sup {yields}} 82.9 and 100 {mu}l injection.

  5. Interaction of Pyrrolobenzodiazepine (PBD) Ligands with Parallel Intermolecular G-Quadruplex Complex Using Spectroscopy and ESI-MS

    Science.gov (United States)

    Raju, Gajjela; Srinivas, Ragampeta; Santhosh Reddy, Vangala; Idris, Mohammed M.; Kamal, Ahmed; Nagesh, Narayana

    2012-01-01

    Studies on ligand interaction with quadruplex DNA, and their role in stabilizing the complex at concentration prevailing under physiological condition, has attained high interest. Electrospray ionization mass spectrometry (ESI-MS) and spectroscopic studies in solution were used to evaluate the interaction of PBD and TMPyP4 ligands, stoichiometry and selectivity to G-quadruplex DNA. Two synthetic ligands from PBD family, namely pyrene-linked pyrrolo[2,1-c][1,4]benzodiazepine hybrid (PBD1), mixed imine-amide pyrrolobenzodiazepine dimer (PBD2) and 5,10,15,20-tetrakis(N-methyl-4-pyridyl)porphyrin (TMPyP4) were studied. G-rich single-stranded oligonucleotide d(5′GGGGTTGGGG3′) designated as d(T2G8), from the telomeric region of Tetrahymena Glaucoma, was considered for the interaction with ligands. ESI-MS and spectroscopic methods viz., circular dichroism (CD), UV-Visible, and fluorescence were employed to investigate the G-quadruplex structures formed by d(T2G8) sequence and its interaction with PBD and TMPyP4 ligands. From ESI-MS spectra, it is evident that the majority of quadruplexes exist as d(T2G8)2 and d(T2G8)4 forms possessing two to ten cations in the centre, thereby stabilizing the complex. CD band of PBD1 and PBD2 showed hypo and hyperchromicity, on interaction with quadruplex DNA, indicating unfolding and stabilization of quadruplex DNA complex, respectively. UV-Visible and fluorescence experiments suggest that PBD1 bind externally where as PBD2 intercalate moderately and bind externally to G-quadruplex DNA. Further, melting experiments using SYBR Green indicate that PBD1 unfolds and PBD2 stabilizes the G-quadruplex complex. ITC experiments using d(T2G8) quadruplex with PBD ligands reveal that PBD1 and PBD2 prefer external/loop binding and external/intercalative binding to quadruplex DNA, respectively. From experimental results it is clear that the interaction of PBD2 and TMPyP4 impart higher stability to the quadruplex complex. PMID:22558271

  6. Interaction of pyrrolobenzodiazepine (PBD ligands with parallel intermolecular G-quadruplex complex using spectroscopy and ESI-MS.

    Directory of Open Access Journals (Sweden)

    Gajjela Raju

    Full Text Available Studies on ligand interaction with quadruplex DNA, and their role in stabilizing the complex at concentration prevailing under physiological condition, has attained high interest. Electrospray ionization mass spectrometry (ESI-MS and spectroscopic studies in solution were used to evaluate the interaction of PBD and TMPyP4 ligands, stoichiometry and selectivity to G-quadruplex DNA. Two synthetic ligands from PBD family, namely pyrene-linked pyrrolo[2,1-c][1,4]benzodiazepine hybrid (PBD1, mixed imine-amide pyrrolobenzodiazepine dimer (PBD2 and 5,10,15,20-tetrakis(N-methyl-4-pyridylporphyrin (TMPyP4 were studied. G-rich single-stranded oligonucleotide d(5'GGGGTTGGGG3' designated as d(T(2G(8, from the telomeric region of Tetrahymena Glaucoma, was considered for the interaction with ligands. ESI-MS and spectroscopic methods viz., circular dichroism (CD, UV-Visible, and fluorescence were employed to investigate the G-quadruplex structures formed by d(T(2G(8 sequence and its interaction with PBD and TMPyP4 ligands. From ESI-MS spectra, it is evident that the majority of quadruplexes exist as d(T(2G(8(2 and d(T(2G(8(4 forms possessing two to ten cations in the centre, thereby stabilizing the complex. CD band of PBD1 and PBD2 showed hypo and hyperchromicity, on interaction with quadruplex DNA, indicating unfolding and stabilization of quadruplex DNA complex, respectively. UV-Visible and fluorescence experiments suggest that PBD1 bind externally where as PBD2 intercalate moderately and bind externally to G-quadruplex DNA. Further, melting experiments using SYBR Green indicate that PBD1 unfolds and PBD2 stabilizes the G-quadruplex complex. ITC experiments using d(T(2G(8 quadruplex with PBD ligands reveal that PBD1 and PBD2 prefer external/loop binding and external/intercalative binding to quadruplex DNA, respectively. From experimental results it is clear that the interaction of PBD2 and TMPyP4 impart higher stability to the quadruplex complex.

  7. ESI(+-MS and GC-MS Study of the Hydrolysis of N-Azobenzyl Derivatives of Chitosan

    Directory of Open Access Journals (Sweden)

    Fernanda S. Pereira

    2014-10-01

    Full Text Available New N-p-chloro-, N-p-bromo-, and N-p-nitrophenylazobenzylchitosan derivatives, as well as the corresponding azophenyl and azophenyl-p-sulfonic acids, were synthesized by coupling N-benzylvchitosan with aryl diazonium salts. The synthesized molecules were analyzed by UV-Vis, FT-IR, 1H-NMR and 15N-NMR spectroscopy. The capacity of copper chelation by these materials was studied by AAS. Chitosan and the derivatives were subjected to hydrolysis and the products were analyzed by ESI(+-MS and GC-MS, confirming the formation of N-benzyl chitosan. Furthermore, the MS results indicate that a nucleophilic aromatic substitution (SnAr reaction occurs under hydrolysis conditions, yielding chloroaniline from N-p-bromo-, and N-p-nitrophenylazo-benzylchitosan as well as bromoaniline from N-p-chloro-, and N-p-nitrophenylazobenzyl-chitosan.

  8. Structural elucidation of in vitro and in vivo metabolites of emodin in rats by LC -ESI-MS/MS

    International Nuclear Information System (INIS)

    Wang, D.; Zhu, Q.; Chen, G.; Liu, B.; Chen, L.

    2013-01-01

    Emodin is a widely occurring natural product and has been studied extensively for its varieties of pharmacological activity. In attempt to know more deeply about its metabolism, this paper investigated the metabolites of emodin in rats, including its in vitro conversion product by intestinal microflora and urinary metabolites. The detection of emodin metabolites was performed by liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) with negative ion mode. By comparing the changes of metabolites in molecular masses (delta M), product ions and retention times with those of the parent drug, six metabolites (8-O-methylemodin, omega-hydroxyemodin, x-hydroxyemodin, emodin glucuronide, hydroxyemodin glucuronide and emodin sulfate) were observed,and what is more, the metabolite hydroxyemodin glucuronide was first reported in this article. For some metabolites, identification of their precise structure needs to be confirmed by other techniques such as the 1H and 13C NMR. (author)

  9. Non-aqueous CE-MS of cinchona alkaloids - characterizationof a novel CE-ESI-MS interface

    DEFF Research Database (Denmark)

    Hansen, Frederik André; Hansen, Steen Honoré; Petersen, Nickolaj J.

    We have recently in our group at the University of Copenhagen developed a robust and simple sheatless CE-ESI-MS interface (capillary electrophoresis – electrospray ionization-mass spectrometry). In this presentation the interface is characterized and compared with HPLC-MS for studying...... a submicron fracture in the capillary close the ESI tip. The fracture provides a zero dead volume and excellent conducting properties due to the large amount of ions in the electric double layer. Electric current exceeding the upper limit of CE instrumentation of up to 300 µA can easily be obtained....... Furthermore, the increased conductivity of the buffer in the fracture generates field free pumping of the analytes towards the ESI spray tip. In this study the device was used to analyze the four major alkaloids (diastereomeric pairs of quinine/quinidine and cinchonine/cinchonidine) in Cinchona bark samples...

  10. ESI-MS study on non-covalent bond complex of rhFKBP12 and new neurogrowth promoter

    Institute of Scientific and Technical Information of China (English)

    WANG; Hongxia; (王红霞); ZHANG; Xuemin; (张学敏); YANG; Songcheng; (杨松成); XIAO; Junhai; (肖军海); NIE; Aihua; (聂爱华); ZHAO; Liqin; (赵丽琴); LI; Song; (李松)

    2003-01-01

    An ESI-MS method for studying the non-covalent bond complex of rhFKBP12 with its nonimmunosuppressive ligands was developed. The method was used to screen out three compounds capable of binding to rhFKBP12 non-covalently from 52 compounds. By competing binding experiment, the binding site and the relative binding strength of these three compounds 000107, 000308 and A2B12 with rhFKBP12 were measured. All of them have the same binding site as FK506 does. X-ray crystalline diffraction experiment of non-covalent bond complex of 000107, 000308 with rhFKBP12 by Tsinghua University showed the same results. Among them 000308 has good effect on stimulating neurite to grow in chicken sensory neuronal cultures.

  11. Identification and determination of the major constituents in traditional Chinese medicine Longdan Xiegan Pill by HPLC-DAD-ESI-MS

    Directory of Open Access Journals (Sweden)

    Hui Liu

    2011-02-01

    Full Text Available A novel and sensitive HPLC-UV method has been developed for the simultaneous determination of twelve major compounds in Longdan Xiegan Pill. The chemical profile of the twelve compounds, including geniposidic acid (1, geniposide(2, gentiopicroside(3, liquiritin(4, crocin(5, baicalin(6, wogonoside(7, baicalein(8, glycyrrhizic acid (9, wogonin (10, oroxylin A (11 and aristolochic acid A (12, was acquired using high-performance liquid chromatography-diode array detector coupled with an electrospray tandem mass spectrometer (HPLC-DAD-ESI-MS. The analysis was performed on a Dikma Platisil ODS C18 column (250 mm × 4. 6 mm, 5 μm with a gradient solvent system of acetonitrile-0. 1% aqueous formic acid. The validation was carried out and the linearities (r > 0. 9996, repeatability (RSD<1. 8%, intra- and inter-day precision (RSD< 1. 3%, and recoveries (ranging from 96. 6% to 103. 4% were acceptable. The limits of detection (LOD of these compounds ranged from 0.29 to 4. 17 ng. Aristolochic acid A, which is the toxic ingredient, was not detected in all the batches of Longdan Xiegan Pill. Furthermore, hierarchical cluster analysis was used to evaluate the variation of the herbal prescription. The proposed method is simple, effective and suitable for the quality control of this traditional Chinese medicine (TCM. Keywords: Longdan Xiegan Pill, high-performance liquid chromatography-diode array detector coupled with an electrospray tandem mass spectrometer (HPLC-DAD-ESI-MS, qualitative evaluation, aristolochic acid A, hierarchical cluster analysis

  12. Proteome profile of functional mitochondria from human skeletal muscle using one-dimensional gel electrophoresis and HPLC-ESI-MS/MS

    DEFF Research Database (Denmark)

    Lefort, Natalie; Yi, Zhengping; Bowen, Benjamin

    2009-01-01

    were functional as evidenced by their response to carbohydrate and fat-derived fuels. Using one-dimensional gel electrophoresis and HPLC-ESI-MS/MS, 823 unique proteins were detected, and 487 of these were assigned to the mitochondrion, including the newly characterized SIRT5, MitoNEET and RDH13...

  13. High temperature liquid chromatography hyphenated with ESI-MS and ICP-MS detection for the structural characterization and quantification of halogen containing drug metabolites

    International Nuclear Information System (INIS)

    Vlieger, Jon S.B. de; Giezen, Mark J.N.; Falck, David; Tump, Cornelis; Heuveln, Fred van; Giera, Martin; Kool, Jeroen; Lingeman, Henk; Wieling, Jaap; Honing, Maarten; Irth, Hubertus; Niessen, Wilfried M.A.

    2011-01-01

    Highlights: → Hyphenation of high temperature liquid chromatography to ICP-MS and ESI-MS. → Structural characterization of kinase inhibitor metabolites with high resolution MS n experiments. → Quantification of drug metabolites with ICP-MS based on Iodine detection. → Significant changes in ESI-MS response after small structural changes. - Abstract: In this paper we describe the hyphenation of high temperature liquid chromatography with ICP-MS and ESI-MS for the characterization of halogen containing drug metabolites. The use of temperature gradients up to 200 deg. C enabled the separation of metabolites with low organic modifier content. This specific property allowed the use of detection methods that suffer from (significant) changes in analyte response factors as a function of the organic modifier content such as ICP-MS. Metabolites of two kinase inhibitors (SB-203580-Iodo and MAPK inhibitor VIII) produced by bacterial cytochrome P450 BM3 mutants and human liver microsomes were identified based on high resolution MS n data. Quantification was done using their normalized and elemental specific response in the ICP-MS. The importance of these kinds of quantification strategies is stressed by the observation that the difference of the position of one oxygen atom in a structure can greatly affect its response in ESI-MS and UV detection.

  14. LC-MS of Metmyoglobin at pH = 2: Separation and Characterization of Apomyoglobin and Heme by ESI-MS and UV-Vis

    Science.gov (United States)

    Stynes, Helen Cleary; Layo, Araceli; Smith, Richard W.

    2004-01-01

    The protein species of apomyoglobin (apoMb) and heme are freed and segregated from the aqueous protein solution of metmyoglobin by liquid chromatography, and are distinguished by UV-Vis absorption or electrospray ionization mass spectrometry (ESI-MS). This is an ingenious and effective approach to characterize apomyoglobin and heme, while students…

  15. Separation and identification of selenotrisulfides in epithelial cell homogenates by LC-ICP-MS and LC-ESI-MS after incubation with selenite

    DEFF Research Database (Denmark)

    Gabel-Jensen, Charlotte; Gammelgaard, Bente; Bendahl, Lars

    2006-01-01

    . The presence of Cys-Se-SG and GS-Se-SG was verified by LC-ESI-MS. Selenotrisulfides were synthesized by reaction of L-cysteine and L-glutathione with sodium selenite. The reaction mixture contained three main products: selenodicysteine (Cys-Se-Cys), selenocysteine glutathione (Cys...

  16. New methodology for capillary electrophoresis with ESI-MS detection: Electrophoretic focusing on inverse electromigration dispersion gradient. High-sensitivity analysis of sulfonamides in waters

    Czech Academy of Sciences Publication Activity Database

    Malá, Zdeňka; Gebauer, Petr; Boček, Petr

    2016-01-01

    Roč. 935, SEP (2016), s. 249-257 ISSN 0003-2670 R&D Projects: GA ČR(CZ) GA16-09135S Institutional support: RVO:68081715 Keywords : electrophoretic focusing * CE-ESI-MS * capillary electrophoresis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.950, year: 2016

  17. Relative quantification of enantiomers of chiral amines by high-throughput LC–ESI-MS/MS using isotopic variants of light and heavy L-pyroglutamic acids as the derivatization reagents

    International Nuclear Information System (INIS)

    Mochizuki, Toshiki; Taniguchi, Sayuri; Tsutsui, Haruhito; Min, Jun Zhe; Inoue, Koichi; Todoroki, Kenichiro; Toyo’oka, Toshimasa

    2013-01-01

    Highlights: ► Development of chiral labeling reagent for a pair of amine enantiomers. ► High-throughput analysis of diastereomers by UPLC–ESI-MS/MS. ► Highly efficient separation and detection of the enantiomers. ► Differential analysis of enantiomer ratio in different sample groups using light and heavy labeling reagents. -- Abstract: L-Pyroglutamic acid (L-PGA) was evaluated as a chiral labeling reagent for the enantioseparation of chiral amines in terms of separation efficiency by reversed-phase chromatography and detection sensitivity by ESI-MS/MS. Several amines and amino acid methyl esters were used as typical representatives of the chiral amines. Both enantiomers of the chiral amines were easily labeled with L-PGAs at room temperature for 60 min in the presence of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide and 1-hydroxy-1H-benzotriazole as the activation reagents. The resulting diastereomers were completely separated by reversed-phase chromatography using the small particle (1.7 μm) ODS column (Rs = 1.6–6.8). A highly sensitive detection at a low-fmol level (1–4 fmol) was also obtained from the multiple reaction monitoring (MRM) chromatograms. Therefore, a high-throughput determination was achieved by the present UPLC–ESI-MS/MS method. An isotope labeling strategy using light and heavy L-PGAs for the differential analysis of chiral amines in different sample groups was also proposed in this paper. As a model study, the differential analysis of the R and S ratio of 1-phenylethylamine (PEA) was performed according to the proposed procedure using light and heavy reagents, i.e., L-PGA and L-PGA-d 5 . The R/S ratio of PEA, spiked at the different concentrations in rat plasma, was almost similar to the theoretical values. Consequently, the proposed strategy using light and heavy chiral labeling reagents seems to be applicable for the differential analysis of chiral amine enantiomers in different sample groups, such as healthy persons and

  18. Quantification of underivatised amino acids on dry blood spot, plasma, and urine by HPLC-ESI-MS/MS.

    Science.gov (United States)

    Giordano, Giuseppe; Di Gangi, Iole Maria; Gucciardi, Antonina; Naturale, Mauro

    2012-01-01

    Enzyme deficiencies in amino acid (AA) metabolism affecting the levels of amino acids and their derivatives in physiological fluids may serve as diagnostically significant biomarkers for one or a group of metabolic disorders. Therefore, it is important to monitor a wide range of free amino acids simultaneously and to quantify them. This is time consuming if we use the classical methods and more than ever now that many laboratories have introduced Newborn Screening Programs for the semiquantitative analysis, detection, and quantification of some amino acids needed to be performed in a short time to reduce the rate of false positives.We have modified the stable isotope dilution HPLC-electrospray ionization (ESI)-MS/MS method previously described by Qu et al. (Anal Chem 74: 2034-2040, 2002) for a more rapid, robust, sensitive, and specific detection and quantification of underivatised amino acids. The modified method reduces the time of analysis to 10 min with very good reproducibility of retention times and a better separation of the metabolites and their isomers.The omission of the derivatization step allowed us to achieve some important advantages: fast and simple sample preparation and exclusion of artefacts and interferences. The use of this technique is highly sensitive, specific, and allows monitoring of 40 underivatized amino acids, including the key isomers and quantification of some of them, in order to cover many diagnostically important intermediates of metabolic pathways.We propose this HPLC-ESI-MS/MS method for underivatized amino acids as a support for the Newborn Screening as secondary test using the same dried blood spots for a more accurate and specific examination in case of suspected metabolic diseases. In this way, we avoid plasma collection from the patient as it normally occurs, reducing anxiety for the parents and further costs for analysis.The same method was validated and applied also to plasma and urine samples with good reproducibility

  19. Screening and Identifying Antioxidative Components in Ginkgo biloba Pollen by DPPH-HPLC-PAD Coupled with HPLC-ESI-MS2

    Science.gov (United States)

    Netrusov, A. I.; Zhou, Qingxin; Guo, Danyang; Liu, Xiaoyong; He, Hailun; Xin, Xue; Wang, Yifen; Chen, Leilei

    2017-01-01

    The Ginkgo biloba is one of ancient trees that exists from billions of years ago, its leaf and nut are used as herbs and foods in China, while so far its pollen does not have any application except pollination. In order to evaluate the antioxidant activity of Ginkgo biloba pollen, and rapidly screen its antioxidative components, the 1,1-diphenyl-2-picrylhydrazyl (DPPH) scavenging ability, total flavonoid, total phenol, and proanthocyanidin of Ginkgo biloba pollen were determined and compared with those of Ginkgo biloba leaf and nut, and the off-line DPPH-HPLC-PAD and HPLC-ESI-MS2 were applied for screening and identifying the antioxidant flavonoids in Ginkgo biloba pollen. The results showed that the DPPH scavenging ability of Ginkgo biloba pollen was much higher than Ginkgo biloba nut, but lower than Ginkgo biloba leaf, while the total content of flavonoid in Ginkgo biloba pollen was approximately 4.37 times higher than in Ginkgo biloba leaf. Further studies found that the major flavonol aglycone in Ginkgo biloba pollen was kaempferol, which accounted for 96.71% of the total aglycones (includes quercetin, kaempferol and isorhamnetin), and the main flavonoid components in Ginkgo biloba pollen were flavonoid glycosides. Finally, ten antioxidant peaks were screened and identified to be flavonoids (including kaempferol and nine flavonoid glycosides), so flavonoids were likely to be the main antioxidant components in GP, and among them, three novel kaempferol glycosides (peaks 1, 2, and 3) were found in Ginkgo biloba pollen for the first time, which had never been found in Ginkgo biloba. PMID:28095510

  20. Determination of Polar Compounds in Guava Leaves Infusions and Ultrasound Aqueous Extract by HPLC-ESI-MS

    Directory of Open Access Journals (Sweden)

    Elixabet Díaz-de-Cerio

    2015-01-01

    Full Text Available Literature lacks publications about polar compounds content in infusion or guava leaves tea. Because of that, a comparison between different times of infusion and a conventional ultrasound aqueous extract was carried out. Several polar compounds have been identified by HPLC-ESI-MS and their antioxidant activity was evaluated by FRAP and ABTS assays. Four different classes of phenolic compounds (gallic and ellagic acid derivatives, flavonols, flavanones, and flavan-3-ols and some benzophenones were determined. The quantification results reported that the order, in terms of concentration of the classes of polar compounds in all samples, was flavonols > flavan-3-ols > gallic and ellagic acid derivatives > benzophenones > flavanones. As expected, the aqueous extract obtained by sonication showed the highest content in the compounds studied. Significative differences were noticed about the different times of infusion and five minutes was the optimal time to obtain the highest content in polar compounds using this culinary method. All the identified compounds, except HHDP isomers and naringenin, were positively correlated with antioxidant activity.

  1. A method for the determination of acrylamide in bakery products using ion trap LC-ESI-MS/MS.

    Science.gov (United States)

    Claus, Achim; Weisz, Georg M; Kammerer, Dietmar R; Carle, Reinhold; Schieber, Andreas

    2005-10-01

    Acrylamide levels of bakery products, e. g., bread and bread rolls, are usually below 100 microg/kg , often even below 50 microg/kg. Therefore, usual analytical methods which have an LOQ greater, not dbl equals 25 microg/kg are not sensitive enough for detailed investigations on acrylamide formation within these commodities. An improved method for trace level determination of acrylamide in bakery products was developed using ion trap LC-ESI-MS/MS. Samples were divided into crumbs and crusts to achieve an initial concentration by removing the crumbs since these are devoid of acrylamide. After sample extraction and clean-up using multimode SPE cartridges, further analyte enrichment was accomplished by solid-phase-supported liquid-liquid extraction with ethyl acetate prior to LC-MS/MS analysis. The method was evaluated using bread, bread rolls, alkali-baked bread rolls, and toast. LOQ was calculated from the confidence interval of the calibration curve and found to be 1.7 ng/mL, corresponding to 17 microg/kg of product. When crumbs and crusts were separated, an LOQ of 10.2 microg/kg of bakery product could be obtained. As demonstrated in preliminary comparative analyses, accuracy of the method met the requirements for determination of trace level acrylamide formation in bakery products. Mean recovery was 102.4% (CV 4.5%), intermediate reproducibility revealed a CV of 2.1%, and a repeatability of CV 6.0%.

  2. LC-ESI-MS/MS analysis of phosphodiesterase-5 inhibitors and their analogues in foods and dietary supplements in Korea.

    Science.gov (United States)

    Jeong, Ji Hye; Lee, Ji Hyun; Kim, Hyung Joo; Park, Hyoung Joon; Hwang, In Sun; Han, Kyoung Moon; Yoon, Chang-Yong; Cho, Sooyeul; Kim, Woo Seong

    2016-01-01

    A number of 188 food and dietary supplement samples were collected from 2009 to the first half of 2013 in Korean online and offline stores. A method to identify phosphodiesterase-5 (PDE-5) inhibitors and their analogues using liquid chromatography-electrospray ionisation-mass spectrometry/mass spectrometry (LC-ESI-MS/MS) was validated. Limit of detection and limit of quantitation of liquid-type and solid-type negative samples ranged from 0.05 to 3.33 ng/mL or ng/g and from 0.15 to 10.00 ng/mL or ng/g, respectively. Recoveries ranged from 83% to 112%. Nineteen PDE-5 inhibitors and their analogues were detected, with tadalafil group compounds being the most frequently observed (53.0%), followed by the sildenafil group (42.5%). Tadalafil concentrations ranged from 0.08 to 138.69 mg/g. Compounds were most frequently detected in capsules (in 40 of 80 adulterated samples). To protect public health and food safety, appropriate monitoring of PDE-5 inhibitors and their analogues in foods and dietary supplements is recommended.

  3. A new LC-ESI-MS/MS method to measure long-chain acylcarnitine levels in cultured cells

    International Nuclear Information System (INIS)

    Jauregui, Olga; Sierra, Adriana Y.; Carrasco, Patricia; Gratacos, Esther; Hegardt, Fausto G.; Casals, Nuria

    2007-01-01

    The quantitative evaluation of long-chain acylcarnitines in lipid extracts from cultured cells or tissues is a prerequisite to study carnitine palmitoyltransferase (CPT) activity. There is thus a need for the accurate measurement of the concentration of long-chain acylcarnitines at the lowest concentration present in lipid extracts. Here we report a fast and reliable quantitative method based on the use of weak acid extraction and liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) to quantify acylcarnitines through hydrophilic interaction chromatography. The method was validated using isotopic dilution and the results allow the analysis of a large number of samples at low concentration levels (down to 0.35 nmol L -1 for palmitoylcarnitine) with good inter- and intra-day precision. The method was used for the quantitative study of changes in concentration of palmitoylcarnitine and other acylcarnitines in PC-12 cells over-expressing CPT1a gene. It was also used to measure CPT1 activity in mitochondria isolated from transfected cells, giving similar results to the more common radiometric method, but with higher sensitivity

  4. A new LC-ESI-MS/MS method to measure long-chain acylcarnitine levels in cultured cells

    Energy Technology Data Exchange (ETDEWEB)

    Jauregui, Olga [Scientific and Technical Services, University of Barcelona (Spain); Sierra, Adriana Y.; Carrasco, Patricia; Gratacos, Esther [Molecular and Cellular Unit, School of Health Sciences, International University of Catalonia (Spain); Hegardt, Fausto G. [Department of Biochemistry and Molecular Biology, University of Barcelona, School of Pharmacy (Spain); Casals, Nuria [Molecular and Cellular Unit, School of Health Sciences, International University of Catalonia (Spain)], E-mail: ncasals@csc.uic.es

    2007-09-05

    The quantitative evaluation of long-chain acylcarnitines in lipid extracts from cultured cells or tissues is a prerequisite to study carnitine palmitoyltransferase (CPT) activity. There is thus a need for the accurate measurement of the concentration of long-chain acylcarnitines at the lowest concentration present in lipid extracts. Here we report a fast and reliable quantitative method based on the use of weak acid extraction and liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) to quantify acylcarnitines through hydrophilic interaction chromatography. The method was validated using isotopic dilution and the results allow the analysis of a large number of samples at low concentration levels (down to 0.35 nmol L{sup -1} for palmitoylcarnitine) with good inter- and intra-day precision. The method was used for the quantitative study of changes in concentration of palmitoylcarnitine and other acylcarnitines in PC-12 cells over-expressing CPT1a gene. It was also used to measure CPT1 activity in mitochondria isolated from transfected cells, giving similar results to the more common radiometric method, but with higher sensitivity.

  5. Polyphenolic compounds in date fruit seed (Phoenix dactylifera): characterisation and quantification by using UPLC-DAD-ESI-MS.

    Science.gov (United States)

    Habib, Hosam M; Platat, Carine; Meudec, Emmanuelle; Cheynier, Veronique; Ibrahim, Wissam H

    2014-04-01

    Date fruit seeds have been demonstrated to possess high antioxidant activities due to their high content of flavonoids and phenolic compounds. The objective of this work was to identify and quantify the phenolic composition of date seeds. Two UPLC-DAD-ESI-MS analyses were performed on the seed of the Khalas variety as follows: (1) an analysis of simple phenolic compounds [phenolic acids, hydroxycinnamic acids, flavonols, flavones, flavan-3-ols (monomers, dimers and trimers)]; and (2) an analysis of all flavan-3-ols (monomers, and proanthocyanidin oligomers and polymers) after depolymerisation. The amount of total phenolic compounds before depolymerisation was found to be 2.194 ± 0.040 g kg(-1) date seed. The analysis of flavan-3-ol monomers and constitutive units of proanthocyanidins after depolymerisation revealed 50.180 ± 1.360 g kg(-1) flavan-3-ols with 46.800 ± 1.012 g kg(-1) epicatechin and 3.380 ± 0.349 g kg(-1) catechin. The results indicate that date seeds are a very rich source of bioactive compounds, thus constituting strong candidates for functional food additives and nutraceuticals. © 2013 Society of Chemical Industry.

  6. Rapid Characterization of Insulin Modifications and Sequence Variations by Proteinase K Digestion and UHPLC-ESI-MS

    Science.gov (United States)

    Yang, Rong-Sheng; Tang, Weijuan; Sheng, Huaming; Meng, Fanyu

    2018-01-01

    Discovery of novel insulin analogs as therapeutics has remained an active area of research. Compared with native human insulin, insulin analog molecules normally incorporate either covalent modifications or amino acid sequence variations. From the drug discovery and development perspective, methods for efficient and detailed characterization of these primary structural changes are very important. In this report, we demonstrate that proteinase K digestion coupled with UPLC-ESI-MS analysis provides a simple and rapid approach to characterize the modifications and sequence variations of insulin molecules. A commercially available proteinase K digestion kit was used to process recombinant human insulin (RHI), insulin glargine, and fluorescein isothiocynate-labeled recombinant human insulin (FITC-RHI) samples. The LC-MS data clearly showed that RHI and insulin glargine samples can be differentiated, and the FITC modifications in all three amine sites of the RHI molecule are well characterized. The end-to-end experiment and data interpretation was achieved within 60 min. This approach is fast and simple, and can be easily implemented in early drug discovery laboratories to facilitate research on more advanced insulin therapeutics. [Figure not available: see fulltext.

  7. Rapid Characterization of Insulin Modifications and Sequence Variations by Proteinase K Digestion and UHPLC-ESI-MS

    Science.gov (United States)

    Yang, Rong-Sheng; Tang, Weijuan; Sheng, Huaming; Meng, Fanyu

    2018-05-01

    Discovery of novel insulin analogs as therapeutics has remained an active area of research. Compared with native human insulin, insulin analog molecules normally incorporate either covalent modifications or amino acid sequence variations. From the drug discovery and development perspective, methods for efficient and detailed characterization of these primary structural changes are very important. In this report, we demonstrate that proteinase K digestion coupled with UPLC-ESI-MS analysis provides a simple and rapid approach to characterize the modifications and sequence variations of insulin molecules. A commercially available proteinase K digestion kit was used to process recombinant human insulin (RHI), insulin glargine, and fluorescein isothiocynate-labeled recombinant human insulin (FITC-RHI) samples. The LC-MS data clearly showed that RHI and insulin glargine samples can be differentiated, and the FITC modifications in all three amine sites of the RHI molecule are well characterized. The end-to-end experiment and data interpretation was achieved within 60 min. This approach is fast and simple, and can be easily implemented in early drug discovery laboratories to facilitate research on more advanced insulin therapeutics. [Figure not available: see fulltext.

  8. Novel Tyrosine Phosphorylation Sites in Rat Skeletal Muscle Revealed by Phosphopeptide Enrichment and HPLC-ESI-MS/MS

    Science.gov (United States)

    Zhang, Xiangmin; Højlund, Kurt; Luo, Moulun; Meyer, Christian; Thangiah, Geetha; Yi, Zhengping

    2012-01-01

    Tyrosine phosphorylation plays a fundamental role in many cellular processes including differentiation, growth and insulin signaling. In insulin resistant muscle, aberrant tyrosine phosphorylation of several proteins has been detected. However, due to the low abundance of tyrosine phosphorylation (tyrosine phosphorylation sites have been identified in mammalian skeletal muscle to date. Here, we used immunoprecipitation of phosphotyrosine peptides prior to HPLC-ESI-MS/MS analysis to improve the discovery of tyrosine phosphorylation in relatively small skeletal muscle biopsies from rats. This resulted in the identification of 87 distinctly localized tyrosine phosphorylation sites in 46 muscle proteins. Among them, 31 appear to be novel. The tyrosine phosphorylated proteins included major enzymes in the glycolytic pathway and glycogen metabolism, sarcomeric proteins, and proteins involved in Ca2+ homeostasis and phosphocreatine resynthesis. Among proteins regulated by insulin, we found tyrosine phosphorylation sites in glycogen synthase, and two of its inhibitors, GSK-3α and DYRK1A. Moreover, tyrosine phosphorylation sites were identified in several MAP kinases and a protein tyrosine phosphatase, SHPTP2. These results provide the largest catalogue of mammalian skeletal muscle tyrosine phosphorylation sites to date and provide novel targets for the investigation of human skeletal muscle phosphoproteins in various disease states. PMID:22609512

  9. Chemical Differentiation of Dendrobium officinale and Dendrobium devonianum by Using HPLC Fingerprints, HPLC-ESI-MS, and HPTLC Analyses

    Science.gov (United States)

    Ye, Zi; Dai, Jia-Rong; Zhang, Cheng-Gang; Lu, Ye; Wu, Lei-Lei; Gong, Amy G. W.; Wang, Zheng-Tao

    2017-01-01

    The stems of Dendrobium officinale Kimura et Migo (Dendrobii Officinalis Caulis) have a high medicinal value as a traditional Chinese medicine (TCM). Because of the limited supply, D. officinale is a high priced TCM, and therefore adulterants are commonly found in the herbal market. The dried stems of a closely related Dendrobium species, Dendrobium devonianum Paxt., are commonly used as the substitute; however, there is no effective method to distinguish the two Dendrobium species. Here, a high performance liquid chromatography (HPLC) method was successfully developed and applied to differentiate D. officinale and D. devonianum by comparing the chromatograms according to the characteristic peaks. A HPLC coupled with electrospray ionization multistage mass spectrometry (HPLC-ESI-MS) method was further applied for structural elucidation of 15 flavonoids, 5 phenolic acids, and 1 lignan in D. officinale. Among these flavonoids, 4 flavonoid C-glycosides were firstly reported in D. officinale, and violanthin and isoviolanthin were identified to be specific for D. officinale compared with D. devonianum. Then, two representative components were used as chemical markers. A rapid and reliable high performance thin layer chromatography (HPTLC) method was applied in distinguishing D. officinale from D. devonianum. The results of this work have demonstrated that these developed analytical methods can be used to discriminate D. officinale and D. devonianum effectively and conveniently. PMID:28769988

  10. HPLC-DAD-ESI/MS(n) analysis of phenolic compounds for quality control of Grindelia robusta Nutt. and bioactivities.

    Science.gov (United States)

    Ferreres, Federico; Grosso, Clara; Gil-Izquierdo, Angel; Valentão, Patrícia; Azevedo, Carolina; Andrade, Paula B

    2014-06-01

    The phenolic composition of herbal tea (HT) and hydromethanolic extract (HME) obtained from Grindelia robusta Nutt. was studied by HPLC-DAD-ESI/MS(n). Thirty six flavonoids and hydroxycinnamic acids were detected, from which thirty are described for the first time in this species. Quantification by HPLC-DAD showed that diosmetin-7-O-glucuronide-3'-O-pentoside+apigenin-7-O-glucuronide-4'-O-pentoside, apigenin-7-O-glucuronide+diosmetin-7-O-glucuronide and 3,5-dicaffeoylquinic acid+3,4-dicaffeoylquinic acid were the major compounds. Since the health-promoting effects of natural phenolic compounds against brain disorders is of increasing interest, HT and HME were also tested against oxygen and nitrogen reactive species and against enzymes related with Alzheimer's disease and depression. Extracts displayed strong in vitro scavenging activity and monoamine oxidase-A (MAO-A) inhibitory activity. The anti-MAO-A capacity was observed at non-toxic concentrations for SH-SY5Y human neuroblastoma cell line, reinforcing the benefits of G. robusta HT. However, no protection against hydrogen peroxide treatment was observed. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. Quantification of the Triazole Antifungal Compounds Voriconazole and Posaconazole in Human Serum or Plasma Using Liquid Chromatography Electrospray Tandem Mass Spectrometry (HPLC-ESI-MS/MS).

    Science.gov (United States)

    Molinelli, Alejandro R; Rose, Charles H

    2016-01-01

    Voriconazole and posaconazole are triazole antifungal compounds used in the treatment of fungal infections. Therapeutic drug monitoring of both compounds is recommended in order to guide drug dosing to achieve optimal blood concentrations. In this chapter we describe an HPLC-ESI-MS/MS method for the quantification of both compounds in human plasma or serum following a simple specimen preparation procedure. Specimen preparation consists of protein precipitation using methanol and acetonitrile followed by a cleanup step that involves filtration through a cellulose acetate membrane. The specimen is then injected into an HPLC-ESI-MS/MS equipped with a C18 column and separated over an acetonitrile gradient. Quantification of the drugs in the specimen is achieved by comparing the response of the unknown specimen to that of the calibrators in the standard curve using multiple reaction monitoring.

  12. Isolation and identification of arctiin and arctigenin in leaves of burdock (Arctium lappa L.) by polyamide column chromatography in combination with HPLC-ESI/MS.

    Science.gov (United States)

    Liu, Shiming; Chen, Kaoshan; Schliemann, Willibald; Strack, Dieter

    2005-01-01

    A simple method involving polyamide column chromatography in combination with HPLC-PAD and HPLC-ESI/MS for isolating and identifying two kinds of lignans, arctiin and arctigenin, in the leaves of burdock (Arctium lappa L.) has been established. After extraction of burdock leaves with 80% methanol, the aqueous phase of crude extracts was partitioned between water and chloroform and the aqueous phase was fractionated on a polyamide glass column. The fraction, eluting with 100% methanol, was concentrated and gave a white precipitate at 4 degrees C from which two main compounds were purified by semi-preparative HPLC. In comparison with the UV and ESI-MS spectra and the HPLC retention time of authentic standards, the compounds were determined to be arctiin and arctigenin. The extraction/separation technique was validated using an internal standard method.

  13. The 4-pyridylmethyl ester as a protecting group for glutamic and aspartic acids: 'flipping' peptide charge states for characterization by positive ion mode ESI-MS.

    Science.gov (United States)

    Garapati, Sriramya; Burns, Colin S

    2014-03-01

    Use of the 4-pyridylmethyl ester group for side-chain protection of glutamic acid residues in solid-phase peptide synthesis enables switching of the charge state of a peptide from negative to positive, thus making detection by positive ion mode ESI-MS possible. The pyridylmethyl ester moiety is readily removed from peptides in high yield by hydrogenation. Combining the 4-pyridylmethyl ester protecting group with benzyl ester protection reduces the number of the former needed to produce a net positive charge and allows for purification by RP HPLC. This protecting group is useful in the synthesis of highly acidic peptide sequences, which are often beset by problems with purification by standard RP HPLC and characterization by ESI-MS. Copyright © 2014 European Peptide Society and John Wiley & Sons, Ltd.

  14. DIRECT INFUSION ESI-MS APPLIED IN THE DETECTION OF BYPRODUCTS DUE TO REDUCTIVE DEGRADATION OF ACETAMIPRID BY ZERO-VALENT IRON

    Directory of Open Access Journals (Sweden)

    Jean C. Cruz

    2015-09-01

    Full Text Available This study investigated the reductive degradation of acetamiprid (5 mg L-1 in aqueous medium (at pH 2.0 induced by zero-valent iron (50 mg. The process was monitored using high-performance liquid chromatography (HPLC to determine the degradation rate as a function of reaction time, and direct infusion electrospray ionization mass spectrometry (DI-ESI-MS to search for (and potentially characterize any possible byproducts formed during degradation. The results obtained via HPLC showed that after 60 min, the degradation of the substrate reached nearly 100% in an acidic medium, whereas the mineralization rate (as determined by total organic carbon measurements was as low as 3%. Data obtained by DI-ESI-MS showed that byproducts were formed mainly by insertions of hydrogen atoms into the nitrile, imine, and pyridine ring moieties, in addition to the observation of chlorine substitution by hydrogen replacement (hydrodechlorination reactions.

  15. Perspectivas mecanisticas de reações organicas catalisadas por paladio : Heck, oxa-Heck e acoplamento de Buchwald-Hartwig por ESI-MS/MS

    OpenAIRE

    Boniek Gontijo Vaz

    2009-01-01

    Resumo: A espectrometria de Massas por eletronspray (ESI-MS) tornou-se um método prático para o estudo de mecanismos reacionais em solução. Neste trabalho importantes reações catalisadas por paládio: reação de Heck-Mizoroki, oxa-Heck e o acoplamento de Buchwald-Hartwig foram monitoradas por ESI-MS visando interceptar espécies que comprovam as atuais propostas mecanísticas ou que abram caminho para novas propostas para estas reações. O monitoramento das reações foi realizado no modo off-line, ...

  16. Surfactant-free microemulsion electrokinetic chromatography (SF-MEEKC) with UV and MS detection - a novel approach for the separation and ESI-MS detection of neutral compounds.

    Science.gov (United States)

    Mohorič, Urška; Beutner, Andrea; Krickl, Sebastian; Touraud, Didier; Kunz, Werner; Matysik, Frank-Michael

    2016-12-01

    Microemulsion electrokinetic chromatography (MEEKC) is a powerful tool to separate neutral species based on differences in their hydrophobic and hydrophilic properties. However, as a major drawback the conventionally used SDS based microemulsions are not compatible with electrospray ionization mass spectrometry (ESI-MS). In this work, a surfactant-free microemulsion (SFME) consisting of water, ethanol, and 1-octanol is used for surfactant-free microemulsion electrokinetic chromatography (SF-MEEKC). Ammonium acetate was added to the SFME enabling electrophoretic separations. The stability of SFMEs containing ammonium acetate was investigated using small-angle X-ray scattering and dynamic light scattering. A method for the separation of a model system of hydrophobic and hydrophilic neutral vitamins, namely the vitamins B 2 and D 3 , and the cationic vitamin B 1 was developed using UV/VIS detection. The influence of the ammonium acetate concentration on the separation performance was studied in detail. The method was characterized concerning reproducibility of migration times and peak areas and concerning the linearity of the calibration data. Furthermore, SF-MEEKC was coupled to ESI-MS investigating the compatibility between SFMEs and the ESI process. The signal intensities of ESI-MS measurements of the model analytes were comparable for SFMEs and aqueous systems. Finally, the vitamin D 3 content of a drug treating vitamin D 3 deficiency was determined by SF-MEEKC coupled to ESI-MS using 25-hydroxycholecalciferol as an internal standard. Graphical abstract The concept of surfactant-free microemulsion electrokinetic chromatography coupled to electrospray ionization mass spectrometry.

  17. Detecting Protein-Glycolipid Interactions Using CaR-ESI-MS and Model Membranes: Comparison of Pre-loaded and Passively Loaded Picodiscs

    Science.gov (United States)

    Li, Jun; Han, Ling; Li, Jianing; Kitova, Elena N.; Xiong, Zi Jian; Privé, Gilbert G.; Klassen, John S.

    2018-04-01

    Catch-and-release electrospray ionization mass spectrometry (CaR-ESI-MS), implemented using model membranes (MMs), is a promising approach for the discovery of glycolipid ligands of glycan-binding proteins (GBPs). Picodiscs (PDs), which are lipid-transporting complexes composed of the human sphingolipid activator protein saposin A and phospholipids, have proven to be useful MMs for such studies. The present work compares the use of conventional (pre-loaded) PDs with passively loaded PDs (PLPDs) for CaR-ESI-MS screening of glycolipids against cholera toxin B subunit homopentamer (CTB5). The pre-loaded PDs were prepared from a mixture of purified glycolipid and phospholipid or a mixture of lipids extracted from tissue, while the PLPDs were prepared by incubating PDs containing only phospholipid with glycolipid-containing lipid mixtures in aqueous solution. Time-dependent changes in the composition of the PLPDs produced by incubation with glycomicelles of the ganglioside GM1 were monitored using collision-induced dissociation of the gaseous PD ions and from the extent of ganglioside binding to CTB5 measured by ESI-MS. GM1 incorporation into PDs was evident within a few hours of incubation. At incubation times ≥ 10 days, GM1 binding to CTB5 was indistinguishable from that observed with pre-loaded PDs produced directly from GM1 at the same concentration. Comparison of ganglioside binding to CTB5 measured for pre-loaded PDs and PLPDs prepared from glycolipids extracted from pig and mouse brain revealed that the PLPDs allow for the detection of a greater number of ganglioside ligands. Together, the results of this study suggest PLPDs may have advantages over conventionally prepared PDs for screening glycolipids against GBPs using CaR-ESI-MS. [Figure not available: see fulltext.

  18. Tandem mass spectrometry approach for the investigation of the steroidal metabolism: structure-fragmentation relationship (SFR) in anabolic steroids and their metabolites by ESI-MS/MS analysis.

    Science.gov (United States)

    Musharraf, Syed Ghulam; Ali, Arslan; Khan, Naik Tameem; Yousuf, Maria; Choudhary, Muhammad Iqbal; Atta-ur-Rahman

    2013-02-01

    Electrospray ionization tandem mass spectrometry (ESI-MS/MS) was used to investigate the effect of different substitutions introduced during metabolism on fragmentation patterns of four anabolic steroids including methyltestosterone, methandrostenolone, cis-androsterone and adrenosterone, along with their metabolites. Collision-induced dissociation (CID) analysis was performed to correlate the major product ions of 19 steroids with structural features. The analysis is done to portray metabolic alteration, such as incorporation or reduction of double bonds, hydroxylations, and/or oxidation of hydroxyl moieties to keto functional group on steroidal skeleton which leads to drastically changed product ion spectra from the respective classes of steroids, therefore, making them difficult to identify. The comparative ESI-MS/MS study also revealed some characteristic peaks to differentiate different steroidal metabolites and can be useful for the unambiguous identification of anabolic steroids in biological fluid. Moreover, LC-ESI-MS/MS analysis of fermented extract of methyltestosterone, obtained by Macrophomina phaseolina was also investigated. Copyright © 2012 Elsevier Inc. All rights reserved.

  19. Comparative HPLC/ESI-MS and HPLC/DAD study of different populations of cultivated, wild and commercial Gentiana lutea L.

    Science.gov (United States)

    Mustafa, Ahmed M; Caprioli, Giovanni; Ricciutelli, Massimo; Maggi, Filippo; Marín, Rosa; Vittori, Sauro; Sagratini, Gianni

    2015-05-01

    The root of Gentiana lutea L., famous for its bitter properties, is often used in alcoholic bitter beverages, food products and traditional medicine to stimulate the appetite and improve digestion. This study presents a new, fast, and accurate HPLC method using HPLC/ESI-MS and HPLC/DAD for simultaneous analysis of iridoids (loganic acid), secoiridoids (gentiopicroside, sweroside, swertiamarin, amarogentin) and xanthones (isogentisin) in different populations of G.lutea L., cultivated in the Monti Sibillini National Park, obtained wild there, or purchased commercially. Comparison of HPLC/ESI-MS and HPLC/DAD indicated that HPLC/ESI-MS is more sensitive, reliable and selective. Analysis of twenty samples showed that gentiopicroside is the most dominant compound (1.85-3.97%), followed by loganic acid (0.11-1.30%), isogentisin (0.03-0.48%), sweroside (0.05-0.35%), swertiamarin (0.08-0.30%), and amarogentin (0.01-0.07%). The results confirmed the high quality of the G.lutea cultivated in the Monti Sibillini National Park. Copyright © 2014 Elsevier Ltd. All rights reserved.

  20. Negative ion ESI-MS analysis of natural yellow dye flavonoids--An isotopic labelling study

    Science.gov (United States)

    McNab, Hamish; Ferreira, Ester S. B.; Hulme, Alison N.; Quye, Anita

    2009-07-01

    Flavonoids are amongst the most commonly used natural yellow colourants in paintings, as lakes, and in historical textiles as mordant dyes. In this paper, evidence from isotopically labelled substrates is used to propose negative ion electrospray collision induced decomposition mechanisms of flavones, flavonols and an isoflavone. These mechanisms include a retro-Diels-Alder fragmentation (observed for flavones and flavonols) and an M-122 fragmentation (characteristic of 3',4'-dihydroxyflavonols). In addition, the presence of a m/z 125 fragment ion is shown to be characteristic of 2'-hydroxyflavonols and an ion at m/z 149 is shown to be characteristic of 4'-hydroxyflavones. Applications of these methods are exemplified by the identification of a minor component of Dyer's camomile (Anthemis tinctoria L.) and the identification of the dye source in green threads sampled from an 18th Century Scottish tartan fragment.

  1. Characterization of the Principal Constituents of Danning Tablets, a Chinese Formula Consisting of Seven Herbs, by an UPLC-DAD-MS/MS Approach

    Directory of Open Access Journals (Sweden)

    Changsen Zhan

    2016-05-01

    Full Text Available Danning Tablets are a traditional Chinese formula showing broad clinical applications in hepatobiliary diseases and containing a diversity of bioactive chemicals. However, the chemical profiling of the formula, which serves as the material foundation of its efficacy, is really a big challenge as Danning Tablets consist of seven herbs from different origins. An ultra-performance liquid chromatography coupled to diode array detection and electrospray ionization mass spectrometry (UPLC-DAD-ESI-MS/MS approach was developed to characterize the principal polyphenol constituents in the formula. As a result, a total of 32 constituents, including 14 anthraquinones and their glucosides, four anthrones, two naphthalene glycosides, two stilbenes and 10 flavonoids were identified based on their retention time, UV absorption and MS/MS fragmentation patterns. The sources of these compounds were also illustrated. Most of the bioactive anthraquinone derivatives were found in Rhei Radix et Rhizoma or Polygoni Cuspidati Rhizoma et Radix, which are the Emperor drugs in the formula for its clinic usage. These findings indicate the merit of using this integrated UPLC-DAD-ESI-MS/MS approach to rapidly illustrate the chemical foundation of complex formulas. The present study will facilitate the quality control of Danning Tablet formulas as well as the individual herbs.

  2. Trace detection of the chlorohydrins of epoxidized soybean oil in foodstuffs by UPLC-ESI-MS/MS.

    Science.gov (United States)

    Suman, Michele; De Dominicis, Emiliano; Commissati, Italo

    2010-09-01

    Epoxidized soybean oil (ESBO) is used as an authorized plasticizer and a stabilizer for plastic polymers such as poly(vinyl chloride) (PVC). Recently, however, there has been a concrete effort devoted to its substitution for other plasticizers such as polyadipates. ESBO is exploited particularly in food closure gaskets for metal lids used to seal glass jars and bottles. The closure gaskets form an airtight seal necessary to prevent microbiological contamination. Thus, there are potential uses for food sterilization and storage. Additionally, the main pathway of PVC degradation involves the elimination of HCl, which can react with the epoxy groups of ESBO to give mono-, polychlorohydrins and/or other cyclic derivatives. The European Food Safety Authority noted that not enough analytical and toxicological data exist to express a formal opinion on the significance for the health effects of such derivatives. At present in the scientific literature, there are only a few indicative results of direct measurements of ESBO derivatives and there are no official analytical methods available for the determination of chlorohydrins directly from foodstuffs. This study presents the first example of the analysis of commercial food sauces for the detection of ESBO-chlorohydrins (as methyl esters). The results are obtained by a dedicated development of an ultraperformance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-ESI-MS/MS) method. Sample preparation was based on the following main steps: organic extraction, transesterification and solid-phase extraction clean up. In particular, four isomers for 18-E-OHCl chlorohydrin and eight isomers for 18-2OHCl chlorohydrin were separated and identified. Different food sauces samples closed in glass jars with twist-off caps were subjected to qualitative determination, which yielded positive results for 18-E-OHCl, whereas no traces of 18-2OHCl were found. 2010 John Wiley & Sons, Ltd.

  3. Untargeted LC-QTOF (ESI + MS Analysis of Small Serum Metabolites Related to Prostate Cancer and Prostate Specific Antigen

    Directory of Open Access Journals (Sweden)

    Ramona Maria Maxim

    2014-11-01

    Full Text Available Prostate cancer has an increasing incidence and there is an urgent need for development of new serum biomarkers for early diagnostic as the ones known are ineffective. The aim of the study was to use untargeted metabolomics in order to identify and characterize small metabolite fingerprints in patients with normal vs pathologic values of PSA ( previously determined by electrochemiluminiscence. A cohort of one hundred patients with different Prostate Specific amtigen values were investigated by untargeted metabolomics. The serum small metabolite profile determined by high performance liquid chromatography coupled with mass spectrometry, LC-QTOF(ESI+MS in order to identify specific biomarkers, for normal patient group (PSA = 0-4 ng.ml and four pathologic groups, having PSA values from 4 to >1000 ng/ml. The major molecules identified in the samples were polar phospholipids, maily lysophosphatidyl choline derivatives, having m/z values from 496 to 524, like LPC(O-16:0/O-1:0, LPC(18:1/2:0 or PS(18:1(9Z/0:0, LPC(18:2(9Z,12Z/0:0 and their isomers and  LPC(O-18:1(11Z/2:0, respectively. Also, small molecules (free fatty acids and prostaglandin derivatives were identified and are significantly different in pathologic vs normal serum samples. Generally the pathologic samples had increased concentrations of all above mentioned molecules. The Principal Component analysis showed , by plot and loadings scores, significant clustering of normal vs pathological groups.

  4. Major signal suppression from metal ion clusters in SFC/ESI-MS - Cause and effects.

    Science.gov (United States)

    Haglind, Alfred; Hedeland, Mikael; Arvidsson, Torbjörn; Pettersson, Curt E

    2018-05-01

    The widening application area of SFC-MS with polar analytes and water-containing samples facilitates the use of quick and simple sample preparation techniques such as "dilute and shoot" and protein precipitation. This has also introduced new polar interfering components such as alkali metal ions naturally abundant in e.g. blood plasma and urine, which have shown to be retained using screening conditions in SFC/ESI-TOF-MS and causing areas of major ion suppression. Analytes co-eluting with these clusters will have a decreased signal intensity, which might have a major effect on both quantification and identification. When investigating the composition of the alkali metal clusters using accurate mass and isotopic pattern, it could be concluded that they were previously not described in the literature. Using NaCl and KCl standards and different chromatographic conditions, varying e.g. column and modifier, the clusters proved to be formed from the alkali metal ions in combination with the alcohol modifier and make-up solvent. Their compositions were [(XOCH 3 ) n  + X] + , [(XOH) n  + X] + , [(X 2 CO 3 ) n  + X] + and [(XOOCOCH 3 ) n  + X] + for X = Na + or K + in ESI+. In ESI-, the clusters depended more on modifier, with [(XCl) n  + Cl] - and [(XOCH 3 ) n  + OCH 3 ] - mainly formed in pure methanol and [(XOOCH) n  + OOCH] - when 20 mM NH 4 Fa was added. To prevent the formation of the clusters by avoiding methanol as modifier might be difficult, as this is a widely used modifier providing good solubility when analyzing polar compounds in SFC. A sample preparation with e.g. LLE would remove the alkali ions, however also introducing a time consuming and discriminating step into the method. Since the alkali metal ions were retained and affected by chromatographic adjustments as e.g. mobile phase modifications, a way to avoid them could therefore be chromatographic tuning, when analyzing samples containing them. Copyright © 2018 Elsevier

  5. HPLC-ESI-MS Characterization of Certain Polyphenolic Compounds of Carica papaya L. Fruit Extracts and Evaluation of Their Potential Against Murine Schistosomiasis mansoni.

    Science.gov (United States)

    Abdel-Lateef, Ezzat El-Sayed; Rabia, Ibrahim Aly; El-Sayed, Mortada Mohamed; Abdel-Hameed, El-Sayed Saleh

    2018-04-10

    The in vivo antischistosomal activities of Carica papaya L. extracts were evaluated and the characterization of the active secondary metabolites of the defatted methanolic extract was performed using HPLC-ESI-MS. The plant fruit powders were extracted with 85% methanol and fractionated using organic solvents. The in vivo antischistosomal effects of the methanolic extracts and its fractions, as well as the assessment of the relationship between the antischistosomal activity of these plant extracts and oxidative stress, was determined. In addition, the defatted methanolic extract was characterized by HPLC-ESI-MS analysis. The number of worms, ova, and the Oogram pattern displayed typical Schistosoma mansoni pathology 8 weeks after infection in mice. Treatment of the infected group with the defatted methanolic extracts significantly decreased worm burden, immature ova and mature ova, while increasing the percentage of dead ova in vivo. The butanol fraction was the most effective fraction reducing worm burden by 77%, ova count in the intestine by 76% and in the liver by 80%, and significantly decreased immature and mature ova ( P group. Additionally, the defatted methanolic extracts improved the reduced glutathione and malondialdehyde levels in hepatic tissues in the treated groups compared to the infected group. The HPLC-ESI-MS analysis of the Carica papaya defatted methanolic extract revealed the presence of several polyphenolic compounds. Carica papaya fruit extracts are rich with phenolic acids and flavonoids and show a significant effect against S. mansoni infections which may be used alternative to PZQ as anti-schistosomal drug against schistosomiasis. © Georg Thieme Verlag KG Stuttgart · New York.

  6. Routine low-level monitoring of polar pesticides and pesticide degradates by HPLC/ESI-MS: Evaluating long-term performance

    Science.gov (United States)

    Furlong, E.T.; Martin, Jeffrey D.; Werner, S.L.; Gates, Paul M.

    2002-01-01

    The sensitivity and selective determination of polar pesticides were analyzed using high-performance liquid chromatography/electrospray ionization-mass spectrometry (HPLC/ESI-MS). The effects of multiple operators and instruments on method performance were evaluated using 440 pairs of fortified reagent-water and blank reagent-water samples. The influence of varying environmental matrices on recovery and precision were also analyzed using 200 fortified ambient water samples and duplicate ambient water samples. The results show that compound stability in filtered water was matrix-, chemical class- and compound-dependent which ranged from 1 day to 2 weeks.

  7. NMR, ESI/MS, and MALDI-TOF/MS analysis of pear juice polymeric proanthocyanidins with potent free radical scavenging activity.

    Science.gov (United States)

    Es-Safi, Nour-Eddine; Guyot, Sylvain; Ducrot, Paul-Henri

    2006-09-20

    The structure of a polymeric proanthocyanidin fraction isolated from pear juice was characterized by NMR, ESI/MS, and MALDI-TOF/MS analyses, and its antioxidant activity was investigated using the DPPH free radical scavenging method. The results obtained from 13C NMR analysis showed the predominance of signals representative of procyanidins. Typical signals in the chemical shift region between 70 and 90 ppm demonstrated the exclusive presence of epicatechin units. The results obtained through negative ESI/MS analysis showed singly and doubly charged ions corresponding to the molecular mass of procyanidins with a degree of polymerization up to 22. The spectra obtained through MALDI-TOF/MS analysis revealed the presence of two series of tannin oligomers. Supporting the observations from NMR spectroscopy, the first series consists of well-resolved tannin identified as procyanidin polymers units with chain lengths of up to 25. A second series of monogalloyl flavan-3-ols polymers with polymerization degree up to 25 were also detected. This is the first mass spectrometric evidence confirming the existence of galloylated procyanidin oligomers in pear fruits. Within each of these oligomers, various signals exist suggesting the presence of several oligomeric tannins. The antioxidant properties of the polymeric fraction were investigated through reduction of the DPPH free radical, and the results obtained showed that the polymeric fraction exhibited a higher antioxidant power compared to those of (+)-catechin and B3 procyanidin dimer.

  8. Comparison of the effects of Mylabris and Acanthopanax senticosus on promising cancer marker polyamines in plasma of a Hepatoma-22 mouse model using HPLC-ESI-MS.

    Science.gov (United States)

    Wang, Qian; Wang, Yixiang; Liu, Ran; Yan, Xu; Li, Yujiao; Fu, Hui; Bi, Kaishun; Li, Qing

    2013-02-01

    A simple and sensitive method for the simultaneous determination of plasma concentrations of five polyamines in normal and Hepatoma-22 mice, and mice treated with Mylabris and Acanthopanax senticosus was developed by HPLC-ESI-MS. Male Kunming mice were divided into nine groups, a control group (inoculation without treatment), a positive group (Cyclophosphamide), treatment groups [Mylabris (4, 8, 16 mg/kg), Acanthopanax senticosus (6, 12, 24 g/kg)] and a normal group (without inoculation). Twenty-four hours after the last administration, plasma samples were collected. The derived polyamines were separated on a C(18) column by a gradient elution using methanol-water with excellent linearity within the range from 2.5 to 1000 ng/mL. Polyamines were confirmed as useful biochemical markers of hepatoma. The differences in anti-cancer therapeutic efficacy between Mylabris and Acanthopanax senticosus might contribute to the variability of polyamine levels in vivo. This HPLC-ESI-MS method was successfully applied to investigate the relationship between polyamines and cancer in mice and might be a useful method to test the activity of potential anti-tumor drugs. Copyright © 2012 John Wiley & Sons, Ltd.

  9. Intoxicación letal con aldicarb: análisis de sangre post mortem mediante LC-ESI-MS/MS

    Directory of Open Access Journals (Sweden)

    Diana Jazmín Mariño Gaviria

    2015-07-01

    Full Text Available El Aldicarb es un plaguicida carbamato de alta toxicidad asociado a intoxicaciones agudas fatales en Colombia.  El presente estudio describe un método analítico para la determinación cuantitativa de aldicarb en sangre postmortem.  Básicamente el método consiste en una precipitación de proteínas de la sangre para luego ser analizada por LC-ESI-MS/MS utilizando el aldicarb-d3 como estándar interno. El método desarrollado en este trabajo fue aplicado a siete casos de intoxicación letal presuntamente con este plaguicida. El aldicarb se encontró en sangre en niveles desde 0,10 y 2,5 µg/mL. De los resultados obtenidos no sólo se expone la utilidad de emplear LC-ESI-MS/MS en el análisis de aldicarb en sangre para su aplicación en toxicología forense con el propósito de contribuir a la búsqueda de la causa de muerte, sino que además evidencia el empleo de este plaguicida en actos suicidas.

  10. Determinants for Tight and Selective Binding of a Medicinal Dicarbene Gold(I) Complex to a Telomeric DNA G-Quadruplex: a Joint ESI MS and XRD Investigation.

    Science.gov (United States)

    Bazzicalupi, Carla; Ferraroni, Marta; Papi, Francesco; Massai, Lara; Bertrand, Benoît; Messori, Luigi; Gratteri, Paola; Casini, Angela

    2016-03-18

    The dicarbene gold(I) complex [Au(9-methylcaffein-8-ylidene)2 ]BF4 is an exceptional organometallic compound of profound interest as a prospective anticancer agent. This gold(I) complex was previously reported to be highly cytotoxic toward various cancer cell lines in vitro and behaves as a selective G-quadruplex stabilizer. Interactions of the gold complex with various telomeric DNA models have been analyzed by a combined ESI MS and X-ray diffraction (XRD) approach. ESI MS measurements confirmed formation of stable adducts between the intact gold(I) complex and Tel 23 DNA sequence. The crystal structure of the adduct formed between [Au(9-methylcaffein-8-ylidene)2 ](+) and Tel 23 DNA G-quadruplex was solved. Tel 23 maintains a characteristic propeller conformation while binding three gold(I) dicarbene moieties at two distinct sites. Stacking interactions appear to drive noncovalent binding of the gold(I) complex. The structural basis for tight gold(I) complex/G-quadruplex recognition and its selectivity are described. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Confirmation of Fructans biosynthesized in vitro from [1-13C]glucose in asparagus tissues using MALDI-TOF MS and ESI-MS.

    Science.gov (United States)

    Suzuki, Takashi; Maeda, Tomoo; Grant, Suzanne; Grant, Gordon; Sporns, Peter

    2013-05-15

    Accumulation of Fructans was confirmed in asparagus tissues that had been cultured for 2 days on media supplemented with glucose. It is very common that Fructans are biosynthesized from sucrose. We hypothesized however that Fructans could also be biosynthesized from glucose. Stem tissues of in vitro-cultured asparagus were subcultured for 72 h on a medium containing 0.5M of [1-(13)C]glucose. A medium containing 0.5M of normal ((12)C) glucose was used as control. Carbohydrates were extracted from the tissues and analyzed using HPLC, MALDI-TOF MS and ESI-MS. HPLC results indicated that the accumulation of short-chain Fructans was similar in both (13)C-labelled and control samples. Short-chain Fructans of DP=3-7 were detected using MALDI-TOF MS. The molecular mass of each oligomer in the (13)C-labelled sample was higher than the mass of the natural sample by 1 m/z unit per sugar moiety. The results of ESI-MS on the HPLC fractions of neokestose and 1-kestose showed that these oligomers (DP=3) were biosynthesized from exogenous glucose added to the medium. We conclude that not only exogenous sucrose but glucose can induce Fructan biosynthesis; fructans of both inulin type and inulin neoseries are also biosynthesized from glucose accumulated in asparagus tissues; the glucose molecules (or its metabolic products) were incorporated into Fructans as structural monomers. Copyright © 2013 Elsevier GmbH. All rights reserved.

  12. Use of ESI-MS to determine reaction pathway for hydrogen sulphide scavenging with 1,3,5-tri-(2-hydroxyethyl)-hexahydro-s-triazine.

    Science.gov (United States)

    Madsen, Henrik T; Søgaard, Erik G

    2012-01-01

    To study the reaction between hydrogen sulphide and 1,3,5-tri-(2-hydroxyethyl)-hexahydro-s-triazine, which is an often used hydrogen sulphide scavenger, electro spray ionisation mass spectrometry (ESI-MS) was used. The investigation was carried out in positive mode, and tandem mass spectrometry was used to investigate the nature of unknown peaks in the mass spectra. The reaction was found to proceed as expected from theory with the triazine reacting with hydrogen sulphide to form the corresponding thiadiazine. This species subsequently reacted with a second hydrogen sulphide molecule to form the dithiazine species, hereby confirming previously obtained results and showing the ability of the ESI-MS method for studying the scavenging reaction. The final theoretical product s-trithiane was not detected. Furthermore, fragmentation products of thiadiazine and dithiazine were detected in the solution, and possible pathways and structures were suggested to describe the observed fragments. In these, thiadiazine fragmented to 2-(methylidene amino)-ethanol and 2-(1,3-thiazetidin-3-yl)-ethanol and N-(2-hydroxyethyl)-N-(sulfanylmethyl)-ethaniminium, which underwent a further fragmentation to N-methyl-N-(2-oxoethyl)-methaniminium. Dithiazine fragmented to N-methyl-N-(2-oxoethyl)-methaniminium as well. The by-product from this reaction is methanedithiol, which was not detected due to its low polarity.

  13. Structural investigations of flavonol glycosides from sea buckthorn (Hippophaë rhamnoides) pomace by NMR spectroscopy and HPLC-ESI-MS(n).

    Science.gov (United States)

    Rösch, Daniel; Krumbein, Angelika; Mügge, Clemens; Kroh, Lothar W

    2004-06-30

    Four flavonol glycosides were isolated from an extract of sea buckthorn pomace (Hippophaë rhamnoides) by Sephadex LH-20 gel chromatography and semipreparative HPLC. Their structures were elucidated by hydrolysis studies, ESI-MS(n), UV, and (1)H and (13)C NMR spectroscopy. The occurrence of the major flavonol glycoside kaempferol 3-O-beta-sophoroside-7-O-alpha-rhamnoside in sea buckthorn is described here for the first time. A further 21 flavonol glycosides of Sephadex LH-20 fractions of sea buckthorn pomace were characterized by HPLC-DAD-ESI-MS. The characteristic MS-MS and MS(3) fragmentation pattern of flavonol glycosides previously identified in sea buckthorn juice and of flavonol glycosides identified by NMR spectroscopy gave valuable indications for their identification. The results demonstrate that loss of the sugar moiety from C-7 of the aglycon is more favored than fission of the glycosidic linkage at the C-3 position. Thus, most of the compounds identified were 7-rhamnosides of isorhamnetin, kaempferol, and quercetin, which exhibit different substitution patterns at the C-3 position, mainly glucosides, rutinosides, and sophorosides. In addition, numerous flavonol glycosides were detected lacking a sugar moiety at C-7. Finally, eight flavonol derivatives were identified that are acylated by hydroxybenzoic or hydoxycinnamic acids.

  14. Simultaneous Release and Labeling of O- and N-Glycans Allowing for Rapid Glycomic Analysis by Online LC-UV-ESI-MS/MS.

    Science.gov (United States)

    Wang, Chengjian; Lu, Yu; Han, Jianli; Jin, Wanjun; Li, Lingmei; Zhang, Ying; Song, Xuezheng; Huang, Linjuan; Wang, Zhongfu

    2018-05-24

    Most glycoproteins and biological protein samples undergo both O- and N-glycosylation, making characterization of their structures very complicated and time-consuming. Nevertheless, to fully understand the biological functions of glycosylation, both the glycosylation forms need to be analyzed. Herein we report a versatile, convenient one-pot method in which O- and N-glycans are simultaneously released from glycoproteins and chromogenically labeled in situ and thus available for further characterization. In this procedure, glycoproteins are incubated with 1-phenyl-3-methyl-5-pyrazolone (PMP) in aqueous ammonium hydroxide, making O-glycans released from protein backbones by β-elimination and N-glycans liberated by alkaline hydrolysis. The released glycans are promptly derivatized with PMP in situ by Knoevenagel condensation and Michael addition, with peeling degradation almost completely prevented. The recovered mixture of O- and N-glycans as bis-PMP derivatives features strong ultraviolet (UV) absorbing ability and hydrophobicity, allowing for high-resolution chromatographic separation and high-sensitivity spectrometric detection. Using this technique, O- and N-glycans were simultaneously prepared from some model glycoproteins and complex biological samples, without significant peeling, desialylation, deacetylation, desulfation or other side-reactions, and then comprehensively analyzed by online HILIC-UV-ESI-MS/MS and RP-HPLC-UV-ESI-MS/MS, with which some novel O- and N-glycan structures were first found. This method provides a simple, versatile strategy for high-throughput glycomics analysis.

  15. Propiedades Físico-químicas por RMN de 1H y Constituyentes en el Aceite de Carapa guianensis por ESI-MS

    Directory of Open Access Journals (Sweden)

    Elson Farias Silva

    2015-01-01

    Full Text Available The Andiroba belongs to the botanical family Meliaceae, found in the Amazon mainly two varieties, Carapa guianensis and C. procera. They are species with large logging utility and extracted oil has many uses, especially in lighting, such as healing use, insecticide and anti-inflammatory. In this paper the physico-chemical properties of oil of C. guianensis in São João da Beacon, Roraima through calculations from 1H NMR spectrum using the computer program PROTÓLEOS properties are studied by ESI-MS technique to determine the constituents of said oil are linolenic acid (9.99%, linoleic acid (13.14%, oleic acid (47.32%, unsaturated (70.45% fatty acid and saturated fatty acids (29.55%. The extracted oil of andiroba oil has a yield of 67.03% being the physicochemical properties of the oil as follows: 48.4 mg I2 / g of iodine; 161.67 mg KOH / g of saponification; 1.84% of acid; 1004.02 g / mol average molecular weight; 159.83 mg KOH / g of ester value; 98.87% percent of ester and 0.9166 g / cm3 for the density at 25 ° C. Constituents determined by ESI-MS include: 1,1'-methyl-2,2'-dicarboxylate diantraquinona, dimethyl pirofosfatosantoninate, 2,4,6-tris- (3,5-di-butyl-4-tec -hidroxibencil styrene, (2,3,7,8,12,13,17,18-octanoilporfirinate -Mg (II.

  16. [Fe(F20 TPP)Cl]-catalyzed amination with arylamines and {[Fe(F20 TPP)(NAr)](PhI=NAr)} + . Intermediate assessed by high-resolution ESI-MS and DFT calculations.

    Science.gov (United States)

    Liu, Yungen; Chen, Guo-Qiang; Tse, Chun-Wai; Guan, Xianguo; Xu, Zheng-Jiang; Huang, Jie-Sheng; Che, Chi-Ming

    2015-01-01

    Amination of CH bonds catalyzed by transition metal complexes via nitrene/imide insertion is an appealing strategy for CN bond formation, and the use of iminoiodinanes, or their in situ generated forms from 'PhI(OAc)2 +primary amides (such as sulfonamides, sulfamates, and carbamates)', as nitrogen sources for the amination reaction has been well documented. In this work, a 'metal catalyst+PhI(OAc)2 +primary arylamines' amination protocol has been developed using [Fe(F20 TPP)Cl] (H2 F20 TPP=meso-tetrakis(pentafluorophenyl)porphyrin) as a catalyst. This catalytic method is applicable for both intra- and intermolecular amination of sp(2) and sp(3) CH bonds (>27 examples), affording the amination products, including natural products such as rutaecarpine, in moderate-to-good yields. ESI-MS analysis and DFT calculations lend support for the involvement of {[Fe(F20 TPP)(NC6 H4 -p-NO2 )](PhI=NC6 H4 -p-NO2 )} + . intermediate in the catalysis. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. ESI-MSn and LC-ESI-MS studies to characterize forced degradation products of bosentan and a validated stability-indicating LC-UV method.

    Science.gov (United States)

    Bansal, Gulshan; Singh, Ranjit; Saini, Balraj; Bansal, Yogita

    2013-01-01

    The present study reports the characterization of forced degradation products of bosentan and a validated stability-indicating HPLC method for the stability testing of bosentan tablets. The forced degradation was carried out under the conditions of hydrolysis, oxidation, dry heat and photolysis. The drug was found unstable in acid, alkali and oxidative media whereas stable to the hydrolysis in water, to dry heat and to photolysis. In total, six degradation products were formed in all conditions which were resolved in a single run on a C-18 column with gradient elution using ammonium acetate buffer (pH 4.5, 5.0mM), methanol and acetonitrile. Structures of all the degradation products were characterized through +ESI-MS(n) and LC-ESI-MS spectral data of bosentan as well as LC-ESI-MS spectral data of the products. The products II-VI were characterized as 6-amino-[2,2']bipyrimidinyl-4,5-diol, 6-amino-5-(2-methoxyphenoxy)-[2,2']-bipyrimidinyl-4-ol, 2-[6-amino-5-(2-methoxyphenoxy)-[2,2']-bipyrimidinyl-4-yloxy]-ethanol, 4-tert-butyl-N-[6-(1-methoxyethoxy)-5-(2-methoxyphenoxy)-[2,2']-bipyrimidinyl-4-yl]-benzenesulfonamide and 4-tert-butyl-N-[6-hydroxy-5-(2-methoxyphenoxy)-[2,2']bipyrimidinyl-4-yl]-benzenesulfonamide, respectively. The peak of the product I was found to be due to two secondary degradation products which co-eluted and were characterized as β-hydroxyethyl p-tert-butylphenylsulfonate (Ia) and 2-[2-(2-hydroxyethoxy)-phenoxy]-ethanol (Ib). These products were formed due to hydrolysis of sulfonamide and alkylaryl ether and the diaryl ether linkages as well as dehydration of the primary alcohol group. The most probable degradation mechanisms were proposed. The HPLC method was found to be stability-indicating, linear (2-100 μg ml(-1)), accurate, precise, sensitive, specific, rugged and robust for quantitation of the drug. The method was applied to the stability testing of the commercially available bosentan tablets successfully. Copyright © 2012 Elsevier B.V. All

  18. ESI-MS/MS Identification of a Bradykinin-Potentiating Peptide from Amazon Bothrops atrox Snake Venom Using a Hybrid Qq-oaTOF Mass Spectrometer

    Science.gov (United States)

    Coutinho-Neto, Antonio; Caldeira, Cleópatra A. S.; Souza, Gustavo H. M. F.; Zaqueo, Kayena D.; Kayano, Anderson M.; Silva, Rodrigo S.; Zuliani, Juliana P.; Soares, Andreimar M.; Stábeli, Rodrigo G.; Calderon, Leonardo A.

    2013-01-01

    A bradykinin-potentiating peptide (BPP) from Amazon Bothrops atrox venom with m/z 1384.7386 was identified and characterized by collision induced dissociation (CID) using an ESI-MS/MS spectra obtained in positive ion mode on a hybrid Qq-oaTOF mass spectrometer, Xevo G2 QTof MS (Waters, Manchester, UK). De novo peptide sequence analysis of the CID fragmentation spectra showed the amino acid sequence ZKWPRPGPEIPP, with a pyroglutamic acid and theoretical monoisotopic m/z 1384.7378, which is similar to experimental data, showing a mass accuracy of 0.6 ppm. The peptide is homologous to other BPP from Bothrops moojeni and was named as BPP-BAX12. PMID:23430539

  19. End-group characterisation of poly(propylene glycol)s by means of electrospray ionisation-tandem mass spectrometry (ESI-MS/MS).

    Science.gov (United States)

    Jackson, Anthony T; Slade, Susan E; Thalassinos, Konstantinos; Scrivens, James H

    2008-10-01

    The end-group functionalisation of a series of poly(propylene glycol)s has been characterised by means of electrospray ionisation-tandem mass spectrometry (ESI-MS/MS). A series of peaks with mass-to-charge ratios that are close to that of the precursor ion were used to generate information on the end-group functionalities of the poly(propylene glycol)s. Fragment ions resulting from losses of both of the end groups were noted from some of the samples. An example is presented of how software can be used to significantly reduce the length of time involved in data interpretation (which is typically the most time-consuming part of the analysis).

  20. Cytotoxic activity of carotenoid rich fractions from Haematococcus pluvialis and Dunaliella salina microalgae and the identification of the phytoconstituents using LC-DAD/ESI-MS.

    Science.gov (United States)

    El-Baz, Farouk K; Hussein, Rehab A; Mahmoud, Khaled; Abdo, Sayeda M

    2018-02-01

    Microalgae represent a rich source that satisfies the growing need for novel ingredients of nutriceuticals, pharmaceuticals, and food supplements. Haematococcus pluvialis and Dunaliella salina microalgae are isolated from the Egyptian hydro-flora and are reported for their potent antioxidant activities. The cytotoxic activity of different fractions of both microalgae was investigated on 4 cell lines HePG2, MCF7, HCT116, and A549. The carotenoid rich fraction of H. pluvialis showed potent cytotoxic activity against colon cancer cell line and moderate activity against both liver and breast cancer cell lines. On the other hand, the carotenoid rich fraction of D. salina showed mild cytotoxic activity on breast and liver cancer cell lines. The carotenoid rich fraction of H. pluvialis was analysed using LC-DAD/ESI-MS and the major carotenoids were identified either free as well as bounded to fatty acids. Copyright © 2017 John Wiley & Sons, Ltd.

  1. Isolation by pressurised fluid extraction (PFE) and identification using CPC and HPLC/ESI/MS of phenolic compounds from Brazilian cherry seeds (Eugenia uniflora L.).

    Science.gov (United States)

    Oliveira, Alessandra L; Destandau, Emilie; Fougère, Laëtitia; Lafosse, Michel

    2014-02-15

    Brazilian cherry seeds are a waste product from juice and frozen pulp production and, the seeds composition was investigated to valorize this by-product. Compounds separation was performed with ethanol by pressurised fluid extraction (PFE). Here we determine the effect of temperature (T), static time (ST), number of cycles (C), and flush volume (VF) on the yield, composition and total phenolic content (TPC) of the seed extracts. T, ST and their interaction positively influenced yield and TPC. Extracts were fractionated by high performance liquid chromatography (HPLC) and centrifugal partition chromatography (CPC). The collected fractions characterizations were made by electrospray ionisation mass spectrometry (ESI/MS) and high resolution mass spectrometry (HRMS) indicated the presence of ellagic acid pentoside and deoxyhexose, quercitrin and kaempferol pentoside. All of these compounds have antioxidant properties and normally are found in plant extracts. These results confirm that Brazilian cherry seed extract is a potentially valuable source of antioxidants. Copyright © 2013 Elsevier Ltd. All rights reserved.

  2. The integrated quality assessment of Chinese commercial dry red wine based on a method of online HPLC-DAD-CL combined with HPLC-ESI-MS.

    Science.gov (United States)

    Yu, Hai-Xiang; Sun, Li-Qiong; Qi, Jin

    2014-07-01

    To apply an integrated quality assessment strategy to investigate the quality of multiple Chinese commercial dry red wine samples. A comprehensive method was developed by combining a high performance liquid chromatography-diode array detector-chemiluminescence (HPLC-DAD-CL) online hyphenated system with an HPLC-ESI-MS technique. Chromatographic and H2O2-scavenging active fingerprints of thirteen batches of different, commercially available Chinese dry red wine samples were obtained and analyzed. Twenty-five compounds, including eighteen antioxidants were identified and evaluated. The dominant and characteristic antioxidants in the samples were identified. The relationships between antioxidant potency and the cultivated variety of grape, producing area, cellaring period, and trade mark are also discussed. The results provide the feasibility for an integrated quality assessment strategy to be efficiently and objectively used in quality (especially antioxidant activity) assessment and identification of dry red wine. Copyright © 2014 China Pharmaceutical University. Published by Elsevier B.V. All rights reserved.

  3. Pharmacokinetic Comparative Study of Gastrodin and Rhynchophylline after Oral Administration of Different Prescriptions of Yizhi Tablets in Rats by an HPLC-ESI/MS Method

    Science.gov (United States)

    Ge, Zhaohui; Liang, Qionglin; Wang, Yiming; Luo, Guoan

    2014-01-01

    Pharmacokinetic characters of rhynchophylline (RIN), gastrodin (GAS), and gastrodigenin (p-hydroxybenzyl alcohol, HBA) were investigated after oral administration of different prescriptions of Yizhi: Yizhi tablets or effective parts of tianma (total saponins from Gastrodiae, EPT) and gouteng (rhynchophylla alkaloids, EPG). At different predetermined time points after administration, the concentrations of GAS, HBA, and RIN in rat plasma were determined by an HPLC-ESI/MS method, and the main pharmacokinetic parameters were investigated. The results showed that the pharmacokinetic parameters C max and AUC0–∞ (P < 0.05) were dramatically different after oral administration of different prescriptions of Yizhi. The data indicated that the pharmacokinetic processes of GAS, HBA, and RIN in rats would interact with each other or be affected by other components in Yizhi. The rationality of the compatibility of Uncaria and Gastrodia elata as a classic “herb pair” has been verified from the pharmacokinetic viewpoint. PMID:25610474

  4. Pharmacokinetic Comparative Study of Gastrodin and Rhynchophylline after Oral Administration of Different Prescriptions of Yizhi Tablets in Rats by an HPLC-ESI/MS Method

    Directory of Open Access Journals (Sweden)

    Zhaohui Ge

    2014-01-01

    Full Text Available Pharmacokinetic characters of rhynchophylline (RIN, gastrodin (GAS, and gastrodigenin (p-hydroxybenzyl alcohol, HBA were investigated after oral administration of different prescriptions of Yizhi: Yizhi tablets or effective parts of tianma (total saponins from Gastrodiae, EPT and gouteng (rhynchophylla alkaloids, EPG. At different predetermined time points after administration, the concentrations of GAS, HBA, and RIN in rat plasma were determined by an HPLC-ESI/MS method, and the main pharmacokinetic parameters were investigated. The results showed that the pharmacokinetic parameters Cmax and Cmax⁡ and AUC0–∞ (P<0.05 were dramatically different after oral administration of different prescriptions of Yizhi. The data indicated that the pharmacokinetic processes of GAS, HBA, and RIN in rats would interact with each other or be affected by other components in Yizhi. The rationality of the compatibility of Uncaria and Gastrodia elata as a classic “herb pair” has been verified from the pharmacokinetic viewpoint.

  5. Identification and quantification of metallothionein isoforms and superoxide dismutase in spiked liver extracts using HPLC-ESI-MS offline coupling and HPLC-ICP-MS online coupling.

    Science.gov (United States)

    Nischwitz, V; Michalke, B; Kettrup, A

    2003-01-01

    A two-dimensional chromatographic method for the characterization of metallothionein isoforms (MT) and superoxide dismutase (SOD) in spiked liver extracts was developed for the optimization of extraction procedures from liver samples. Element-specific detection (ICP-MS) and molecule-specific detection (ESI-MS) were applied for maximum species information. A special focus was laid on the quantitative data evaluation (species stoichiometry, calibration with and without matrix, recovery), which is neglected in most MT/SOD publications with hyphenated techniques. Linearity, precision (residual standard deviation of calibration curves <10%), and detection limits (<0.6 mg L(-1) for MT isoforms and 13 mg L(-1) for SOD) prove the suitability of the method for quantification. An alternative quantification is proposed for the extension towards other lesser or even unknown trace element species, especially the native porcine MT and SOD.

  6. High throughput HPLC-ESI(-)-MS/MS methodology for mercapturic acid metabolites of 1,3-butadiene: Biomarkers of exposure and bioactivation.

    Science.gov (United States)

    Kotapati, Srikanth; Esades, Amanda; Matter, Brock; Le, Chap; Tretyakova, Natalia

    2015-11-05

    1,3-Butadiene (BD) is an important industrial and environmental carcinogen present in cigarette smoke, automobile exhaust, and urban air. The major urinary metabolites of BD in humans are 2-(N-acetyl-L-cystein-S-yl)-1-hydroxybut-3-ene/1-(N-acetyl-L-cystein-S-yl)-2-hydroxybut-3-ene (MHBMA), 4-(N-acetyl-L-cystein-S-yl)-1,2-dihydroxybutane (DHBMA), and 4-(N-acetyl-L-cystein-S-yl)-1,2,3-trihydroxybutyl mercapturic acid (THBMA), which are formed from the electrophilic metabolites of BD, 3,4-epoxy-1-butene (EB), hydroxymethyl vinyl ketone (HMVK), and 3,4-epoxy-1,2-diol (EBD), respectively. In the present work, a sensitive high-throughput HPLC-ESI(-)-MS/MS method was developed for simultaneous quantification of MHBMA and DHBMA in small volumes of human urine (200 μl). The method employs a 96 well Oasis HLB SPE enrichment step, followed by isotope dilution HPLC-ESI(-)-MS/MS analysis on a triple quadrupole mass spectrometer. The validated method was used to quantify MHBMA and DHBMA in urine of workers from a BD monomer and styrene-butadiene rubber production facility (40 controls and 32 occupationally exposed to BD). Urinary THBMA concentrations were also determined in the same samples. The concentrations of all three BD-mercapturic acids and the metabolic ratio (MHBMA/(MHBMA+DHBMA+THBMA)) were significantly higher in the occupationally exposed group as compared to controls and correlated with BD exposure, with each other, and with BD-hemoglobin biomarkers. This improved high throughput methodology for MHBMA and DHBMA will be useful for future epidemiological studies in smokers and occupationally exposed workers. Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.

  7. Randomized double-blinded pilot clinical study of the antidiabetic activity of Balanites aegyptiaca and UPLC-ESI-MS/MS identification of its metabolites.

    Science.gov (United States)

    Rashad, Hend; Metwally, Fateheya M; Ezzat, Shahira M; Salama, Maha M; Hasheesh, Adel; Abdel Motaal, Amira

    2017-12-01

    Balanites aegyptiaca Del. (Zygophyllaceae) fruits are traditionally known for the treatment of hyperglycaemia. Several in vitro and in vivo studies proposed some mechanisms of action. However, clinical trials in human beings were never reported to date. To investigate the antidiabetic efficacy of the 70% ethanol extract of the pericarps of B. aegyptiaca (BE) within a nutritional intervention in elderly people. Ultra-performance electrospray ionization-mass spectroscopy (UPLC-ESI-MS/MS) analysis was used for metabolic profiling of BE which was incorporated in hard gelatine capsules (400 mg/day) and tested on 30 type 2 diabetes (T2D) Egyptian patients for 8 weeks. According to sex, age and body mass index participants were divided into two equivalent groups, placebo and treatment. Thirteen compounds were identified in BE using UPLC-ESI-MS/MS analysis among which five steroidal saponins, seven phenolic compounds and a sterol glucoside. At the end of the 8-week treatment, the treated group showed 26.88% decrease in 2 h postprandial plasma glucose relative to 2.6% increase in the placebo group, while fasting plasma glucose was reduced to 10.3%. Treatment with BE capsules for 8 weeks produced significant reduction in the plasma triglyceride, total cholesterol and low-density lipoprotein cholesterol by 9.0, 12.76 and 21.35%, respectively, with 29.8% increase in the high-density lipoprotein cholesterol. Plasma alanine transaminase and aspartate transaminase were reduced by 42.6 and 43.3%, respectively. Administration of the BE capsules to T2D resulted in significant improvements in the glycaemic markers and the lipid profile, without adverse effects or hypoglycaemia.

  8. HepG2 cells biospecific extraction and HPLC-ESI-MS analysis for screening potential antiatherosclerotic active components in Bupeuri radix.

    Science.gov (United States)

    Liu, Shuqiang; Tan, Zhibin; Li, Pingting; Gao, Xiaoling; Zeng, Yuaner; Wang, Shuling

    2016-03-20

    HepG2 cells biospecific extraction method and high performance liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS) analysis was proposed for screening of potential antiatherosclerotic active components in Bupeuri radix, a well-known Traditional Chinese Medicine (TCM). The hypothesis suggested that when cells are incubated together with the extracts of TCM, the potential bioactive components in the TCM should selectively combine with the receptor or channel of HepG2 cells, then the eluate which contained biospecific component binding to HepG2 cells was identified using HPLC-ESI-MS analysis. The potential bioactive components of Bupeuri radix were investigated using the proposed approach. Five compounds in the saikosaponins of Bupeuri radix were detected as these components selectively combined with HepG2 cells, among these compounds, two potentially bioactive compounds namely saikosaponin b1 and saikosaponin b2 (SSb2) were identified by comparing with the chromatography of the standard sample and analysis of the structural clearance characterization of MS. Then SSb2 was used to assess the uptake of DiI-high density lipoprotein (HDL) in HepG2 cells for antiatherosclerotic activity. The results have showed that SSb2, with indicated concentrations (5, 15, 25, and 40 μM) could remarkably uptake dioctadecylindocarbocyanine labeled- (DiI) -HDL in HepG2 cells (Vs control group, *PESI-MS analysis is a rapid, convenient, and reliable method for screening potential bioactive components in TCM and SSb2 may be a valuable novel drug agent for the treatment of atherosclerosis. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. HPLC-DAD-ESI-MS/MS analysis of fruits from Firmiana simplex (L.) and evaluation of their antioxidant and antigenotoxic properties.

    Science.gov (United States)

    Ghareeb, Mosad Ahmed; Mohamed, Tamer; Saad, Amal Mohamed; Refahy, Laila Abdel-Ghany; Sobeh, Mansour; Wink, Michael

    2018-01-01

    The secondary metabolites of the fruits of Firmiana simplex (L.) were analysed by LC-DAD-ESI-MS/MS; furthermore, we evaluated their antioxidant and antigenotoxic properties. The antioxidant activity was investigated using the 2,2'-diphenyl-1-picrylhydrazyl radical (DPPH), the 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid) diammonium salt (ABTS) and the ferric reducing antioxidant power (FRAP) assays. The antigenotoxic potential was determined via the comet assay. The ethyl acetate fraction (EtOAc) was analysed by LC-DAD-ESI-MS/MS: phenolic acids and flavonoids were the main polyphenols of the fruits. The EtOAc fraction yielded the highest content of polyphenols with 314.61 mg GAE/g extract, followed by 297.51, 153.75, 101.47, 97.19 for dichloromethane, butanol, methanol and water extracts, respectively. As expected, a strong correlation exists between the antioxidant activity of the investigated extracts and their total phenolic content. In the DPPH assay, the IC 50 value of the most active EtOAc fraction was 6.79 μg/ml, relative to 2.92 μg/ml of the standard ascorbic acid. ABTS and FRAP assays supported the results of DPPH assay. Moreover, using the comet assay, we could show that the phenol-rich EtOAc extract exhibits an antigenotoxic potential in human liver cancer cells (Hep-G2) treated with hydrogen peroxide (H 2 O 2 ) as a genotoxic agent. The fruits of Firmiana simplex may be a good natural source of antioxidant and antigenotoxic agents. © 2017 Royal Pharmaceutical Society.

  10. Determination of phosphatidylethanolamine molecular species in various food matrices by liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS2).

    Science.gov (United States)

    Zhou, Li; Zhao, Minjie; Ennahar, Saïd; Bindler, Françoise; Marchioni, Eric

    2012-04-01

    A liquid chromatographic-electrospray ionization-tandem mass spectrometric (LC-ESI-MS(2)) method has been developed for determination of the molecular species of phosphatidylethanolamine (PE) in four food matrices (soy, egg yolk, ox liver, and krill oil). The extraction and purification method consisted of a pressurized liquid extraction procedure for total lipid (TL) extraction, purification of phospholipids (PLs) by adsorption on a silica gel column, and separation of PL classes by semi-preparative normal-phase HPLC. Separation and identification of PE molecular species were performed by reversed-phase HPLC coupled with electrospray ionization tandem mass spectrometry (ESI-MS(2)). Methanol containing 5 mmol L(-1) ammonium formate was used as the mobile phase. A variety of PE molecular species were detected in the four food matrices. (C16:0-C18:2)PE, (C18:2-C18:2)PE, and (C16:0-C18:1)PE were the major PE molecular species in soy. Egg yolk PE contained (C16:0-C18:1)PE, (C18:0-C18:1)PE, (C18:0-C18:2)PE, and (C16:0-C18:2)PE as the major molecular species. Ox liver PE was rich in the species (C18:0-C18:1)PE, (C18:0-C20:4)PE, and (C18:0-C18:2)PE. Finally, krill oil which was particularly rich in (C16:0(alkyl)-C22:6(acyl))plasmanylethanolamine (PakE), (C16:0-C22:6)PE, and (C16:0-C20:5)PE, seemed to be an interesting potential source for supplementation of food with eicosapentaenoic acid and docosahexaenoic acid.

  11. Characterization of a PEGylated protein therapeutic by ion exchange chromatography with on-line detection by native ESI MS and MS/MS.

    Science.gov (United States)

    Muneeruddin, K; Bobst, C E; Frenkel, R; Houde, D; Turyan, I; Sosic, Z; Kaltashov, I A

    2017-01-16

    Detailed profiling of both enzymatic (e.g., glycosylation) and non-enzymatic (e.g., oxidation and deamidation) post-translational modifications (PTMs) is frequently required for the quality assessment of protein-based drugs. Challenging as it is, this task is further complicated for the so-called second-generation biopharmaceuticals, which also contain "designer PTMs" introduced to either enhance their pharmacokinetic profiles (e.g., PEGylated proteins) or endow them with therapeutic activity (e.g., protein-drug conjugates). Such modifications of protein covalent structure can dramatically increase structural heterogeneity, making the very notion of "molecular mass" meaningless, as ions representing different glycoforms of a PEGylated protein may have nearly identical distributions of ionic current as a function of m/z, making their contributions to the mass spectrum impossible to distinguish. In this work we demonstrate that a combination of ion exchange chromatography (IXC) with on-line detection by electrospray ionization mass spectrometry (ESI MS) and methods of ion manipulation in the gas phase (limited charge reduction and collision-induced dissociation) allows meaningful structural information to be obtained on a structurally heterogeneous sample of PEGylated interferon β-1a. IXC profiling of the protein sample gives rise to a convoluted chromatogram with several partially resolved peaks which can represent both deamidation and different glycosylation patterns within the protein, as well as varying extent of PEGylation. Thus, profiling the protein with on-line IXC/ESI/MS/MS allows it to be characterized by providing information on three different types of PTMs (designer, enzymatic and non-enzymatic) within a single protein therapeutic.

  12. Two-dimensional HPLC coupled to ICP-MS and electrospray ionisation (ESI)-MS/MS for investigating the bioavailability in vitro of arsenic species from edible seaweed

    Energy Technology Data Exchange (ETDEWEB)

    Garcia-Sartal, Cristina; Barciela-Alonso, Maria del Carmen; Bermejo-Barrera, Pilar [University of Santiago de Compostela, Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, Santiago de Compostela (Spain); Taebunpakul, Sutthinun [LGC Limited, Teddington, Middlesex (United Kingdom); Imperial College of Science, Technology and Medicine, South Kensington, Department of Materials, London (United Kingdom); National Institute of Metrology (Thailand), Pathumthani (Thailand); Stokes, Emma; Goenaga-Infante, Heidi [LGC Limited, Teddington, Middlesex (United Kingdom)

    2012-04-15

    Edible seaweed consumption is a route of exposure to arsenic. However, little attention has been paid to estimate the bioaccessibility and/or bioavailability of arsenosugars in edible seaweed and their possible degradation products during gastrointestinal digestion. This work presents first use of combined inductively coupled plasma mass spectroscopy (ICP-MS) with electrospray ionization tandem mass spectrometry (ESI-MS/MS) with two-dimensional HPLC (size exclusion followed by anion exchange) to compare the qualitative and quantitative arsenosugars speciation of different edible seaweed with that of their bioavailable fraction as obtained using an in vitro gastrointestinal digestion procedure. Optimal extraction conditions for As species from four seaweed namely kombu, wakame, nori and sea lettuce were selected as a compromise between As extraction efficiency and preservation of compound identity. For most investigated samples, the use of ammonium acetate buffer as extractant and 1 h sonication in a water bath followed by HPLC-ICP-MS resulted in 40-61% of the total As to be found in the buffered aqueous extract, of which 86-110% was present as arsenosugars (glycerol sugar, phosphate sugar and sulfonate sugar for wakame and kombu and glycerol sugar and phosphate sugar for nori). The exception was sea lettuce, for which the arsenosugar fraction (glycerol sugar, phosphate sugar) only comprised 44% of the total extracted As. Interestingly, the ratio of arsenobetaine and dimethylarsinic acid to arsenosugars in sea lettuce extracts seemed higher than that for the rest of investigated samples. After in vitro gastrointestinal digestion, approximately 11-16% of the total As in the solid sample was found in the dialyzates with arsenosugars comprising 93-120% and 41% of the dialyzable As fraction for kombu, wakame, nori and sea lettuce, respectively. Moreover, the relative As species distribution in seaweed-buffered extracts and dialyzates was found to be very similar

  13. HPLC-UV, MALDI-TOF-MS and ESI-MS/MS analysis of the mechlorethamine DNA crosslink at a cytosine-cytosine mismatch pair.

    Directory of Open Access Journals (Sweden)

    Pornchai Rojsitthisak

    Full Text Available Mechlorethamine [ClCH(2CH(2N(CH(3CH(2CH(2Cl], a nitrogen mustard alkylating agent, has been proven to form a DNA interstrand crosslink at a cytosine-cytosine (C-C mismatch pair using gel electrophoresis. However, the atomic connectivity of this unusual crosslink is unknown.HPLC-UV, MALDI-TOF-MS, and ESI-MS/MS were used to determine the atomic connectivity of the DNA C-C crosslink formed by mechlorethamine, MALDI-TOF-MS of the HPLC-purified reaction product of mechlorethamine with the DNA duplex d[CTCACACCGTGGTTC]•d[GAACCACCGTGTGAG] (underlined bases are a C-C mismatch pair indicated formation of an interstrand crosslink at m/z 9222.088 [M-2H+Na](+. Following enzymatic digestion of the crosslinked duplex by snake venom phosphodiesterase and calf intestinal phosphatase, ESI-MS/MS indicated the presence of dC-mech-dC [mech = CH(2CH(2N(CH(3CH(2CH(2] at m/z 269.2 [M](2+ (expected m/z 269.6, exact mass 539.27 and its hydrolytic product dC-mech-OH at m/z 329.6 [M](+ (expected m/z 329.2. Fragmentation of dC-mech-dC gave product ions at m/z 294.3 and 236.9 [M](+, which are both due to loss of the 4-amino group of cytosine (as ammonia, in addition to dC and dC+HN(CH(3CH = CH(2, respectively. The presence of m/z 269.2 [M](2+ and loss of ammonia exclude crosslink formation at cytosine N(4 or O(2 and indicate crosslinking through cytosine N(3 with formation of two quaternary ammonium ions.Our results provide an important addition to the literature, as the first example of the use of HPLC and MS for analysis of a DNA adduct at the N(3 position of cytosine.

  14. Isolation and determination of ivermectin in post-mortem and in vivo tissues of dung beetles using a continuous solid phase extraction method followed by LC-ESI+-MS/MS.

    Directory of Open Access Journals (Sweden)

    Antonio J Ortiz

    Full Text Available A new analytical method based on solvent extraction, followed by continuous solid-phase extraction (SPE clean-up using a polymeric sorbent, was demonstrated to be applicable for the detection of ivermectin in complex biological matrices of dung beetles (hemolymph, excreta or dry tissues using liquid chromatography combined with positive electrospray ionization tandem mass spectrometry (LC/ESI+-MS/MS. Using a signal-to-noise ratio of 3:1, the limit of detection (LOD in the insect matrices at trace levels was 0.01 ng g-1 and the limit of quantification (LOQ was 0.1 ng g-1. The proposed method was successfully used to quantitatively determine the levels of ivermectin in the analysis of small samples in in vivo and post mortem samples, demonstrating the usefulness for quantitative analyses that are focused on future pharmacokinetic and bioavailability studies in insects and the establishment of a new protocol to study the impact of ivermectin on non-target arthropods such as dung beetles and other insects that are related with the "dung community". Because satisfactory precision and accuracy values were obtained in both in vivo matrices, we suggest that the method can be consistently used for quantitative determinations that are focused on future pharmacokinetic and bioavailability studies in insects. Furthermore, this new analytical method was successfully applied to biological samples of dead dung beetles from the field suggesting that the method can be used to establish a new routine analysis of ivermectin residues in insect carcasses that is applied to complement typical mortality tests.

  15. Profiling of dehydropyrrolizidine alkaloids and their N-oxides in herbarium-preserved specimens of amsinckia species using HPLC-esi(+)MS.

    Science.gov (United States)

    Colegate, Steven M; Welsh, Stanley L; Gardner, Dale R; Betz, Joseph M; Panter, Kip E

    2014-07-30

    Species of the Amsinckia genus (Boraginaceae) are known to produce potentially hepato-, pneumo-, and/or genotoxic dehydropyrrolizidine alkaloids. However, the taxonomic differentiation of Amsinckia species can be very subtle and there seems to be marked differences in toxicity toward grazing livestock. Methanol extracts of mass-limited leaf samples from herbarium specimens (collected from 1899 to 2013) of 10 Amsinckia species and one variety were analyzed using HPLC-esi(+)MS and MS/MS for the presence of potentially toxic dehydropyrrolizidine alkaloids and/or their N-oxides. Dehydropyrrolizidine alkaloids were detected in all specimens examined ranging from about 1 to 4000 μg/g of plant. Usually occurring mainly as their N-oxides, the predominant alkaloids were the epimeric lycopsamine and intermedine. Also sometimes observed in higher concentrations were the 3'- and 7-acetyl derivatives of lycopsamine/intermedine and their N-oxides. Within a designated species, an inconsistent profile was often observed that may be due to natural variation, taxonomic misassignment, or nonuniform degradation due to plant collection and storage differences.

  16. Identification of some chemical constituents of Indigofera hirsuta Linn. (Fabaceae) by HPLC-ESI-MS (TOF) and evaluation of the anti radical activity

    International Nuclear Information System (INIS)

    Moura, Adriana Candido da Silva; Vilegas, Wagner; Santos, Lourdes Campaner dos

    2011-01-01

    A rapid analytical approach, suitable to characterize the compounds present in the aqueous and methanol extracts prepared from the aerial parts of Indigofera hirsute, was developed. The method based on high-performance liquid chromatography coupled to mass spectrometry, electrospray positive ionization and detection by time of flight (HPLC-ESI-MS-TOF) identified, tryptophan, uracil, rutin, kempferol-3-Oβ - -D-glucopyranoside, gallic acid and methyl gallate. The antiradical activity of this extract was evaluated using DPPH assay, with gallic acid as antiradical pattern. The study revealed the antiradical activity of methyl galatte (EC 50 = 5 ± 0.3 μg mL -1 ) gallic acid (EC 50 = 5 ± 0.2 μg mL -1 ) and rutin (EC 50 = 21.6 ± 0.6 μg m L -1 ), isolated from methanol extract (EC 50 = 67.7 ± 0.9 μg mL -1 ), which showed strong antiradical activity. (author)

  17. Phenolic Profiling of Duchesnea indica Combining Macroporous Resin Chromatography (MRC with HPLC-ESI-MS/MS and ESI-IT-MS

    Directory of Open Access Journals (Sweden)

    Mingzhi Zhu

    2015-12-01

    Full Text Available Duchesnea indica (D. indica is an important traditional Chinese medicine, and has long been clinically used to treat cancer in Asian countries. It has been described previously as a rich source of phenolic compounds with a broad array of diversified structures, which are the major active ingredients. However, an accurate and complete phenolic profiling has not been determined yet. In the present work, the total phenolic compounds in crude extracts from D. indica were enriched and fractionated over a macroporous resin column, then identified by HPLC-ESI-MS/MS and ESI-IT-MS (ion trap MS. A total of 27 phenolic compounds were identified in D. indica, of which 21 compounds were identified for the first time. These 27 phenolic compounds encompassing four phenolic groups, including ellagitannins, ellagic acid and ellagic acid glycosides, hydroxybenzoic acid and hydroxycinnamic acid derivatives, and flavonols, were then successfully quantified using peak areas against those of the corresponding standards with good linearity (R2 > 0.998 in the range of the tested concentrations. As a result, the contents of individual phenolic compounds varied from 6.69 mg per 100 g dry weight (DW for ellagic acid to 71.36 mg per 100 g DW for brevifolin carboxylate. Not only did this study provide the first phenolic profiling of D. indica, but both the qualitative identification and the subsequent quantitative analysis of 27 phenolic compounds from D. indica should provide a good basis for future exploration of this valuable medicinal plant.

  18. Ecdysteroids in Sida tuberculata R.E. Fries (Malvaceae): chemical composition by LC-ESI-MS and selective anti-Candida krusei activity.

    Science.gov (United States)

    da Rosa, Hemerson Silva; de Camargo, Vanessa Brum; Camargo, Graziela; Garcia, Cássia V; Fuentefria, Alexandre M; Mendez, Andreas S L

    2015-09-01

    Sida tuberculata is found in a region of South America and has traditionally been consumed as an infusion or tea. The chemical composition and antifungal activity of aqueous infusions from leaves and roots were investigated. LC-ESI-MS mass spectra were successfully obtained and used to identify four ecdysteroids: 20-hydroxyecdysone-3-O-β-D-glycopyranoside, 20-hydroxyecdysone, 20-hydroxyecdysone-3-O-β-D-xylose and a hydroxyecdysterone derivative. The in vitro antifungal activity was studied, and the minimal inhibitory concentration (MIC) and minimal fungicidal concentration (MFC) were established against Candida krusei isolates. The antibiofilm activity was evaluated by the determination of the biofilm removal efficiency in contaminated central venous catheter (CVC) coupons. The preparations exhibited antifungal activity against the species tested, with MICs ranging from 3.90 to 62.50 μg/ml. The infusion removed the C. krusei biofilm after 90 min of exposure. The observed bioactivity and composition of ecdysteroids will contribute to the future development of antifungal substances for clinical use or as food additives. Copyright © 2015 Elsevier Ltd. All rights reserved.

  19. Biological Evaluation and Molecular Docking of Protocatechuic Acid from Hibiscus sabdariffa L. as a Potent Urease Inhibitor by an ESI-MS Based Method

    Directory of Open Access Journals (Sweden)

    Sherif T. S. Hassan

    2017-10-01

    Full Text Available Studies on enzyme inhibition remain a crucial area in drug discovery since these studies have led to the discoveries of new lead compounds useful in the treatment of several diseases. In this study, protocatechuic acid (PCA, an active compound from Hibiscus sabdariffa L. has been evaluated for its inhibitory properties against jack bean urease (JBU as well as its possible toxic effect on human gastric epithelial cells (GES-1. Anti-urease activity was evaluated by an Electrospray Ionization-Mass Spectrometry (ESI-MS based method, while cytotoxicity was assayed by the MTT method. PCA exerted notable anti-JBU activity compared with that of acetohydroxamic acid (AHA, with IC50 values of 1.7 and 3.2 µM, respectively. PCA did not show any significant cytotoxic effect on (GES-1 cells at concentrations ranging from 1.12 to 3.12 µM. Molecular docking study revealed high spontaneous binding ability of PCA to the active site of urease. Additionally, the anti-urease activity was found to be related to the presence of hydroxyl moieties of PCA. This study presents PCA as a natural urease inhibitor, which could be used safely in the treatment of diseases caused by urease-producing bacteria.

  20. Biological Evaluation and Molecular Docking of Protocatechuic Acid from Hibiscus sabdariffa L. as a Potent Urease Inhibitor by an ESI-MS Based Method.

    Science.gov (United States)

    Hassan, Sherif T S; Švajdlenka, Emil

    2017-10-11

    Studies on enzyme inhibition remain a crucial area in drug discovery since these studies have led to the discoveries of new lead compounds useful in the treatment of several diseases. In this study, protocatechuic acid (PCA), an active compound from Hibiscus sabdariffa L. has been evaluated for its inhibitory properties against jack bean urease (JBU) as well as its possible toxic effect on human gastric epithelial cells (GES-1). Anti-urease activity was evaluated by an Electrospray Ionization-Mass Spectrometry (ESI-MS) based method, while cytotoxicity was assayed by the MTT method. PCA exerted notable anti-JBU activity compared with that of acetohydroxamic acid (AHA), with IC 50 values of 1.7 and 3.2 µM, respectively. PCA did not show any significant cytotoxic effect on (GES-1) cells at concentrations ranging from 1.12 to 3.12 µM. Molecular docking study revealed high spontaneous binding ability of PCA to the active site of urease. Additionally, the anti-urease activity was found to be related to the presence of hydroxyl moieties of PCA. This study presents PCA as a natural urease inhibitor, which could be used safely in the treatment of diseases caused by urease-producing bacteria.

  1. ESI-MS studies of the reactions of novel platinum(II) complexes containing O,O'-chelated acetylacetonate and sulfur ligands with selected model proteins.

    Science.gov (United States)

    Marzo, Tiziano; De Pascali, Sandra A; Gabbiani, Chiara; Fanizzi, Francesco P; Messori, Luigi; Pratesi, Alessandro

    2017-08-01

    A group of mixed-ligand Pt(II) complexes bearing acetylacetonate and sulphur ligands were recently developed in the University of Lecce as a new class of prospective anticancer agents that manifested promising pharma-cological properties in preliminary in vitro and in vivo tests. Though modelled on the basis of cisplatin, these Pt(II) complexes turned out to exhibit a profoundly distinct mode of action as they were found to act mainly on non-genomic targets rather than on DNA. Accordingly, we have explored here their reactions with two representative model proteins through an established ESI-MS procedure with the aim to describe their general interaction mechanism with protein targets. A pronounced reactivity with the tested proteins was indeed documented; the nature of the resulting metallodrug-protein interactions could be characterised in depth in the various cases. Preferential binding to protein targets compared to DNA is supported by independent ICP-OES measurements. The implications of these findings are discussed.

  2. Label-free measurement of the yeast short chain TAG lipase activity by ESI-MS after one-step esterification.

    Science.gov (United States)

    Ham, Hye Jin; Seo, Jongcheol; Yoon, Hye-Joo; Shin, Seung Koo

    2017-03-01

    Triacylglycerol (TAG) lipases hydrolyze ester bonds in TAG and release diacylglycerol (DAG), monoacylglycerol (MAG), and FA. We present a one-step chemical derivatization method for label-free quantification of a mixture of TAG, DAG, and MAG following lipase assay by ESI-MS. Because the ionization efficiencies of TAG, DAG, and MAG are not identical, lipase reaction products, DAG and MAG, are derivatized to TAG species by esterifying their hydroxyl groups using acyl chloride, whose acyl chain contains one less (or one more) -CH 2 group than that of substrate TAG. This resulted in three TAG species that were separated by 14 Da from one another and exhibited similar ion responses representing their molar amounts in the mass spectra. A good linear correlation was observed between peak intensity ratios and molar ratios in calibration curve. This method enables simultaneous quantification of TAG, DAG, and MAG in lipase assay and, in turn, allows stoichiometric determination of the concentrations of FAs released from TAG and DAG separately. By applying this strategy to measure both TAG and DAG lipolytic activities of the yeast Tgl2 lipase, we demonstrated its usefulness in studying enzymatic catalysis, as lipase enzymes often show dissimilar activities toward these lipids. Copyright © 2017 by the American Society for Biochemistry and Molecular Biology, Inc.

  3. HPLC-ESI-MS(n) Analysis, Fed-Batch Cultivation Enhances Bioactive Compound Biosynthesis and Immune-Regulative Effect of Adventitious Roots in Pseudostellaria heterophylla.

    Science.gov (United States)

    Wang, Juan; Li, Jing; Li, Hongfa; Wu, Xiaolei; Gao, Wenyuan

    2015-09-01

    A electrospray ionization tandem mass spectrometry (ESI-MS(n)) analysis was performed in order to identify the active composition in Pseudostellaria heterophylla adventitious roots. Pseudostellarin A, C, D, and G were identified from P. heterophylla adventitious roots on the basis of LC-MS(n) analysis. The culture conditions of adventitious roots were optimized, and datasets were subjected to a partial least squares discriminant analysis (PLS-DA), in which the growth ratio and some compounds showed a positive correlation with an aeration volume of 0.3 vvm and inoculum density of 0.15 %. Fed-batch cultivation enhanced the contents of total saponin, polysaccharides, and specific oxygen uptaker rate (SOUR). The maximum dry root weight (4.728 g l(-1)) was achieved in the 3/4 Murashige and Skoog (MS) medium group. PLS-DA showed that polysaccharides contributed significantly to the clustering of different groups and showed a positive correlation in the MS medium group. The delayed-type hypersensitivity (DTH) reaction on the mice induced by 2,4-dinitrofluorobenzene (DNFB) was applied to compare the immunocompetence effects of adventitious roots (AR) with field native roots (NR) of P. heterophylla. As a result, AR possessed a similar immunoregulation function as NR.

  4. Determination of low levels of perchlorate in lettuce and spinach using ion chromatography-electrospray ionization mass spectrometry (IC-ESI-MS).

    Science.gov (United States)

    Seyfferth, Angelia L; Parker, David R

    2006-03-22

    A sample preparation method was developed to quantify environmentally relevant (low micrograms per liter) concentrations of perchlorate (ClO4(-)) in leafy vegetables using IC-ESI-MS. Lettuce and spinach were macerated, centrifuged, and filtered, and the aqueous extracts were rendered water-clear using a one-step solid-phase extraction method. Total time for extraction and sample preparation was 6 h. Ion suppression was demonstrated and was likely due to unknown organics still present in the extract solution after cleanup. However, this interference was readily eliminated using a Cl(18)O4(-) internal standard at 1 microg/L in all standards and samples. Hydroponically grown perchlorate-free butterhead lettuce was spiked to either 10.3 or 37.7 microg/kg of fresh weight (FW), and recoveries were between 91 and 98% and between 93 and 101%, respectively. Five types of lettuce and spinach from a local grocery store were then analyzed; they contained from 0.6 to 6.4 microg/kg of FW. Spike recoveries using the store-bought samples ranged from 89 to 100%. The method detection limit for perchlorate in plant extracts is 40 ng/L, and the corresponding minimum reporting limit is 200 ng/L or 0.8 microg/kg of FW.

  5. α-Glucosidase inhibition and antioxidant activity of an oenological commercial tannin. Extraction, fractionation and analysis by HPLC/ESI-MS/MS and (1)H NMR.

    Science.gov (United States)

    Muccilli, Vera; Cardullo, Nunzio; Spatafora, Carmela; Cunsolo, Vincenzo; Tringali, Corrado

    2017-01-15

    Two batches of the oenological tannin Tan'Activ R, (toasted oak wood - Quercus robur), were extracted with ethanol. A fractionation on XAD-16 afforded four fractions for each extract. Extracts and fractions were evaluated for antioxidant activity (DPPH), polyphenol content (GAE) and yeast α-glucosidase inhibitory activity. Comparable results were obtained for both columns, fractions X1B and X2B showing the highest antioxidant activity. Fractions X1C and X2C notably inhibited α-glucosidase, with IC50=9.89 and 8.05μg/mL, respectively. Fractions were subjected to HPLC/ESI-MS/MS and (1)H NMR analysis. The main phenolic constituents of both X1B and X2B were a monogalloylglucose isomer (1), a HHDP-glucose isomer (2), castalin (3) gallic acid (4), vescalagin (5), and grandinin (or its isomer roburin E, 6). X1C and X2C showed a complex composition, including non-phenolic constituents. Fractionation of X2C gave a subfraction, with enhanced α-glucosidase inhibitory activity (IC50=6.15μg/mL), with castalagin (7) as the main constituent. Copyright © 2016 Elsevier Ltd. All rights reserved.

  6. Determination and Pharmacokinetic Study of Three Diterpenes in Rat Plasma by UHPLC-ESI-MS/MS after Oral Administration of Rosmarinus officinalis L. Extract

    Directory of Open Access Journals (Sweden)

    Liqian Wang

    2017-06-01

    Full Text Available Rosmarinus officinalis L. is commonly used as a spice and flavoring agent. Diterpenes are the main active compounds of R. officinalis. An Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry (UHPLC-ESI-MS/MS method was developed for the determination of carnosol, rosmanol, and carnosic acid isolated from R. officinalis in rat plasma, and applied to a pharmacokinetic study after oral administration of R. officinalis extract. Sample preparation involved a liquid-liquid extraction of the analytes with ethyl acetate. Butylparaben was employed as an internal standard (I.S.. Chromatographic separation was carried out on a C18 column (ACQUITY UPLC® HSS T3, 1.8 μm, 2.1 mm × 100 mm with a gradient system consisting of the mobile phase solution A (0.1% formic acid in water and solution B (acetonitrile at the flow rate of 0.3 mL/min. The quantification was obtained using multiple reaction monitoring (MRM mode with electrospray ionization (ESI. The UHPLC-MS/MS assay was validated for linearity, accuracy, precision, extraction recovery, matrix effect and stability. This study described a simple, sensitive and validated UHPLC-MS/MS method for the simultaneous determination of three diterpene compounds in rat plasma after oral administration of R. officinalis extract, and investigated on their pharmacokinetic studies as well.

  7. LC/DAD/ESI/MS method for the determination of imidacloprid, thiacloprid, and spinosad in olives and olive oil after field treatment.

    Science.gov (United States)

    Angioni, Alberto; Porcu, Luciano; Pirisi, Filippo

    2011-10-26

    The behavior in the field and the transfer from olives to olive oil during the technological process of imidacloprid, thiacloprid, and spinosad were studied. The extraction method used was effective in extracting the analytes of interest, and no interfering peaks were detected in the chromatogram. The residue levels found in olives after treatment were 0.14, 0.04, and 0.30 mg/kg for imidacloprid, thiacloprid, and spinosad, respectively, far below the maximum residue levels (MRLs) set for these insecticides in EU. At the preharvest interval (PHI), no residue was detected for imidacloprid and thiacloprid, while spinosad showed a residue level of 0.04 mg/kg. The study of the effect of the technological process on pesticide transfer in olive oil showed that these insecticides tend to remain in the olive cake. The LC/DAD/ESI/MS method showed good performance with adequate recoveries ranging from 80 to 119% and good method limits of quantitation (LOQs) and of determination (LODs). No matrix effect was detected.

  8. Determination of Irgarol-1051 and its related s-triazine species in coastal sediments and mussel tissues by HPLC-ESI-MS/MS.

    Science.gov (United States)

    Tsang, Vic Wing-Hang; Lei, Ngai-Yu; Lam, Michael Hon-Wah

    2009-10-01

    A mild, low-temperature analytical approach based on sonication assisted extraction coupled with HPLC electrospray ionization triple quadrupole tandem mass spectrometry has been developed for the simultaneous qualitative and quantitative determination of the four Irgarol-related s-triazine species, namely Irgarol-1051, M1, M2 and M3, in coastal sediments and Green-lipped mussel samples. Mild extraction conditions were necessary for the preservation of the thermally unstable M2. The Multiple Reaction Monitoring (MRM) mode of detection by ESI-MS/MS enabled reliable qualitative identification and sensitive quantitative determination of those s-triazines. This determination method was applied to evaluate the degree of Irgarol-1051 contamination in the sediments and biota of the coastal environment of Hong Kong--one of the busiest maritime ports in the world. All the four s-triazine species were observed in all of the samples. This is the first time that the newly identified M2 and M3 are detected in coastal sediments and biota tissues.

  9. Selective detection of carbohydrates and their peptide conjugates by ESI-MS using synthetic quaternary ammonium salt derivatives of phenylboronic acids.

    Science.gov (United States)

    Kijewska, Monika; Kuc, Adam; Kluczyk, Alicja; Waliczek, Mateusz; Man-Kupisinska, Aleksandra; Lukasiewicz, Jolanta; Stefanowicz, Piotr; Szewczuk, Zbigniew

    2014-06-01

    We present new tags based on the derivatives of phenylboronic acid and apply them for the selective detection of sugars and peptide-sugar conjugates in mass spectrometry. We investigated the binding of phenylboronic acid and its quaternary ammonium salt (QAS) derivatives to carbohydrates and peptide-derived Amadori products by HR-MS and MS/MS experiments. The formation of complexes between sugar or sugar-peptide conjugates and synthetic tags was confirmed on the basis of the unique isotopic distribution resulting from the presence of boron atom. Moreover, incorporation of a quaternary ammonium salt dramatically improved the efficiency of ionization in mass spectrometry. It was found that the formation of a complex with phenylboronic acid stabilizes the sugar moiety in glycated peptides, resulting in simplification of the fragmentation pattern of peptide-derived Amadori products. The obtained results suggest that derivatization of phenylboronic acid as QAS is a promising method for sensitive ESI-MS detection of carbohydrates and their conjugates formed by non-enzymatic glycation or glycosylation.

  10. Sesamin and sesamolin as unexpected contaminants in various cold-pressed plant oils: NP-HPLC/FLD/DAD and RP-UPLC-ESI/MS(n) study.

    Science.gov (United States)

    Górnaś, Paweł; Siger, Aleksander; Pugajeva, Iveta; Segliņa, Dalija

    2014-04-01

    Thirteen cold-pressed oils (Japanese quince seed, black caraway, flaxseed, rapeseed, hemp, peanut, sunflower, pumpkin, hazelnut, poppy, walnut, almond and sesame oil) manufactured by the same company over a 2-year period (2011-12) were assessed for lipophilic compounds. The presence of sesamin and sesamolin, two characteristic lignans of sesame oil, were detected in all tested plant oils. Both lignans were identified by NP-HPLC/FLD/DAD and confirmed by a RP-UPLC-ESI/MS(n) method. The lowest amount of sesamin and sesamolin was found for Japanese quince seed oil (0.10 and 0.27 mg/100 g), and the highest, excluding sesame oil, for almond oil (36.21 and 105.42 mg/100 g, respectively). The highly significant correlation between sesamolin and sesamin concentrations was found in all samples tested (r = 0.9999; p products manufactured by the same company can contribute to a lesser regard for the quality of the final product. Moreover, less attention paid to the quality of final product can be related to the health risks of consumers especially sensitive to allergens. Therefore, proper cleaning of processing equipment is needed to prevent cross-contact of cold-pressed oils.

  11. Discrimination of Isomers of Released N- and O-Glycans Using Diagnostic Product Ions in Negative Ion PGC-LC-ESI-MS/MS

    Science.gov (United States)

    Ashwood, Christopher; Lin, Chi-Hung; Thaysen-Andersen, Morten; Packer, Nicolle H.

    2018-03-01

    Profiling cellular protein glycosylation is challenging due to the presence of highly similar glycan structures that play diverse roles in cellular physiology. As the anomericity and the exact linkage type of a single glycosidic bond can influence glycan function, there is a demand for improved and automated methods to confirm detailed structural features and to discriminate between structurally similar isomers, overcoming a significant bottleneck in the analysis of data generated by glycomics experiments. We used porous graphitized carbon-LC-ESI-MS/MS to separate and detect released N- and O-glycan isomers from mammalian model glycoproteins using negative mode resonance activation CID-MS/MS. By interrogating similar fragment spectra from closely related glycan isomers that differ only in arm position and sialyl linkage, product fragment ions for discrimination between these features were discovered. Using the Skyline software, at least two diagnostic fragment ions of high specificity were validated for automated discrimination of sialylation and arm position in N-glycan structures, and sialylation in O-glycan structures, complementing existing structural diagnostic ions. These diagnostic ions were shown to be useful for isomer discrimination using both linear and 3D ion trap mass spectrometers when analyzing complex glycan mixtures from cell lysates. Skyline was found to serve as a useful tool for automated assessment of glycan isomer discrimination. This platform-independent workflow can potentially be extended to automate the characterization and quantitation of other challenging glycan isomers. [Figure not available: see fulltext.

  12. Studies into the phenolic patterns of different tissues of pineapple (Ananas comosus [L.] Merr.) infructescence by HPLC-DAD-ESI-MS (n) and GC-MS analysis.

    Science.gov (United States)

    Steingass, Christof B; Glock, Mona P; Schweiggert, Ralf M; Carle, Reinhold

    2015-08-01

    In a comprehensive study, more than 60 phenolic compounds were detected in methanolic extracts from different tissues of pineapple infructescence by high-performance liquid chromatography with diode array detection and electrospray ionisation multiple-stage mass spectrometry (HPLC-DAD-ESI-MS (n) ) as well as by gas chromatography-mass spectrometry (GC-MS). The analytical workflow combining both methods revealed numerous compounds assigned for the first time as pineapple constituents by their mass fragmentations. Pineapple crown tissue was characterised by depsides of p-coumaric and ferulic acid. In contrast, major phenolic compounds in pineapple pulp extracts were assigned to diverse S-p-coumaryl, S-coniferyl and S-sinapyl derivatives of glutathione, N-L-γ-glutamyl-L-cysteine and L-cysteine, which were also identified in the peel. The latter was additionally characterised by elevated concentrations of p-coumaric, ferulic and caffeic acid depsides and glycerides, respectively. Two peel-specific cyanidin hexosides were found. Elevated concentrations of isomeric N,N'-diferuloylspermidines may be a useful tool for the detection of fraudulent peel usage for pineapple juice production. Mass fragmentation pathways of characteristic pineapple constituents are proposed, and their putative biological functions are discussed.

  13. Use of Electro-spray Ionization Mass Spectrometry (ESI-MS) for the characterization of complexes 'ligand - metallic cations' in solution

    Energy Technology Data Exchange (ETDEWEB)

    Berthon, Laurence; Zorz, Nicole; Lagrave, Stephanie; Gannaz, Benoit; Hill, Clement [CEA-Marcoule DEN-DRCP-SCPS-LCSE, BP 17171, 30207 Bagnols sur Ceze cedex (France)

    2008-07-01

    In the framework of nuclear waste reprocessing, separation processes of minor actinides from fission products are developed by Cea. In order to understand the mechanisms involved in the extraction processes, the 'ligand/metallic cation' complexes, formed in the organic phases are characterized by electro-spray-mass-spectrometry (ESI-MS). This paper deals with the extraction of lanthanides (III) and americium (III) cations by an organic phase composed of a malonamide or / and a dialkyl phosphoric acid, diluted in an aliphatic diluent. For the dialkyl phosphoric acid, Ln(DEHP){sub 3}(HDEHP){sub 3} complexes are observed and in the presence of a large excess of Ln(NO{sub 3}){sub 3}, dinuclear species are also observed. For the malonamide extractant, it appears that the complexes formed in the organic phase are of the Nd(NO{sub 3}){sub 3}D{sub x} type, with 2 {<=} x {<=} 4: their distributions depend on the ratio [Ln]/[DMDOHEMA]. When the two extractants are present in the organic phase, mixed 'Ln-malonamide-dialkyl phosphoric acid' species are observed. The influence of several parameters, such as extractant concentration, solute concentration, aqueous acidity and the nature of the cations (lanthanides or americium) are studied. (authors)

  14. Investigation of natural phosphatidylcholine sources: separation and identification by liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS2) of molecular species.

    Science.gov (United States)

    Le Grandois, Julie; Marchioni, Eric; Zhao, Minjie; Giuffrida, Francesca; Ennahar, Saïd; Bindler, Françoise

    2009-07-22

    This study is a contribution to the exploration of natural phospholipid (PL) sources rich in long-chain polyunsaturated fatty acids (LC-PUFAs) with nutritional interest. Phosphatidylcholines (PCs) were purified from total lipid extracts of different food matrices, and their molecular species were separated and identified by liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS(2)). Fragmentation of lithiated adducts allowed for the identification of fatty acids linked to the glycerol backbone. Soy PC was particularly rich in species containing essential fatty acids, such as (18:2-18:2)PC (34.0%), (16:0-18:2)PC (20.8%), and (18:1-18:2)PC (16.3%). PC from animal sources (ox liver and egg yolk) contained major molecular species, such as (16:0-18:2)PC, (16:0-18:1)PC, (18:0-18:2)PC, or (18:0-18:1)PC. Finally, marine source (krill oil), which was particularly rich in (16:0-20:5)PC and (16:0-22:6)PC, appeared to be an interesting potential source for food supplementation with LC-PUFA-PLs, particularly eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA).

  15. Simultaneous Determination of Seven Phenolic Acids in Rat Plasma Using UHPLC-ESI-MS/MS after Oral Administration of Echinacea purpurea Extract

    Directory of Open Access Journals (Sweden)

    Yan Du

    2017-09-01

    Full Text Available A rapid and sensitive Ultra High Performance Liquid Chromatography Electrospray Ionization Tandem Mass Spectrometry (UHPLC-ESI-MS/MS method was developed and validated to simultaneously determine the concentration of seven phenolic acids (syringic acid, ferulic acid, caffeic acid, vanillic acid, p-coumaric acid, 3,4-dihydroxybenzoic acid and 4-hydroxybenzoic acid in rat plasma after oral administration of Echinacea purpurea extract. After mixing with the internal standard (IS, butylparaben, plasma samples were prepared by liquid–liquid extraction with ethyl acetate. The separation was performed using the Agilent Eclipse Plus C18 column (1.8 μm, 2.1 mm × 50 mm with a gradient system consisting of solution A (0.1% acetic acid in water and solution B (methanol at a flow rate of 0.3 mL/min. The detection was accomplished by a multiple reaction monitoring (MRM mode with electrospray ionization (ESI. The method was validated in terms of linearity, precision, accuracy, extraction recovery, matrix effect and stability. This method was successfully applied to study the pharmacokinetic properties of the seven compounds after oral administration of Echinacea purpurea extract in rats.

  16. Identification and quantification of phenolic compounds of selected fruits from Madeira Island by HPLC-DAD-ESI-MS(n) and screening for their antioxidant activity.

    Science.gov (United States)

    Spínola, Vítor; Pinto, Joana; Castilho, Paula C

    2015-04-15

    Five fruits species commonly cultivated and consumed in Madeira Island (Portugal) were investigated for their phenolic profile by means of reversed phase high-performance liquid chromatography coupled to diode array detection and electrospray ionisation mass spectrometry (HPLC-DAD-ESI/MS(n)) and antioxidant potential. A large number of compounds were characterised, flavonoids and phenolic acids being the major components found in target samples, 39 compounds (flavonoids, phenolic acids, terpenoids, cyanogenic glycosides and organic acids) were identified in cherimoyas, lemons, papayas, passion-fruits and strawberries for the first time. Furthermore, all samples were systematically analysed for their total phenolic and flavonoid contents along with two radical scavenging methods (ABTS and ORAC) for antioxidant activity measurement. Target fruits presented high phenolic contents which is responsible for most of the antioxidant activity against radical reactive species (R(2)>0.80). Quantitative data showed that anthocyanins, in particular pelargonidin-3-O-hexoside (>300 mg/100 mL), present only in strawberries were the compounds in largest amounts but are the ones which contribute less to the antioxidant activity. Copyright © 2014 Elsevier Ltd. All rights reserved.

  17. Identification of new derivatives of 2-S-glutathionylcaftaric acid in aged white wines by HPLC-DAD-ESI-MS(n).

    Science.gov (United States)

    Cejudo-Bastante, María Jesús; Pérez-Coello, María Soledad; Hermosín-Gutiérrez, Isidro

    2010-11-10

    Glutathione, a natural occurring antioxidant, is a thiol-containing peptide present in grape must and wine. It is able to regenerate the o-diphenol group of enzymatically oxidized trans-caftaric acid, giving rise to 2-S-glutathionyl-trans-caftaric acid (also known as grape reaction product, GRP) and thus inhibiting the browning of wine. The amount of GRP present in a wine provides information on the oxidation history of the wine over its elaboration and aging. GRP has been proved to suffer hydrolysis in model solutions and wines. To know the actual content of glutathione involved in white wine browning inhibition as GRP, the GRP-derived products have been studied in 1-year-aged white wines by HPLC-DAD-ESI-MS(n). Online UV-vis spectra and pseudomolecular ions [(M + H)(+)] obtained by LC-MS supported the formation of some of the expected GRP hydrolysis products, mainly 2-S-glutathionyl-trans-caffeic acid (trans-GSCf), together with minor 2-S-(cysteinylglycyl)-trans-caftaric acid, 2-S-(γ-glutamylcysteinyl)-trans-caftaric acid, and 2-S-cysteinyl-trans-caftaric acid. On the basis of UV-vis and LC-MS(2) spectra, new GRP derivatives in aged white wines have been tentatively characterized for the first time as three monoethyl esters of GRP (GRP-Et) and also the cis isomers of GRP, GSCf, and some of the GRP-Et.

  18. Preliminary UHPLC–PDA–ESI-MS screening of light-accelerated autoxidation products of the tetrapyrrole biliverdin

    NARCIS (Netherlands)

    Weesepoel, Y.J.A.; Gruppen, H.; Vincken, J.P.

    2015-01-01

    The application of phycobiliproteins, e.g. blue C-phycocyanin, as natural water-soluble food colourants is emerging. The chromophore of these proteins comprises a number of tetrapyrroles (or phycocyanobilins), which have an extensive conjugated system, vulnerable to autoxidation. To assess the

  19. Development and validation of a method for the analysis of Ochratoxin A in roasted coffee by liquid chromatography/electrospray-mass spectrometry in Tandem (LC/ESI-MS/MS

    Directory of Open Access Journals (Sweden)

    Raquel D. C. C. Bandeira

    2012-01-01

    Full Text Available A method using LC/ESI-MS/MS for the quantitative analysis of Ochratoxin A in roasted coffee was described. Linearity was demonstrated (r = 0.9175. The limits of detection and quantification were 1.0 and 3.0 ng g-1, respectively. Trueness, repeatability and intermediate precision values were 89.0-108.8%; 2.4-13.7%; 12.5-17.8%, respectively. To the best of our knowledge, this is the first report in which Ochratoxin A in roasted coffee is analysed by LC/ESI-MS/MS, contributing to the field of mycotoxin analysis, and it will be used for future production of Certified Reference Material.

  20. Thin-film microextraction coupled to LC-ESI-MS/MS for determination of quaternary ammonium compounds in water samples.

    Science.gov (United States)

    Boyacı, Ezel; Sparham, Chris; Pawliszyn, Janusz

    2014-01-01

    The dual nature of the quaternary ammonium compounds, having permanently charged hydrophilic quaternary ammonium heads and long-chain hydrophobic tails, makes the sample preparation step and analysis of these compounds challenging. A high-throughput method based on thin-film solid-phase microextraction (SPME) and liquid chromatography mass spectrometry was developed for simultaneous quantitative analysis of nine benzylic and aliphatic quaternary ammonium compounds. Chromatographic separation and detection of analytes were obtained in reverse-phase mode in 8 min using a triple quadrupole mass spectrometer. Hydrophilic lipophilic balance particle-coated blades were found to be the most suitable among the different coatings tested in terms of recoveries and carryover on the blades. For desorption solvents, 70/30, v/v (A/B) with 0.1 % formic acid (where A is 10 mM ammonium acetate in acetonitrile/water (95/5 , v/v) and B is 0.1 %  (v/v) formic acid in isopropyl alcohol) was shown to be the most efficient solvent for the desorption of the analytes from the SPME sorbent. The SPME method was optimised in terms of extraction, pH, and preconditioning, as well as extraction and desorption times. Optimum conditions were 45 min of extraction time and 15 min of desorption time, all with agitation. The extraction was found to be optimum in a range of pH 6.0 to 8.0, which is consistent with the natural pH of water samples. Wide linear dynamic ranges with the developed method were obtained for each compound, enabling the application of the method for a wide range of concentrations. The developed method was validated according to the Food and Drug Administration criteria. The proposed method is the first SPME-based approach describing the applicability of the high-throughput thin-film SPME in a 96-well system for analysis of such challenging compounds.

  1. Pharmacokinetics of taurolidine following repeated intravenous infusions measured by HPLC-ESI-MS/MS of the derivatives taurultame and taurinamide in glioblastoma patients.

    Science.gov (United States)

    Stendel, Ruediger; Scheurer, Louis; Schlatterer, Kathrin; Stalder, Urs; Pfirrmann, Rolf W; Fiss, Ingo; Möhler, Hanns; Bigler, Laurent

    2007-01-01

    Taurolidine is known to have antimicrobial activity. Furthermore, at lower concentrations, it has been found to exert a selective antineoplastic effect in vitro and in vivo. The aim of this study was to investigate the pharmacokinetics of taurolidine in vivo following repeated intravenous infusion in a schedule used for the treatment of glioblastoma. As a prerequisite, the pharmacokinetics of taurolidine in human blood plasma and whole blood in vitro was investigated. The pharmacokinetics of taurolidine and its derivatives taurultame and taurinamide were investigated in human blood plasma and in whole blood in vitro using blood from a healthy male volunteer. During repeated intravenous infusion therapy with taurolidine, plasma samples were taken every hour for a period of 13 hours per day in seven patients (three male, four female; mean age 48.4 +/- 12.8 years, range 27-66 years) with a glioblastoma. Following dansyl derivatisation, the concentrations of taurultame and taurinamide were determined using a new method based on high-performance liquid chromatography (HPLC) online coupled to electrospray ionisation tandem mass spectrometry (ESI-MS/MS) in the multiple reaction monitoring mode. Under the experimental conditions used, taurolidine could not be determined directly and was back-calculated from the taurultame and taurinamide values. The new HPLC-ESI-MS/MS method demonstrated high accuracy and reproducibility. In vitro plasma concentrations of taurultame and taurinamide remained constant over the incubation period. In whole blood in vitro, a time-dependent formation of taurinamide was observed. At the start of the incubation, the taurultame-taurinamide ratio (TTR) was 0.95 at an initial taurolidine concentration of 50 microg/mL, and 1.69 at 100 microg/mL. The concentration of taurultame decreased at the same rate as the taurinamide concentration increased, showing logarithmic kinetics. The calculated taurolidine concentration remained largely constant over the

  2. Rapid, simple and highly sensitive LC-ESI-MS/MS method for the quantification of tamsulosin in human plasma.

    Science.gov (United States)

    Ramakrishna, N V S; Vishwottam, K N; Manoj, S; Koteshwara, M; Wishu, S; Varma, D P

    2005-12-01

    A simple, rapid, sensitive and specific liquid chromatography-tandem mass spectrometry method was developed and validated for quantification of tamsulosin (I), a highly selective alpha1-adrenoceptor antagonist used for the treatment of patients with symptomatic benign prostatic hyperplasia. The analyte and internal standard, mosapride (II) were extracted by liquid-liquid extraction with diethyl ether-dichloromethane (70:30, v/v) using a Glas-Col Multi-Pulse Vortexer. The chromatographic separation was performed on a reverse phase Waters symmetry C18 column with a mobile phase of 0.03% formic acid-acetonitrile (30:70, v/v). The protonated analyte was quantitated in positive ionization by multiple reaction monitoring with a mass spectrometer. The mass transitions m/z 409.1 solidus in circle 228.1 and m/z 422.3 solidus in circle 198.3 were used to measure I and II, respectively. The assay exhibited a linear dynamic range of 0.1-50.0 ng/mL for tamsulosin in human plasma. The lower limit of quantitation was 100 pg/mL with a relative standard deviation of less than 10%. Acceptable precision and accuracy were obtained for concentrations over the standard curve ranges. A run time of 2.0 min for each sample made it possible to analyze a throughput of more than 400 human plasma samples per day. The validated method has been successfully used to analyze human plasma samples for application in pharmacokinetic, bioavailability or bioequivalence studies. (c) 2005 John Wiley & Sons, Ltd.

  3. Comparison of total phenolic content, scavenging activity and HPLC-ESI-MS/MS profiles of both young and mature leaves and stems of Andrographis paniculata.

    Science.gov (United States)

    Chua, Lee Suan; Yap, Ken Choy; Jaganath, Indu Bala

    2013-12-01

    The total phenolic content and radical scavenging activity of Andrographis paniculata has been investigated to estimate the amount of phenolic compounds and diterpene lactones, respectively in the plant extracts. The stem extracts exhibited higher total phenolic content and scavenging activity than those of the leaf extracts from both young and mature plants. A range of 19.6-47.8 mg extract of A. paniculata from different parts of the plant is equivalent to the scavenging activity exhibited by one mg of standard Trolox. HPLC-ESI-MS/MS was also used to identify simultaneously the phytochemicals from the leaves and stems of both young and mature plant samples. Of the identified compounds, seven of the sixteen diterpene lactones, three of the six flavonoids, five of the six phenolic acids and two cyclic acids are reported here for the first time for this species. Multivariate statistical approaches such as Hierarchiral Component Analysis (HCA) and Principle Component Analysis (PCA) have clustered the plant extracts into the leaf and stem groups, regardless of plant age. Further classification based on the phytochemical profiles revealed that mostly phenolic acids and flavonoids were from the young leaf extracts, and diterpenoids and their glycosides from the mature leaf extracts. However, the phytochemical profiles for the stems of both young and mature plants were not significantly different as presented in the dendrogram of HCA and the score plot of PCA. The marker for mature plants might be the m/z 557 ion (dihydroxyl dimethyl 19-[(beta-D-glucopyranosyl)oxy]-19-oxo-ent-labda-8(17),13-dien-16,15-olide), whereas the m/z 521 ion (propyl neoandrographolide) could be the marker for leaf extracts.

  4. RP-UHPLC-UV-ESI-MS/MS analysis of LPMO generated C4-oxidized gluco-oligosaccharides after non-reductive labeling with 2-aminobenzamide.

    Science.gov (United States)

    Frommhagen, Matthias; van Erven, Gijs; Sanders, Mark; van Berkel, Willem J H; Kabel, Mirjam A; Gruppen, Harry

    2017-08-07

    Lytic polysaccharide monooxygenases (LPMOs) are able to cleave recalcitrant polysaccharides, such as cellulose, by oxidizing the C1 and/or C4 atoms. The analysis of the resulting products requires a variety of analytical techniques. Up to now, these techniques mainly focused on the identification of non-oxidized and C1-oxidized oligosaccharides. The analysis of C4-oxidized gluco-oligosaccharides is mostly performed by using high pressure anion exchange chromatography (HPAEC). However, the alkaline conditions used during HPAEC analysis lead to tautomerization of C4-oxidized gluco-oligosaccharides, which limits the use of this technique. Here, we describe the use of reverse phase-ultra high performance liquid chromatography (RP-UHPLC) in combination with non-reductive 2-aminobenzamide (2-AB) labeling. Non-reductive 2-AB labeling enabled separation of C4-oxidized gluco-oligosaccharides from their non-oxidized counterparts. Moreover, RP-UHPLC does not require buffered mobile phases, which reduce mass spectrometry (MS) sensitivity. The latter is seen as an advantage over other techniques such as hydrophilic interaction liquid chromatography and porous graphitized carbon coupled to MS. RP-UHPLC coupled to UV detection and mass spectrometry allowed the identification of both labeled non-oxidized and C4-oxidized oligosaccharides. Non-reductive labeling kept the ketone at the C4-position of LPMO oxidized oligosaccharides intact, while selective reducing agents such as sodium triacetoxyborohydride (STAB) reduced this ketone group. Our results show that RP-UHPLC-UV-ESI-MS in combination with non-reductively 2-AB labeling is a suitable technique for the separation and identification of LPMO-generated C4-oxidized gluco-oligosaccharides. Copyright © 2017 The Authors. Published by Elsevier Ltd.. All rights reserved.

  5. Dissociation Behavior of a TEMPO-Active Ester Cross-Linker for Peptide Structure Analysis by Free Radical Initiated Peptide Sequencing (FRIPS) in Negative ESI-MS.

    Science.gov (United States)

    Hage, Christoph; Ihling, Christian H; Götze, Michael; Schäfer, Mathias; Sinz, Andrea

    2017-01-01

    We have synthesized a homobifunctional amine-reactive cross-linking reagent, containing a TEMPO (2,2,6,6-tetramethylpiperidine-1-oxy) and a benzyl group (Bz), termed TEMPO-Bz-linker, to derive three-dimensional structural information of proteins. The aim for designing this novel cross-linker was to facilitate the mass spectrometric analysis of cross-linked products by free radical initiated peptide sequencing (FRIPS). In an initial study, we had investigated the fragmentation behavior of TEMPO-Bz-derivatized peptides upon collision activation in (+)-electrospray ionization collision-induced dissociation tandem mass spectrometry (ESI-CID-MS/MS) experiments. In addition to the homolytic NO-C bond cleavage FRIPS pathway delivering the desired odd-electron product ions, an alternative heterolytic NO-C bond cleavage, resulting in even-electron product ions mechanism was found to be relevant. The latter fragmentation route clearly depends on the protonation of the TEMPO-Bz-moiety itself, which motivated us to conduct (-)-ESI-MS, CID-MS/MS, and MS 3 experiments of TEMPO-Bz-cross-linked peptides to further clarify the fragmentation behavior of TEMPO-Bz-peptide molecular ions. We show that the TEMPO-Bz-linker is highly beneficial for conducting FRIPS in negative ionization mode as the desired homolytic cleavage of the NO-C bond is the major fragmentation pathway. Based on characteristic fragments, the isomeric amino acids leucine and isoleucine could be discriminated. Interestingly, we observed pronounced amino acid side chain losses in cross-linked peptides if the cross-linked peptides contain a high number of acidic amino acids. Graphical Abstract ᅟ.

  6. Determination of reduced homocysteine in human serum by elemental labelling and liquid chromatography with ICP-MS and ESI-MS detection.

    Science.gov (United States)

    Espina, Juan Gómez; Montes-Bayón, Maria; Blanco-González, Elisa; Sanz-Medel, Alfredo

    2015-10-01

    Analytical methods allowing sensitive determination of reduced homocysteine (rHcy), one of the so-called biothiols, in human serum is a topic of growing interest due to its close relation to several human disorders, mainly cardiovascular diseases. Although most widely used analytical strategies to determine total Hcy involve derivatization by means of fluorescent labels, this work proposes the use of ebselen, a Se-containing labelling agent to derivatize the reactive sulfhydryl group of the Hcy molecule in its "free" reduced form, which is more likely to play different roles in disease pathogenesis. Optimization of the derivatization and separation conditions by high-performance liquid chromatography (HPLC) to isolate the excess of derivatizing reagent is carried out here using UV/VIS detection. Further, the study of the Se labelling reaction by electrospray ionization tandem mass spectrometry (ESI-MS/MS) provides a stoichiometry of the derivative of 1:1. The main advantage of using ebselen as a labelling agent is the presence of the Se atom in the molecule that allows the use of inductively coupled plasma mass spectrometry (ICP-MS) as a sensitive and selective Se detector. The coupling of HPLC with ICP-MS provided excellent features for the determination of Se-derivatized rHcy (detection limit of 9.6 nM) in real samples. Quantification was accomplished by using post-column isotope dilution (ID) of Se in serum samples, after precipitation of the main serum proteins. Quantitative results for "free" rHcy turned out to be around 0.18-0.22 μM in serum samples from healthy individuals that could be directly analyzed without sample preconcentration.

  7. New and vintage solutions to enhance the plasma metabolome coverage by LC-ESI-MS untargeted metabolomics: the not-so-simple process of method performance evaluation.

    Science.gov (United States)

    Tulipani, Sara; Mora-Cubillos, Ximena; Jáuregui, Olga; Llorach, Rafael; García-Fuentes, Eduardo; Tinahones, Francisco J; Andres-Lacueva, Cristina

    2015-03-03

    Although LC-MS untargeted metabolomics continues to expand into exiting research domains, methodological issues have not been solved yet by the definition of unbiased, standardized and globally accepted analytical protocols. In the present study, the response of the plasma metabolome coverage to specific methodological choices of the sample preparation (two SPE technologies, three sample-to-solvent dilution ratios) and the LC-ESI-MS data acquisition steps of the metabolomics workflow (four RP columns, four elution solvent combinations, two solvent quality grades, postcolumn modification of the mobile phase) was investigated in a pragmatic and decision tree-like performance evaluation strategy. Quality control samples, reference plasma and human plasma from a real nutrimetabolomic study were used for intermethod comparisons. Uni- and multivariate data analysis approaches were independently applied. The highest method performance was obtained by combining the plasma hybrid extraction with the highest solvent proportion during sample preparation, the use of a RP column compatible with 100% aqueous polar phase (Atlantis T3), and the ESI enhancement by using UHPLC-MS purity grade methanol as both organic phase and postcolumn modifier. Results led to the following considerations: submit plasma samples to hybrid extraction for removal of interfering components to minimize the major sample-dependent matrix effects; avoid solvent evaporation following sample extraction if loss in detection and peak shape distortion of early eluting metabolites are not noticed; opt for a RP column for superior retention of highly polar species when analysis fractionation is not feasible; use ultrahigh quality grade solvents and "vintage" analytical tricks such as postcolumn organic enrichment of the mobile phase to enhance ESI efficiency. The final proposed protocol offers an example of how novel and old-fashioned analytical solutions may fruitfully cohabit in untargeted metabolomics

  8. Determination of prodrug treosulfan and its biologically active monoepoxide in rat plasma, liver, lungs, kidneys, muscle, and brain by HPLC-ESI-MS/MS method.

    Science.gov (United States)

    Romański, Michał; Kasprzyk, Anna; Teżyk, Artur; Widerowska, Agnieszka; Żaba, Czesław; Główka, Franciszek

    2017-06-05

    A prodrug treosulfan (TREO) is currently investigated in clinical trials for conditioning prior to hematopoietic stem cell transplantation. Bioanalysis of TREO and its active derivatives, monoepoxide (S,S-EBDM) and diepoxide, in plasma and urine underlay the pharmacokinetic studies of these compounds but cannot explain an organ pharmacological action or toxicity. Recently, distribution of TREO and S,S-EBDM into brain, cerebrospinal fluid, and aqueous humor of the eye has been investigated in animal models and the obtained results presented clinical relevance. In this paper, a selective and rapid HPLC-ESI-MS/MS method was elaborated and validated for the studies of disposition of TREO and S,S-EBDM in rat plasma, liver, lungs, kidneys, muscle, and brain. The two analytes and codeine, internal standard (IS), were isolated from 50μL of plasma and 100μL of supernatants of the tissues homogenates using ultrafiltration Amicon vials. Chromatographic resolution was accomplished on C18 column with isocratic elution. The limits of quantitation of TREO and S,S-EBDM in the studied matrices ranged from 0.11 to 0.93μM. The HPLC-MS/MS method was adequately precise and accurate within and between runs. The IS-normalized matrix effect differed among the tissues and was the most pronounced in a liver homogenate supernatant (approximately 0.55 for TREO and 0.35 for S,S-EBDM). Stability of the analytes in experimental samples was also established. The validated method for the first time enabled determination of TREO and S,S-EBDM in the six life-important tissues in rats following administration of the prodrug. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Antioxidant capacity, polyphenolic content and tandem HPLC-DAD-ESI/MS profiling of phenolic compounds from the South American berries Luma apiculata and L. chequén.

    Science.gov (United States)

    Simirgiotis, Mario J; Bórquez, Jorge; Schmeda-Hirschmann, Guillermo

    2013-08-15

    Native Myrtaceae fruits were gathered by South American Amerindians as a food source. At present, there is still some regional consume of the small berries from trees belonging to genus Luma that occurs in southern Chile and Argentina. The aerial parts and berries from Luma apiculata and Luma chequen were investigated for phenolic constituents and antioxidant capacity. A high performance electrospray ionisation mass spectrometry method was developed for the rapid identification of phenolics in polar extracts from both species. Thirty-one phenolic compounds were detected and 27 were identified or tentatively characterised based on photodiode array UV-vis spectra (DAD), ESI-MS-MS spectrometric data and spiking experiments with authentic standards. Twelve phenolic compounds were detected in L. apiculata fruits and 12 in the aerial parts while L. chequen yielded 10 compounds in fruits and 16 in aerial parts, respectively. From the compounds occurring in both Luma species, seven were identified as tannins or their monomers, 15 were flavonol derivatives and five were anthocyanins. The whole berry and aerial parts extracts presented high antioxidant capacity in the DPPH assay (IC50 of 10.41±0.02 and 2.44±0.03 μg/mL for L. apiculata, 12.89±0.05 and 3.22±0.05 for L. chequen, respectively), which can be related to the diverse range of phenolics detected. The antioxidant capacity together with the high polyphenolic contents and compounds identified can support at least in part, their use as botanical drugs. From the compounds identified in both species, 3-O-(6″-O-galloyl)-hexose derivatives of myricetin, quercetin, laricitrin and isorhamnetin are reported for the first time for the genus Luma. Copyright © 2013 Elsevier Ltd. All rights reserved.

  10. Identification and Determination of Flavonoids in Astragali Radix by High Performance Liquid Chromatography Coupled with DAD and ESI-MS Detection

    Directory of Open Access Journals (Sweden)

    Yu-Ling Wang

    2011-03-01

    Full Text Available A method for the analysis of flavonoids in Astragali Radix by high-performance liquid chromatography (HPLC combined with photodiode-array detection (DAD and an electrospray ionization (ESI - mass spectrometry (MS was developed. After the samples were extracted with ethanol, the optimum separation conditions for these analytes were achieved using a gradient elution system and a 2.0 × 150 mm Shimadzu VP-ODS column. Eight flavonoids were identified to exist in Astragali Radix based on their characteristic UV data and mass spectra. The concentrations of three major components in this herb—ononin, calycosin and formononetin—were determined by LC/ESI-MS in positive selective ion monitoring (SIM mode. The calibration curves were linear in the range of 0.9~180.0 μg·mL−1 for ononin, 1.8~360.0 μg·mL−1 for calycosin and 1.4~280 μg·mL−1 for formononetin, respectively. The limits of quantification (LOQ and detection (LOD were 0.9 μg· mL−1 and 0.2 μg mL−1 for ononin, 1.8 μg mL−1 and 0.5 μg·mL−1 for calycosin, 1.4 μg mL−1 and 0.5 μg·mL−1 for formononetin, respectively. The standard recoveries were between 95.4~104.7%. The developed method was proven to be useful for the quantitative and qualitative analysis of flavonoid constituents in various resources of Astragali Radix.

  11. Pharmacokinetic study of harmane and its 10 metabolites in rat after intravenous and oral administration by UPLC-ESI-MS/MS.

    Science.gov (United States)

    Li, Shuping; Teng, Liang; Liu, Wei; Cheng, Xuemei; Jiang, Bo; Wang, Zhengtao; Wang, Chang-Hong

    2016-09-01

    Context The β-carboline alkaloid harmane is widely distributed in common foods, beverages and hallucinogenic plants. Harmane exerts potential in therapies for Alzheimer's and depression diseases. However, little information on its dynamic metabolic profiles and pharmacokinetics in vivo is currently available. Objective This study investigates the dynamic metabolic profiles and pharmacokinetic properties of harmane and its metabolites in rats in vivo. Materials and methods A highly selective, sensitive and rapid ultra-performance liquid chromatography combined with electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) method was developed and well-validated for simultaneous quantitative determination of harmane and its uncertain endogenous metabolite harmine, as well as for semiquantitative determination of 10 harmane metabolites in rats after intravenous injection and oral administration of harmane at 1.0 and 30.0 mg/kg, respectively. Results The calibration curves of harmane and harmine showed excellent linearity within the concentration range of 1-2000 ng/mL with acceptable accuracy, precision, selectivity, recovery, matrix effect and stability. Ten metabolites, including harmane but not harmine, were detected and identified after intravenous and oral administration of harmane. The absolute bioavailability of harmane following an oral dose was 19.41 ± 3.97%. According to the AUC0-t values of all the metabolites, the metabolic levels of phase II metabolites were higher than those of phase I metabolites, and the sulphation pathways were the dominant metabolic routes for harmane in both routes of administration. Discussion and conclusion The pharmacokinetic properties of harmane and its 10 metabolites in rats were determined. Sulphate conjugation was the predominant metabolic process of harmane in rats.

  12. Identification and determination of flavonoids in astragali radix by high performance liquid chromatography coupled with DAD and ESI-MS detection.

    Science.gov (United States)

    Lv, Yan-Wen; Hu, Wei; Wang, Yu-Ling; Huang, Lan-Fang; He, Yun-Biao; Xie, Xian-Zhen

    2011-03-09

    A method for the analysis of flavonoids in Astragali Radix by high-performance liquid chromatography (HPLC) combined with photodiode-array detection (DAD) and an electrospray ionization (ESI)--mass spectrometry (MS) was developed. After the samples were extracted with ethanol, the optimum separation conditions for these analytes were achieved using a gradient elution system and a 2.0 x 150 mm Shimadzu VP-ODS column. Eight flavonoids were identified to exist in Astragali Radix based on their characteristic UV data and mass spectra. The concentrations of three major components in this herb--ononin, calycosin and formononetin--were determined by LC/ESI-MS in positive selective ion monitoring (SIM) mode. The calibration curves were linear in the range of 0.9~180.0 μg·mL⁻¹ for ononin, 1.8~360.0 μg·mL⁻¹ for calycosin and 1.4~280 μg·mL⁻¹ for formononetin, respectively. The limits of quantification (LOQ) and detection (LOD) were 0.9 μg· mL⁻¹ and 0.2 μg mL⁻¹ for ononin, 1.8 μg mL⁻¹ and 0.5 μg·mL-1 for calycosin, 1.4 μg mL⁻¹ and 0.5 μg·mL⁻¹ for formononetin, respectively. The standard recoveries were between 95.4~104.7%. The developed method was proven to be useful for the quantitative and qualitative analysis of flavonoid constituents in various resources of Astragali Radix.

  13. Effects of Different Extraction Methods on the Extraction Rates of Five Chemical Ingredients of Swertia mussotii Franch by UPLC-ESI-MS/MS

    Science.gov (United States)

    Xiong, Yaokun; Zhou, Lifen; Zhao, Yonghong; Liu, Yun; Liu, Xia; Zhu, Genhua; Yan, Zhihong; Liu, Zhiyong

    2018-01-01

    Objective: To compare the effects of three extraction methods (ultrasound, reflux and percolation) on the contents of gentiopicroside, mangiferin, swertiamain, sweroside and oleanolic acid in Swertia mussotii Franch. Method: The contents of five components were determined by UPLC-ESI/MS. In the solvent system, eluent A was 0.05% (v: v) formic acid with 1mM/L ammonium acetate aqueous solution and eluent B was acetonitrile. Chromatographic separations were achieved using an Agilent EC-C18 column (4.6×100 mm, 2.7 um) at 30 °C. The flow rate was set at 0.8mL/min. The compound ionization was adopted at negative ionization mode by electro spray ionization (ESI). The quantification was performed in multiple reaction monitoring (MRM). Results: The linear ranges of swertiamarin, gentiopicroside, mangiferin, sweroside and oleanolic acid are 80∼7450 ng/mL, 103∼6600 ng/mL, 100∼8000 ng/mL, 130∼8450 ng/mL, 100∼7000 ng/mL, respectively. As a result, the content of oleanolic acid was the highest extracted by ultrasonic extraction and the content of mangiferin was the highest extracted by reflux extraction. For percolation extraction, the contents of five components were between ultrasound and reflux extraction. Conclusion: For five components, there are significant differences between the three different extraction methods. The results could provide a reference for the quality control of Swertia mussotii Franch and the research and development of new drugs.

  14. UHPLC-ESI-MS Analysis of Purified Flavonoids Fraction from Stem of Dendrobium denneaum Paxt. and Its Preliminary Study in Inducing Apoptosis of HepG2 Cells

    Directory of Open Access Journals (Sweden)

    Chunhua Zhou

    2018-01-01

    Full Text Available Dendrobium denneaum paxt., which has been widely used for health prevention in traditional Chinese medicine (TCM, is one of the most popular tonic herbs in China. In order to analyze its flavonoids, characterization and antitumor activity of crude extract and flavonoids rich fractions from D. denneaum paxt. were investigated. Flavonoids extracted from D. denneaum paxt. were clearly enriched in fraction II after determining the total flavonoids content; there were 15 characteristic peaks which have been detected; ultra-high performance liquid chromatography-electrospray ionization/mass spectrometry (UHPLC-ESI-MS/MS was applied for structural elucidation of compounds. 13 characteristic peaks including flavonoid-O-glycosides and flavonoid-C-glycosides were determined or preliminarily characterized through comparing retention times and UV and MS spectra with standard compounds or documented literature. The antitumor activity of fraction II on human liver cancer cells HepG2 was investigated. MTT assay method was used to test the antiproliferation activity and to confirm the appropriate treatment concentration as well as inducing time. The morphological changes of the apoptosis cells after being induced by fraction II were observed by a Hoechst reagent and the apoptosis rate was tested by flow cytometry. The results showed that fraction II can inhibit HepG2 cells from proliferation in a dose-dependent and time-dependent manner. The apoptosis experiments indicated that fraction II can significantly induce apoptosis in HepG2 cells in a concentration over 50 μg/mL for 48 h and the most effective level was 150 μg/mL for 48 h.

  15. Investigation of targeted pyrrolizidine alkaloids in traditional Chinese medicines and selected herbal teas sourced in Ireland using LC-ESI-MS/MS.

    Science.gov (United States)

    Griffin, Caroline T; Gosetto, Francesca; Danaher, Martin; Sabatini, Stefano; Furey, Ambrose

    2014-01-01

    Publications linking hepatotoxicity to the use of herbal preparations are escalating. Herbal teas, traditional Chinese medicines (TCMs) and dietary supplements have been shown to contain pyrrolizidine alkaloids (PAs). Acute PA toxicosis of the liver can result in sinusoidal-obstruction syndrome, also known as veno-occlusive disease (VOD). This paper describes a sensitive and robust method for the detection of targeted PAs and their N-oxides (PANOs) in herbal products (selected herbal teas and TCMs) sourced within Ireland. The sample preparation includes a simple acidic extraction with clean-up via solid-phase extraction (SPE). Sample extracts were accurately analysed by using LC-ESI-MS/MS applying for the first time a pentafluorophenyl (PFP) core-shell column to the chromatographic separation of PAs and PANOs. The method was validated for selectivity, taking into consideration matrix effects, specificity, linearity, precision and trueness. Limits of detection (LOD) and limits of quantitation (LOQ) were quantified for all PAs and PANOs ranging from 0.4 to 1.9 µg kg⁻¹ and from 1.3 to 6.3 µg kg⁻¹, respectively. In this study 10 PAs and four PANOs were targeted because they are commercially available as reference standards. Therefore, this study can only report the levels of these PAs and PANOs analysed in the herbal teas and TCMs. The results reported represent the minimum levels of PAs and PANOs present in the samples analysed; commercially available herbal teas (n = 18) and TCMs (n = 54). A total of 50% herbal teas and 78% Chinese medicines tested positive for one or more PAs and/or PANOs included within this study, ranging from 10 to 1733 and from 13 to 3668 µg kg⁻¹, respectively.

  16. Effects of derivatization reagents consisting of n-alkyl chloroformate/n-alcohol combinations in LC-ESI-MS/MS analysis of zwitterionic antiepileptic drugs.

    Science.gov (United States)

    Kostić, Nađa; Dotsikas, Yannis; Malenović, Anđelija; Medenica, Mirjana

    2013-11-15

    In the current study, three antiepileptic drugs with zwitterionic properties, namely vigabatrin, pregabalin and gabapentin, were chosen as model analytes to undergo derivatization by applying various n-alkyl chloroformate/n-alcohol combinations, followed by LC-ESI-MS/MS analysis. The employment of 16 combinations per drug using methyl, ethyl, propyl or butyl chloroformate coupled with methanol, ethanol, propanol or butanol, greatly affected a series of parameters of the derivatives, such as retention time on C8 column, signal expressed via areas, limit of detection values, as well as the yields of the main and side reactions. Practically, even slight modification of n-alkyl group of either chloroformate or alcohol resulted in significant changes in the chromatographic and mass spectrometric behavior of the novel derivative. It was clearly demonstrated that all the estimated parameters were highly correlated with the length of n-alkyl groups of the involved chloroformate and alcohol. The most significant influence was monitored in peak area values, indicating that the length of the n-alkyl chain plays an important role in electrospray ionization efficiency. For this parameter, increasing the n-alkyl chain from methyl to butyl led to increment up to 2089%, 508.7% and 1075% for area values of derivatized vigabatrin, pregabalin and gabapentin, respectively. These changes affected also the corresponding values of limits of detection, with the estimated improvements up to 1553%, 397.7% and 875.0% for the aforementioned derivatized drugs, respectively. Besides the obvious utilization of these conclusions in the development of bioanalytical methods for these analytes with the current protocol, this study offers valuable data which can be useful in more general approaches, giving insights into the effects of this derivatization reaction and its performances. Copyright © 2013 Elsevier B.V. All rights reserved.

  17. Determination of triazine herbicides and their metabolites in multiple medicinal parts of traditional Chinese medicines using streamlined pretreatment and UFLC-ESI-MS/MS.

    Science.gov (United States)

    Liu, Congmin; Dou, Xiaowen; Zhang, Lei; Li, Qian; Qin, Jia'an; Duan, Yaping; Yang, Meihua

    2018-01-01

    A rapid, sensitive, and reliable ultra-fast liquid chromatography combined with electrospray ionization tandem mass spectrometry (UFLC-ESI-MS/MS) method was established and applied to simultaneous determination of 31 triazine herbicides and their metabolites in multiple medicinal parts of traditional Chinese medicines (TCMs). A streamlined pretreatment approach using one-step extraction and dilution was proposed, which provided high-throughput processing, excellent recovery, and negligible interference. Afterwards, multiple-reaction monitoring (MRM) and information-dependent acquisition (IDA) triggered enhanced product ion spectra (EPI) was adopted to identify and quantify the targets in a single analysis. The optimized method was then validated according to the guidelines of the European Commission for the following parameters: Matrix effects, specificity, accuracy, precision, linearity, range, and stability. The LOD and LOQ for the 31 triazine herbicides were 0.1-10 μg kg -1 and 0.5-25 μg kg -1 , respectively. Recoveries at three concentration levels were within 67.9-120.3% with an associated precision RSD <20%. Using the proposed approach, trazines herbicides were determined from 44 commercially available TCMs. The detection rate of triazine herbicides residues was 15.9% of the total samples. Among them, atrazine, simeton, and simetryn were found in the radix, herba, and seed TCMs with values far below the referenced maximum residue limits (MRLs), but no residues were detected in either the flos or fructus. Taken together, this method has the potential to provide a means for triazines screening in extensive matrices, thereby laying the foundation for pesticide registration on TCMs. Moreover, it has the potential to guide further triazine residue control in TCMs. Copyright © 2017 Elsevier Ltd. All rights reserved.

  18. HPLC-ESI-MS/MS assessment of the tetrahydro-metabolites of cortisol and cortisone in bovine urine: promising markers of dexamethasone and prednisolone treatment.

    Science.gov (United States)

    Chiesa, Luca; Panseri, Sara; Pavlovic, Radmila; Cannizzo, Francesca Tiziana; Biolatti, Bartolomeo; Divari, Sara; Villa, Roberto; Arioli, Francesco

    2016-07-01

    The effects of long-term administration of low doses of dexamethasone (DX) and prednisolone (PL) on the metabolism of endogenous corticosteroids were investigated in veal calves. In addition to cortisol (F) and cortisone (E), whose interconversion is regulated by 11β-hydroxysteroid dehydrogenases (11βHSDs), special attention was paid to tetrahydrocortisol (THF), allo-tetrahydrocortisol (aTHF), tetrahydrocortisone (THE) and allo-tetrahydrocortisone (aTHE), which are produced from F and E by catalytic activity of 5α and 5β-reductases. A specifically developed HPLC-ESI-MS/MS method achieved the complete chromatographic separation of two pairs of diastereoisomers (THF/aTHF and THE/aTHE), which, with appropriate mass fragmentation patterns, provided an unambiguous conformation. The method was linear (r(2) > 0.9905; 0.5-25 ng ml(-1)), with LOQQ of 0.5 ng ml(-1). Recoveries were in range 75-114%, while matrix effects were minimal. The experimental study was carried out on three groups of male Friesian veal calves: group PL (n = 6, PL acetate 15 mg day(-1) p.o. for 31 days); group DX (n = 5, 5 mg of estradiol (E2) i.m., weekly, and 0.4 mg day(-1) of DX p.o. for 31 days) and a control group (n = 8). Urine was collected before, during (twice) and at the end of treatment. During PL administration, the tetrahydro-metabolite levels decreased gradually and remained low after the suspension of treatment. DX reduced urinary THF that persisted after the treatment, while THE levels decreased during the experiment, but rebounded substantially after the DX was withdrawn. Both DX and PL significantly interfered with the production of F and E, leading to their complete depletion. Taken together, the results demonstrate the influence of DX and PL administration on 11βHSD activity and their impact on dysfunction of the 5-reductase pathway. In conclusion, profiling tetrahydro-metabolites of F and E might serve as an alternative, indirect but reliable, non

  19. Profiling of ornithine lipids in bacterial extracts of Rhodobacter sphaeroides by reversed-phase liquid chromatography with electrospray ionization and multistage mass spectrometry (RPLC-ESI-MS(n)).

    Science.gov (United States)

    Granafei, Sara; Losito, Ilario; Trotta, Massimo; Italiano, Francesca; de Leo, Vincenzo; Agostiano, Angela; Palmisano, Francesco; Cataldi, Tommaso R I

    2016-01-15

    Ornithine lipids (OLs), a sub-group of the large (and of emerging interest) family of lipoamino acids of bacterial origin, contain a 3-hydroxy fatty acyl chain linked via an amide bond to the α-amino group of ornithine and via an ester bond to a second fatty acyl chain. OLs in extracts of Rhodobacter sphaeroides (R. sphaeroides) were investigated by high-performance reversed phase liquid chromatography (RPLC) with electrospray ionization mass spectrometry (ESI-MS) in negative ion mode using a linear ion trap (LIT). The presence of OLs bearing both saturated (i.e, 16:0, 17:0, 18:0, 19:0 and 20:0) and unsaturated chains (i.e., 18:1, 19:1, 19:2 and 20:1) was ascertained and their identification, even for isomeric, low abundance and partially co-eluting species, was achieved by low-energy collision induced dissociation (CID) multistage mass spectrometry (MS(n), n = 2-4). OLs signatures found in two R. sphaeroides strains, i.e., wild type 2.4.1 and mutant R26, were examined and up to 16 and 17 different OL species were successfully identified, respectively. OLs in both bacterial strains were characterized by several combinations of fatty chains on ester-linked and amide-linked 3-OH fatty acids. Multistage MS spectra of monoenoic amide-linked 3-OH acyl chains, allowed the identification of positional isomer of OL containing 18:1 (i.e. 9-octadecenoic) and 20:1 (i.e. 11-eicosenoic) fatty acids. The most abundant OL ([M-H](-) at m/z 717.5) in R. sphaeroides R26 was identified as OL 3-OH 20:1/19:1 (i.e., 3-OH-eicosenoic acid amide-linked to ornithine and esterified to a nonadecenoic chain containing a cyclopropane ring). An unusual OL (m/z 689.5 for the [M-H](-) ion), most likely containing a cyclopropene ester-linked acyl chain (i.e., OL 3-OH 18:0/19:2), was retrieved only in the carotenoidless mutant strain R26. Based on the biosynthetic pathways already known for cyclopropa(e)ne ring-including acyl chains, a plausible explanation was invoked for the enzymatic

  20. Validation of HPLC-ESI-MS/MS Protocol to Analyze EtG in Hair for Assessment of Chronic Excessive Alcohol Use in Thailand in Conjunction with AUDIT.

    Science.gov (United States)

    Thananchai, Thiwaphorn; Junkuy, Anongphan; Kittirattanapaiboon, Phunnapa; Sribanditmongkol, Pongruk

    2016-06-01

    Hair analysis for chronic excessive alcohol (ethanol) use has focused on ethyl glucuronide (EtG), a minor metabolite of ethanol. Preferred methods have involved high-performance liquid chromatography (HPLC) combined with tandem mass spectrometry (MS/MS) in line with an electrospray ionization (ESI) source. EtG analysis in hair has not yet been introduced to Thailand To validate an in-house HPLC-ESI-MS/MS hair analysis protocol for EtG and to apply it to a field sample of alcohol drinkers to assess different risk levels of alcohol consumption as measured by the Alcohol Use Disorders Identification Test (AUDIT). Validation procedures followed guidelines of the US Food and Drug Administration, the European Medicines Agency, and the Scientific Working Group for Forensic Toxicology. One hundred twenty subjects reported consuming alcohol during a 3-month period prior to enrollment. After taking the Thai-language version of AUDIT, subjects were divided on the basis of test scores into low, medium, and high-risk groups for chronic excessive alcohol use. The protocol satisfied the international standards for selectivity, specificity, accuracy, precision, and calibration curve. There was no significant matrix effect. Limits of detection and quantification (LOD/LOQ) were set at 15 pg of EtG per mg of hair. The protocol was not able to detect EtG in low-risk subjects (n = 38). Detection rates for medium-risk (n = 42) and high-risk subjects (n = 40) were 14.3% and 85%, respectively. The median of EtG concentration between these two groups were significantly different. Sensitivity and specificity were both more than 90% when EtG concentrations of high-risk subjects were compared with the 30 pg/mg cutoff recommended by the Society of Hair Testing (SoHT) for diagnosing chronic excessive alcohol consumption, based on an average ethanol daily intake greater than 60 g. The in-house protocol for EtG analysis in hair was validated according to international standards. The protocol is a

  1. Evaluation of γ-oryzanol content and composition from the grains of pigmented rice-germplasms by LC-DAD-ESI/MS.

    Science.gov (United States)

    Kim, Heon Woong; Kim, Jung Bong; Shanmugavelan, Poovan; Kim, Se Na; Cho, Young Sook; Kim, Haeng Ran; Lee, Jeong-Tae; Jeon, Weon-Tai; Lee, Dong Jin

    2013-04-15

    Rice is the staple food and one of the world’s three major grain crops. Rice contains more than 100 bioactive substances including phytic acid, isovitexin, γ-oryzanol, phytosterols, octacosanol, squalene, γ-aminobutyric acid (GABA), tocopherol, tocotrienol derivatives, etc. Out of them, γ-oryzanol is known to have important biological profile such as anti-oxidants, inhibitor of cholesterol oxidation, reduce serum cholesterol levels in animals, effective in the treatment of inflammatory diseases, inhibit tumor growth, reduce blood pressure and promotes food storage stability when used as a food additive, etc. Hence in the present investigation, we aimed to evaluate the content and composition of γ-oryzanol from pigmented rice germplasms using a liquid chromatography with diode array detection and electrospray ionization-mass spectrometry (LC-DAD-ESI/MS). In the present study, 33 exotic pigmented rice accessions (red, white and purple) have been evaluated. Among them, the contents of γ-oryzanol varied from 3.5 to 21.0 mg/100 g with a mean of 11.2 mg/100 g. A total of ten components of γ-oryzanol including Δ⁷-stigmastenyl ferulate were identified of which, cycloartenyl ferulate, 24-methylenecycloartanyl ferulate, campesteryl ferulate and sitosteryl ferulate were identified as the major components. The mean proportions of steryl ferulates were in the descending order of 24-methylenecycloartanyl ferulate > cycloartenyl ferulate > campesteryl ferulate > sitosteryl ferulate > Δ⁷-campestenyl ferulate > campestanyl ferulate > sitostanyl ferulate > Δ⁷-stigmastenyl ferulate > stigamsteryl ferulate > Δ⁷-sitostenyl ferulate. Almost 11 accessions (33%) showed higher content than the control rice Chucheongbyeo and higher proportions ranged from 10 to 15 mg/100 g. Interestingly, the red rice accession Liberian Coll. B11/B-11 (21.0 mg/100 g) showed higher content γ-oryzanol than control rice Jeokjinjubyeo (19.1 mg/100 g) and the purple rice accession Padi Adong

  2. UPLC-ESI-MS/MS method for the quantitative measurement of aliphatic diamines, trimethylamine N-oxide, and β-methylamino-l-alanine in human urine.

    Science.gov (United States)

    Bhandari, Deepak; Bowman, Brett A; Patel, Anish B; Chambers, David M; De Jesús, Víctor R; Blount, Benjamin C

    2018-04-15

    This work describes a quantitative high-throughput analytical method for the simultaneous measurement of small aliphatic nitrogenous biomarkers, i.e., 1,6-hexamethylenediamine (HDA), isophoronediamine (IPDA), β-methylamino-l-alanine (BMAA), and trimethylamine N-oxide (TMAO), in human urine. Urinary aliphatic diamines, HDA and IPDA, are potential biomarkers of environmental exposure to their corresponding diisocyanates. Urinary BMAA forms as a result of human exposure to blue-green algae contaminated food. And, TMAO is excreted in urine due to the consumption of carnitine- and choline-rich diets. These urinary biomarkers represent classes of small aliphatic nitrogen-containing compounds (N-compounds) that have a high aqueous solubility, low logP, and/or high basic pK a . Because of the highly polar characteristics, analysis of these compounds in complex sample matrices is often challenging. We report on the development of ion-pairing chemistry based ultra-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-ESI-MS/MS) method for the simultaneous measurement of these biomarkers in human urine. Chromatographic separation was optimized using heptafluorobutyric acid-(HFBA-) based mobile phase and a reversed-phase C18 column. All four analytes were baseline separated within 2.6 min with an overall run time of 5 min per sample injection. Sample preparation involved 4 h of acid hydrolysis followed by automated solid phase extraction (SPE) performed using strong cation exchange sorbent bed with 7 N ammonia solution in methanol as eluent. Limits of detection ranged from 0.05 ng/mL to 1.60 ng/mL. The inter-day and intra-day accuracy were within 10%, and reproducibility within 15%. The method is accurate, fast, and well-suited for biomonitoring studies within targeted groups, as well as larger population-based studies such as the U. S. National Health and Nutrition Examination Survey (NHANES). Published by Elsevier B.V.

  3. Determination of isopropylthioxanthone (ITX) in milk, yoghurt and fat by HPTLC-FLD, HPTLC-ESI/MS and HPTLC-DART/MS.

    Science.gov (United States)

    Morlock, Gertrud; Schwack, Wolfgang

    2006-06-01

    Two new HPTLC methods for quantification of isopropyl-9H-thioxanthen-9-one (ITX) in milk, yoghurt and fat samples have been developed. Extraction of ITX from milk and yoghurt was performed with a mixture of cyclohexane and ethyl acetate by employment of accelerated solvent extraction (ASE). For soy bean oil and margarine, a simple partitioning of ITX into acetonitrile was used. ITX and 2,4-diethyl-9H-thioxanthen-9-one (DTX) used as internal standard have been separated on silica gel 60 HPTLC plates with a mixture of toluene and n-hexane (4:1, v/v) and on RP18 HPTLC plates with a mixture of acetonitrile and water (9:1, v/v). Development was performed anti-parallel from both plate sides leading to a throughput of 36 separations in 7 min. Fluorescence measurement at 254/>400 nm was used for quantification. Limits of detection (S/N of 3) have been established to be 64 pg for ITX and DTX on both types of HPTLC plates. In fatty matrix (spiked butter) LOD of ITX was determined to be 1 mug kg(-1). In the working range monitored (20-200 microg kg(-1)) polynomial regression of ITX showed a relative standard deviation (sdv) of +/-1.51 % (r = 0.99981). Starting with the limit of quantification the response was linear (sdv = +/-2.18 %, r = 0.99893). Regarding repeatability (n = 9) a coefficient of variation (CV) of 1.1 % was obtained for ITX at 32 ng on silica gel plates and of 2.9 % on reversed-phase plates. Repeatabilities (n = 4) of ITX determination at 20, 50 and 100 microg kg(-1) in milk, yoghurt, soybean oil and margarine showed CVs between +/-1.0 and 6.4 %. The results prove that modern planar chromatography is a rapid and cost-efficient alternative method to quantify ITX in milk-based or fatty matrices. Only positive results are confirmed by online ESI/MS in the SIM mode (LOQ 128 pg) and by DART/MS involving a minimal employment of the MS device, which is a further advantage of HPTLC. Overall mean recovery rates of ITX at 20 or 50 and 100 microg kg(-1) (n = 8) were 41

  4. Determination of vandetanib in human plasma and cerebrospinal fluid by liquid chromatography electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS).

    Science.gov (United States)

    Bai, Feng; Johnson, Jennifer; Wang, Fan; Yang, Lei; Broniscer, Alberto; Stewart, Clinton F

    2011-09-01

    A sensitive and precise LC-ESI-MS/MS method for the determination of vandetanib (ZD6474) in human plasma and cerebrospinal fluid (CSF) using [(13)C,d(3)]-ZD6474 as an internal standard (ISTD) was developed and validated. Sample preparation consisted of a simple liquid-liquid extraction with tert-butyl methyl ether containing 0.1% or 0.5% ammonium hydroxide. ZD6474 and ISTD were separated on a Kinetex C18 column (2.6 μm, 50 mm × 2.1 mm) at ambient temperature with an isocratic mobile phase (acetonitrile/10mM ammonium formate=50/50, v/v, at pH 5.0) delivered at 0.11 mL/min. The retention time of both compounds was at 1.60 min in a runtime of three min. Detection was achieved by an API-3200 LC-MS/MS system, monitoring m/z 475.1/112.1 and m/z 479.1/116.2 for vandetanib and ISTD, respectively. The method was linear in the range of 0.25-50 ng/mL (R(2) ≥ 0.990) for the CSF curve and from 1.0 to 3000 ng/mL (R(2) ≥ 0.992) for the plasma curve. The mean recovery for vandetanib was 80%. Within-day and between-day precisions were ≤ 8.8% and ≤ 5.9% for CSF and plasma, respectively. Within-day and between-day accuracies ranged from 95.0 to 98.5% for CSF, and from 104.0 to 108.5% for plasma. Analysis of plasma from six different sources showed no matrix effect for vandetanib (MF=0.98, %CV ≤ 4.97, n=6). This method was successfully applied to the analysis of pharmacokinetic samples from children with brain tumors treated with oral vandetanib. Copyright © 2011 Elsevier B.V. All rights reserved.

  5. Determination of crenolanib in human serum and cerebrospinal fluid by liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS).

    Science.gov (United States)

    Roberts, Michael S; Turner, David C; Owens, Thandranese S; Ramachandran, Abhijit; Wetmore, Cynthia; Throm, Stacy L; Stewart, Clinton F

    2013-06-15

    A LC-ESI-MS/MS method for the determination of crenolanib (CP-868,596) in human serum was developed and validated employing d4-CP-868,596 as an internal standard (ISTD). In addition to human serum, the method was also partially validated for crenolanib determination in human cerebrospinal fluid (CSF) samples. Sample aliquots (50μl of serum or CSF) were prepared for analysis using liquid-liquid extraction (LLE) with tert-butyl methyl ether. Chromatography was performed using a phenomenex Gemini C18 column (3μm, 100mm×4.6mm I.D.) in a column heater set at 50°C and an isocratic mobile phase (methanol/water/formic acid at a volume ratio of 25/25/0.15, v/v/v). The flow rate was 0.45mL/min, and the retention time for both analyte and ISTD was less than 3.5min. Samples were analyzed with an API-5500 LC-MS/MS system (ESI) in positive ionization mode coupled to a Shimadzu HPLC system. The ion transitions monitored were m/z 444.4→373.1 and m/z 448.2→374.2 for crenolanib and ISTD, respectively. The method was linear over the range of 5-1000ng/mL for serum and 0.5-1000ng/mL for CSF. For human serum, both intra-day and inter-day precision were <4%, while intra-day and inter-day accuracy were within 8% of nominal values. Recovery was greater than 50% for both the analyte and ISTD. For CSF samples, both intra-day and inter-day precision were <9% except at the lower limit of quantification (LLOQ) which was <17%. The intra-day and inter-day accuracy were within 11% of the nominal CSF concentrations. After validation, this method was successfully applied to the analysis of serial pharmacokinetic samples obtained from a child treated with oral crenolanib. Copyright © 2013 Elsevier B.V. All rights reserved.

  6. ALLocator: an interactive web platform for the analysis of metabolomic LC-ESI-MS datasets, enabling semi-automated, user-revised compound annotation and mass isotopomer ratio analysis.

    Science.gov (United States)

    Kessler, Nikolas; Walter, Frederik; Persicke, Marcus; Albaum, Stefan P; Kalinowski, Jörn; Goesmann, Alexander; Niehaus, Karsten; Nattkemper, Tim W

    2014-01-01

    Adduct formation, fragmentation events and matrix effects impose special challenges to the identification and quantitation of metabolites in LC-ESI-MS datasets. An important step in compound identification is the deconvolution of mass signals. During this processing step, peaks representing adducts, fragments, and isotopologues of the same analyte are allocated to a distinct group, in order to separate peaks from coeluting compounds. From these peak groups, neutral masses and pseudo spectra are derived and used for metabolite identification via mass decomposition and database matching. Quantitation of metabolites is hampered by matrix effects and nonlinear responses in LC-ESI-MS measurements. A common approach to correct for these effects is the addition of a U-13C-labeled internal standard and the calculation of mass isotopomer ratios for each metabolite. Here we present a new web-platform for the analysis of LC-ESI-MS experiments. ALLocator covers the workflow from raw data processing to metabolite identification and mass isotopomer ratio analysis. The integrated processing pipeline for spectra deconvolution "ALLocatorSD" generates pseudo spectra and automatically identifies peaks emerging from the U-13C-labeled internal standard. Information from the latter improves mass decomposition and annotation of neutral losses. ALLocator provides an interactive and dynamic interface to explore and enhance the results in depth. Pseudo spectra of identified metabolites can be stored in user- and method-specific reference lists that can be applied on succeeding datasets. The potential of the software is exemplified in an experiment, in which abundance fold-changes of metabolites of the l-arginine biosynthesis in C. glutamicum type strain ATCC 13032 and l-arginine producing strain ATCC 21831 are compared. Furthermore, the capability for detection and annotation of uncommon large neutral losses is shown by the identification of (γ-)glutamyl dipeptides in the same strains

  7. Fuzzy clustering evaluation of the discrimination power of UV-Vis and (±) ESI-MS detection system in individual or coupled RPLC for characterization of Ginkgo Biloba standardized extracts.

    Science.gov (United States)

    Medvedovici, Andrei; Albu, Florin; Naşcu-Briciu, Rodica Domnica; Sârbu, Costel

    2014-02-01

    Discrimination power evaluation of UV-Vis and (±) electrospray ionization/mass spectrometric techniques, (ESI-MS) individually considered or coupled as detectors to reversed phase liquid chromatography (RPLC) in the characterization of Ginkgo Biloba standardized extracts, is used in herbal medicines and/or dietary supplements with the help of Fuzzy hierarchical clustering (FHC). Seventeen batches of Ginkgo Biloba commercially available standardized extracts from seven manufacturers were measured during experiments. All extracts were within the criteria of the official monograph dedicated to dried refined and quantified Ginkgo extracts, in the European Pharmacopoeia. UV-Vis and (±) ESI-MS spectra of the bulk standardized extracts in methanol were acquired. Additionally, an RPLC separation based on a simple gradient elution profile was applied to the standardized extracts. Detection was made through monitoring UV absorption at 220 nm wavelength or the total ion current (TIC) produced through (±) ESI-MS analysis. FHC was applied to raw, centered and scaled data sets, for evaluating the discrimination power of the method with respect to the origins of the extracts and to the batch to batch variability. The discrimination power increases with the increase of the intrinsic selectivity of the spectral technique being used: UV-Vis

  8. ALLocator: an interactive web platform for the analysis of metabolomic LC-ESI-MS datasets, enabling semi-automated, user-revised compound annotation and mass isotopomer ratio analysis.

    Directory of Open Access Journals (Sweden)

    Nikolas Kessler

    Full Text Available Adduct formation, fragmentation events and matrix effects impose special challenges to the identification and quantitation of metabolites in LC-ESI-MS datasets. An important step in compound identification is the deconvolution of mass signals. During this processing step, peaks representing adducts, fragments, and isotopologues of the same analyte are allocated to a distinct group, in order to separate peaks from coeluting compounds. From these peak groups, neutral masses and pseudo spectra are derived and used for metabolite identification via mass decomposition and database matching. Quantitation of metabolites is hampered by matrix effects and nonlinear responses in LC-ESI-MS measurements. A common approach to correct for these effects is the addition of a U-13C-labeled internal standard and the calculation of mass isotopomer ratios for each metabolite. Here we present a new web-platform for the analysis of LC-ESI-MS experiments. ALLocator covers the workflow from raw data processing to metabolite identification and mass isotopomer ratio analysis. The integrated processing pipeline for spectra deconvolution "ALLocatorSD" generates pseudo spectra and automatically identifies peaks emerging from the U-13C-labeled internal standard. Information from the latter improves mass decomposition and annotation of neutral losses. ALLocator provides an interactive and dynamic interface to explore and enhance the results in depth. Pseudo spectra of identified metabolites can be stored in user- and method-specific reference lists that can be applied on succeeding datasets. The potential of the software is exemplified in an experiment, in which abundance fold-changes of metabolites of the l-arginine biosynthesis in C. glutamicum type strain ATCC 13032 and l-arginine producing strain ATCC 21831 are compared. Furthermore, the capability for detection and annotation of uncommon large neutral losses is shown by the identification of (γ-glutamyl dipeptides in

  9. Development of Asset Management Control Application for Direktorat Jenderal Sumber Daya dan Perangkat Pos dan Informatika

    Directory of Open Access Journals (Sweden)

    Richard Richard

    2017-09-01

    Full Text Available The purpose of this research was to identify problems, analyze needs, and develop management information system especially the process internal control of asset management on Direktorat Jenderal Sumber Daya dan Perangkat Pos dan Informatika (SDPPI - government communication and informatics organization. This system development used the System Development Life Cycle (SDLC method which refers to 4 phases. Those were initiation and business feasibility, requirements definitions, functional design, and verification. The analysis used to support the research methods was Enterprise Architecture (EA and SWOT. The analysis was conducted on business process that was running at the moment. The results show that the management information system in the form of web-based applications can help the process based on activity logging assets, assets allocation, complaints, and user guide in accordance with the needs of the Direktorat Jendral SDPPI. The design of this application can also help the existing asset management process to become more efficient and effective.

  10. Development of a rapid and sensitive LC-ESI/MS/MS assay for the quantification of propofol using a simple off-line dansyl chloride derivatization reaction to enhance signal intensity.

    Science.gov (United States)

    Beaudry, Francis; Guénette, Sarah Annie; Winterborn, Andrew; Marier, Jean-Francois; Vachon, Pascal

    2005-09-15

    A rapid, selective and sensitive method was developed for the determination of propofol concentration using an off-line dansyl chloride derivatization step to enhance signal intensity. The method consisted of a protein precipitation extraction followed by derivatization with dansyl chloride and analysis by liquid chromatography ionspray tandem mass spectrometry (LC-ESI/MS/MS). The separation was achieved using a 100 mm x 2 mm C8 analytical column combined with an isocratic mobile phase composed of 80:20 acetonitrile: 0.5% formic acid in water. Signal intensity of the propofol-dansyl chloride derivative was increased up to 200-fold as compared to the underivatized propofol in positive electrospray mode. An analytical range of 20-20,000 ng/mL was used in the calibration curve of plasma and blood samples. The novel method met all requirements of specificity, sensitivity, linearity, precision, accuracy and stability. A pharmacokinetic study was performed in rats and the novel analytical method was used as a routine analysis to provide enhanced measurements of plasma and blood concentrations of propofol. Blood and plasma pharmacokinetic results show that a very important fraction of propofol distributes into red blood cells. In conclusion, a rapid and sensitive LC-ESI/MS/MS method using a derivatization agent was developed to enhance signal intensity of propofol. Routine analysis with the novel method provided accurate results and enhanced the detection levels of plasma and blood concentrations of propofol to better characterize the in vivo biodisposition of propofol.

  11. Theory of the Protein Equilibrium Population Snapshot by H/D Exchange Electrospray Ionization Mass Spectrometry (PEPS-HDX-ESI-MS) Method used to obtain Protein Folding Energies/Rates and Selected Supporting Experimental Evidence.

    Science.gov (United States)

    Liyanage, Rohana; Devarapalli, Nagarjuna; Pyland, Derek B; Puckett, Latisha M; Phan, N H; Starch, Joel A; Okimoto, Mark R; Gidden, Jennifer; Stites, Wesley E; Lay, Jackson O

    2012-12-15

    Protein equilibrium snapshot by hydrogen/deuterium exchange electrospray ionization mass spectrometry (PEPS-HDX-ESI-MS or PEPS) is a method recently introduced for estimating protein folding energies and rates. Herein we describe the basis for this method using both theory and new experiments. Benchmark experiments were conducted using ubiquitin because of the availability of reference data for folding and unfolding rates from NMR studies. A second set of experiments was also conducted to illustrate the surprising resilience of the PEPS to changes in HDX time, using staphylococcal nuclease and time frames ranging from a few seconds to several minutes. Theory suggests that PEPS experiments should be conducted at relatively high denaturant concentrations, where the protein folding/unfolding rates are slow with respect to HDX and the life times of both the closed and open states are long enough to be sampled experimentally. Upon deliberate denaturation, changes in folding/unfolding are correlated with associated changes in the ESI-MS signal upon fast HDX. When experiments are done quickly, typically within a few seconds, ESI-MS signals, corresponding to the equilibrium population of the native (closed) and denatured (open) states can both be detected. The interior of folded proteins remains largely un-exchanged. Amongst MS methods, the simultaneous detection of both states in the spectrum is unique to PEPS and provides a "snapshot" of these populations. The associated ion intensities are used to estimate the protein folding equilibrium constant (or the free energy change, ΔG). Linear extrapolation method (LEM) plots of derived ΔG values for each denaturant concentration can then be used to calculate ΔG in the absence of denaturant, ΔG(H(2)O). In accordance with the requirement for detection of signals for both the folded and unfolded states, this theoretical framework predicts that PEPS experiments work best at the middle of the denaturation curve where natured

  12. Profiling of adrenocorticotropic hormone and arginine vasopressin in human pituitary gland and tumor thin tissue sections using droplet-based liquid-microjunction surface-sampling-HPLC-ESI-MS-MS.

    Science.gov (United States)

    Kertesz, Vilmos; Calligaris, David; Feldman, Daniel R; Changelian, Armen; Laws, Edward R; Santagata, Sandro; Agar, Nathalie Y R; Van Berkel, Gary J

    2015-08-01

    Described here are the results from the profiling of the proteins arginine vasopressin (AVP) and adrenocorticotropic hormone (ACTH) from normal human pituitary gland and pituitary adenoma tissue sections, using a fully automated droplet-based liquid-microjunction surface-sampling-HPLC-ESI-MS-MS system for spatially resolved sampling, HPLC separation, and mass spectrometric detection. Excellent correlation was found between the protein distribution data obtained with this method and data obtained with matrix-assisted laser desorption/ionization (MALDI) chemical imaging analyses of serial sections of the same tissue. The protein distributions correlated with the visible anatomic pattern of the pituitary gland. AVP was most abundant in the posterior pituitary gland region (neurohypophysis), and ATCH was dominant in the anterior pituitary gland region (adenohypophysis). The relative amounts of AVP and ACTH sampled from a series of ACTH-secreting and non-secreting pituitary adenomas correlated with histopathological evaluation. ACTH was readily detected at significantly higher levels in regions of ACTH-secreting adenomas and in normal anterior adenohypophysis compared with non-secreting adenoma and neurohypophysis. AVP was mostly detected in normal neurohypophysis, as expected. This work reveals that a fully automated droplet-based liquid-microjunction surface-sampling system coupled to HPLC-ESI-MS-MS can be readily used for spatially resolved sampling, separation, detection, and semi-quantitation of physiologically-relevant peptide and protein hormones, including AVP and ACTH, directly from human tissue. In addition, the relative simplicity, rapidity, and specificity of this method support the potential of this basic technology, with further advancement, for assisting surgical decision-making. Graphical Abstract Mass spectrometry based profiling of hormones in human pituitary gland and tumor thin tissue sections.

  13. Diagnostic fragment-ion-based and extension strategy coupled to DFIs intensity analysis for identification of chlorogenic acids isomers in Flos Lonicerae Japonicae by HPLC-ESI-MS(n).

    Science.gov (United States)

    Zhang, Jia-Yu; Zhang, Qian; Li, Ning; Wang, Zi-Jian; Lu, Jian-Qiu; Qiao, Yan-Jiang

    2013-01-30

    A method of modified diagnostic fragment-ion-based extension strategy (DFIBES) coupled to DFIs (diagnostic fragmentation ions) intensity analysis was successfully established to simultaneously screen and identify the chlorogenic acids (CGAs) in Flos Lonicerae Japonicae (FLJ) by HPLC-ESI-MS(n). DFIs, such as m/z 191 [quinic acid-H](-), m/z 179 [caffeic acid-H](-) and m/z 173 [quinic acid-H-H2O](-) were determined or proposed from the fragmentation patterns analysis of corresponding reference substances for every chemical family of CGAs. A "structure extension" method was then proposed based on the well-demonstrated fragmentation patterns and was successively applied into the rapid screening of CGAs in FLJ. Considering that substitution isomerism is a common phenomenon, a full ESI-MS(n) fragmentation analysis according to the intensity of DFIs has been performed to identify the CGA isomers. Based on the DFIs and intensity analysis, 41 peaks attributed to CGAs including 4 caffeoylquinic acids (CQA), 7 CQA glycosides, 6 dicaffeoylquinic acids (DiCQA), 10 DiCQA glycosides, 1 tricaffeoylquinic acids (TriCQA), 4p-coumaroylquinic acids (pCoQA), 3 feruloylquinic acids (FQA) and 6 caffeoylferuloylquinic acids (CFQA) were identified preliminarily in a 65-min chromatographic run. It was the first time to systematically report the presence of CGAs in FLJ, especially for CQA glycosides, DiCQA glycosides, TriCQA, pCoQA and CFQA. All the results indicated that the method of developed DFIBES coupled to DFIs analysis was feasible, reliable and universal for screening and identifying the constituents with the same carbon skeletons especially the isomeric compounds from the complex extract of TCMs. Copyright © 2012 Elsevier B.V. All rights reserved.

  14. A method of coupling the Paternò-Büchi reaction with direct infusion ESI-MS/MS for locating the C[double bond, length as m-dash]C bond in glycerophospholipids.

    Science.gov (United States)

    Stinson, Craig A; Xia, Yu

    2016-06-21

    Tandem mass spectrometry (MS/MS) coupled with soft ionization is established as an essential platform for lipid analysis; however, determining high order structural information, such as the carbon-carbon double bond (C[double bond, length as m-dash]C) location, remains challenging. Recently, our group demonstrated a method for sensitive and confident lipid C[double bond, length as m-dash]C location determination by coupling online the Paternò-Büchi (PB) reaction with nanoelectrospray ionization (nanoESI) and MS/MS. Herein, we aimed to expand the scope of the PB reaction for lipid analysis by enabling the reaction with infusion ESI-MS/MS at much higher flow rates than demonstrated in the nanoESI setup (∼20 nL min(-1)). In the new design, the PB reaction was effected in a fused silica capillary solution transfer line, which also served as a microflow UV reactor, prior to ESI. This setup allowed PB reaction optimization and kinetics studies. Under optimized conditions, a maximum of 50% PB reaction yield could be achieved for a standard glycerophosphocholine (PC) within 6 s of UV exposure over a wide flow rate range (0.1-10 μL min(-1)). A solvent composition of 7 : 3 acetone : H2O (with 1% acid or base modifier) allowed the highest PB yields and good lipid ionization, while lower yields were obtained with an addition of a variety of organic solvents. Radical induced lipid peroxidation was identified to induce undesirable side reactions, which could be effectively suppressed by eliminating trace oxygen in the solution via N2 purge. Finally, the utility of coupling the PB reaction with infusion ESI-MS/MS was demonstrated by analyzing a yeast polar lipid extract where C[double bond, length as m-dash]C bond locations were revealed for 35 glycerophospholipids (GPs).

  15. Simultaneous quantitative determination of multiple bioactive markers in Ocimum sanctum obtained from different locations and its marketed herbal formulations using UPLC-ESI-MS/MS combined with principal component analysis.

    Science.gov (United States)

    Pandey, Renu; Chandra, Preeti; Srivastava, Mukesh; Mishra, D K; Kumar, Brijesh

    2015-01-01

    Ocimum sanctum L., with phenolic acids, flavonoids, propenyl phenols and terpenoids as active pharmacological constituents, is a popular medicinal herb and is present as an ingredient in many herbal formulations. Therefore, development of a reliable analytical method for simultaneous determination of the pharmacologically active constituents of O. sanctum is of high importance. To develop and validate a new, rapid, sensitive and selective UPLC-ESI/MS/MS method for simultaneous determination of 23 bioactive markers including phenolic acids, flavonoids, propenyl phenol and terpenoid in the leaf extract and marketed herbal formulations of O. sanctum. An UPLC-ESI/MS/MS method using negative electrospray ionisation (ESI) in multiple-reaction-monitoring (MRM) mode was used for simultaneous determination. Chromatographic separation was achieved on an Acquity UPLC BEH C18 -column using a gradient elution with 0.1% formic acid in water and 0.1% formic acid in acetonitrile. Principal component analysis (PCA) was applied to correlate and discriminate eight geographical collections of O. sanctum based on quantitative data of the analytes. The developed method was validated as per International Conference on Harmonization guidelines and found to be accurate, with overall recovery in the range 95.09-104.84% (RSD ≤ 1.85%), precise (RSD ≤ 1.98%) and linear (r(2)  ≥ 0.9971) over the concentration range of 0.5-1000 ng/mL. Ursolic acid was found to be the most abundant marker in all the samples investigated, except for the marketed tablet. The method established is simple, rapid and sensitive, hence it can be reliably utilised for the quality control of O. sanctum and derived herbal formulations. Copyright © 2015 John Wiley & Sons, Ltd.

  16. Simultaneous determination of amlodipine, valsartan and hydrochlorothiazide by LC–ESI-MS/MS and its application to pharmacokinetics in rats

    Directory of Open Access Journals (Sweden)

    Shankar Ganesh Gadepalli

    2014-12-01

    Full Text Available Polypill is a fixed-dose combination that contains three or more active ingredients used as a single daily pill to achieve a large effect in preventing cardiovascular disease with minimal adverse effects. A novel and accurate liquid chromatography tandem mass spectrometry method using electrospray ionization mode has been developed and validated for the simultaneous determination of amlodipine (AMD, valsartan (VAL using losartan (LOS as an internal standard (IS, and hydrochlorothiazide (HCT using furosemide (FSD as an IS. The separation was carried on Aquasil C18 (50 mm×2.1 mm, 5 µm reversed phase column using acetonitrile and water containing 0.1% formic acid (50:50, v/v as the mobile phase. The method was validated in terms of linearity, accuracy and precision over the concentration range of 1–1000 ng/mL. The intra and inter-day precision and accuracy, stability and extraction recoveries of all the analytes were in the acceptable range. This method can be successfully applied to the pharmacokinetic study of AMD, VAL and HCT when given as a polypill. Keywords: Amlodipine, Valsartan, Hydrochlorothiazide, Exforge HCT, Polypill

  17. Simultaneous quantitation of hydroxychloroquine and its metabolites in mouse blood and tissues using LC-ESI-MS/MS: An application for pharmacokinetic studies.

    Science.gov (United States)

    Chhonker, Yashpal S; Sleightholm, Richard L; Li, Jing; Oupický, David; Murry, Daryl J

    2018-01-01

    Hydroxychloroquine (HCQ) has been shown to disrupt autophagy and sensitize cancer cells to radiation and chemotherapeutic agents. However, the optimal delivery method, dose, and tumor concentrations required for these effects are not known. This is in part due to a lack of sensitive and reproducible analytical methods for HCQ quantitation in small animals. As such, we developed and validated a selective and sensitive liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) method for simultaneous quantitation of hydroxychloroquine and its metabolites in mouse blood and tissues. The chromatographic separation and detection of analytes were achieved on a reversed phase Thermo Aquasil C 18 (50×4.6mm, 3μ) column, with gradient elution using 0.2% formic acid and 0.1% formic acid in methanol as mobile phase at a flow rate of 0.5mL/min. Simple protein precipitation was utilized for extraction of analytes from the desired matrix. Analytes were separated and quantitated using MS/MS with an electrospray ionization source in positive multiple reaction monitoring (MRM) mode. The MS/MS response was linear over the concentration range from 1 to 2000ng/mL for all analytes with a correlation coefficient (R 2 ) of 0.998 or better. The within- and between-day precision (relative standard deviation, % RSD) and accuracy were within the acceptable limits per FDA guidelines. The validated method was successfully applied to a preclinical pharmacokinetic mouse study involving low volume blood and tissue samples for hydroxychloroquine and metabolites. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Application of HPLC and ESI-MS techniques in the analysis of phenolic acids and flavonoids from green leafy vegetables (GLVs).

    Science.gov (United States)

    Kumar, B Ramesh

    2017-12-01

    Diets containing high proportions of fruits and vegetables reduce the risk of onset of chronic diseases. The role of herbal medicines in improving human health is gaining popularity over the years, which also increases the need for safety and efficiency of these products. Green leafy vegetables (GLVs) are the richest source of phenolic compounds with excellent antioxidant properties. Increased consumption of diets containing phenolic compounds may give positive and better results to human health and significantly improves the immune system. Highly selective, susceptible and versatile analytical techniques are necessary for extraction, identification, and quantification of phenolic compounds from plant extracts, which helps to utilize their important biological properties. Recent advances in the pre-treatment procedures, separation techniques and spectrometry methods are used for qualitative and quantitative analysis of phenolic compounds. The online coupling of liquid chromatography with mass spectrometry (LC-MS) has become a useful tool in the metabolic profiling of plant samples. In this review, the separation and identification of phenolic acids and flavonoids from GLVs by LC-MS have been discussed along with the general extraction procedures and other sources of mass spectrometer used. The review is devoted to the understanding of the structural configuration, nature and accumulation pattern of phenolic acids and flavonoids in plants and to highlighting the recent developments in the chemical investigation of these compounds by chromatographic and spectroscopic techniques. It concludes with the advantages of the combination of these two methods and prospects.

  19. Application of HPLC and ESI-MS techniques in the analysis of phenolic acids and flavonoids from green leafy vegetables (GLVs)

    Institute of Scientific and Technical Information of China (English)

    Ramesh Kumar Bonta

    2017-01-01

    Diets containing high proportions of fruits and vegetables reduce the risk of onset of chronic diseases.The role of herbal medicines in improving human health is gaining popularity over the years,which also increases the need for safety and efficiency of these products.Green leafy vegetables(GLVs)are the richest source of phenolic compounds with excellent antioxidant properties. Increased consumption of diets containing phenolic compounds may give positive and better results to human health and significantly improves the immune system.Highly selective,susceptible and versatile analytical techniques are necessary for extraction,identifica-tion, and quantification of phenolic compounds from plant extracts, which helps to utilize their important biological properties. Recent advances in the pre-treatment procedures, separation techniques and spectro-metry methods are used for qualitative and quantitative analysis of phenolic compounds.The online coupling of liquid chromatography with mass spectrometry(LC–MS)has become a useful tool in the metabolic profiling of plant samples.In this review,the separation and identification of phenolic acids and flavonoids from GLVs by LC–MS have been discussed along with the general extraction procedures and other sources of mass spectrometer used. The review is devoted to the understanding of the structural configuration, nature and accumulation pattern of phenolic acids and flavonoids in plants and to highlighting the recent developments in the chemical investigation of these compounds by chromatographic and spectroscopic techniques.It concludes with the advantages of the combination of these two methods and prospects.

  20. The application of HPLC ESI MS in the investigation of the flavonoids and flavonoid glycosides of a Caribbean Lamiaceae plant with potential for bioaccumulation.

    Science.gov (United States)

    Peter, Sonia R; Peru, Kerry M; Fahlman, Brian; McMartin, Dena W; Headley, John V

    2015-01-01

    As part of an exchange technology program between the government of Barbados and Environment Canada, methanolic and aqueous extracts from the flavonoid-rich Lamiaceae family were characterized using negative-ion electrospray mass spectrometry. The species investigated is part of the Caribbean Pharmacopoeia, and is used for a variety of health issues, including colds, flu, diabetes, and hypertension. The extracts were investigated for structural elucidation of phenolics, identification of chemical taxonomic profile, and evidence of bio-accumulator potential. The methanolic and aqueous leaf extracts of Plectranthus amboinicus yielded rosmarinic acid, ladanein, cirsimaritin, and other methoxylated flavonoids. This genus also shows a tendency to form conjugates with monosaccharides, including glucose, galactose, and rhamnose. The aqueous extract yielded four isomeric rhamnosides. The formation of conjugates by Plectranthus amboinicus is thus evidence of high bioaccumulator significance.

  1. Modifications of the acidic soluble salivary proteome in human children from birth to the age of 48months investigated by a top-down HPLC-ESI-MS platform.

    Science.gov (United States)

    Manconi, B; Cabras, T; Pisano, E; Sanna, M T; Olianas, A; Fanos, V; Faa, G; Nemolato, S; Iavarone, F; Castagnola, M; Messana, I

    2013-10-08

    During the first year of life the infant oral environment undergoes dramatic changes. To investigate how the salivary proteome of human children evolves during infant development we have analyzed whole saliva of 88 children aged between 0 and 48months by a top-down platform based on RP-HPLC-ESI-MS. Children were divided according to their age into five groups (A, 0-6months, N=17; B, 7-12months, N=14; C, 13-24months, N=32; D, 25-36months, N=16; E, 37-48months, N=9). The proteins and peptides analyzed were histatins (histatin-1, histatin-3 1/24), acidic proline-rich proteins, statherin, P-B peptide, and salivary cystatins. Protein and peptide quantification based on the area of the RP-HPLC-ESI-MS extracted ion current peak evidenced that: (i) concentrations of the major salivary proteins/peptides showed a minimum in the 0-6-month-old group and increased with age; (ii) the level of histatin-1 reached a maximum in the 7-12-month-old group, a minimum in the 13-24-month-aged babies and it increased again in the 25-36-month-old group; (iii) S-type cystatins were almost undetectable in the 0-6-month-old group; (iv) P-B peptide concentration greatly increased with age; (v) histatin-3 1/24 and statherin concentrations did not show any age-related variation. The top-down proteomic approach undertaken in this work reveals that the salivary proteome of human children from birth to 48months of age shows important quantitative modifications. The concentrations of the major salivary proteins, with the exception of statherin and histatin-3 1/24, showed a minimum in the 0-6-month-old group when the expression in salivary glands is probably not fully activated. Concentrations of the salivary proteins slowly increased with age, with different trends. Only histatin-1 showed the highest concentration in the 7-12-month-old group, followed by a decrease in the 13-24-month-aged children. This particular trend could be related to the phenomenon of eruption of primary dentition. This study

  2. Psidium guajava L. leaves as source of proanthocyanidins: Optimization of the extraction method by RSM and study of the degree of polymerization by NP-HPLC-FLD-ESI-MS.

    Science.gov (United States)

    Díaz-de-Cerio, Elixabet; Pasini, Federica; Verardo, Vito; Fernández-Gutiérrez, Alberto; Segura-Carretero, Antonio; Caboni, Maria Fiorenza

    2017-01-30

    Due to the importance of the proanthocyanidins (PAs) bioactivity and its relationship with the PAs degree of polymerization (DP), an experimental design was carried out to establish the best extraction conditions in order to evaluate the proanthocyanidins content and their degree of polymerization in Psidium guajava leaves at different oxidation state. Optimal conditions achieved by response surface methodology were 50% acetone/water (v/v), 48°C, 30min, and 0% acetic acid (v/v). The highest DP has been found in the low oxidized state (DP 13 plus the polymers). Medium and high oxidized state leaves reported a DP 11 plus the polymers. The total amounts of proanthocyanidins (sum of PAs by HPLC-FLD-ESI-MS) decreased when oxidation state of leaves increased (15.8±0.4, 12.6±0.4, and 10.5±0.3mg/g leaf dry weight (d.w.) in low, medium and high oxidized state leaves, respectively). Guava leaves present an interesting source of low DP-PAs. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Hepatoprotective and antioxidant effect of Bauhinia hookeri extract against carbon tetrachloride-induced hepatotoxicity in mice and characterization of its bioactive compounds by HPLC-PDA-ESI-MS/MS.

    Science.gov (United States)

    Al-Sayed, Eman; Martiskainen, Olli; Seif el-Din, Sayed H; Sabra, Abdel-Nasser A; Hammam, Olfat A; El-Lakkany, Naglaa M; Abdel-Daim, Mohamed M

    2014-01-01

    The hepatoprotective and antioxidant activity of Bauhinia hookeri ethanol extract (BHE) against CCl4-induced liver injury was investigated in mice. BHE was administered (500 and 1000 mg/kg/day) along with CCl4 for 6 weeks. The hepatic marker enzymes: alanine aminotransferase (ALT), aspartate aminotransferase (AST), and alkaline phosphatase (ALP) were determined in the serum. The antioxidant parameters: glutathione (GSH), superoxide dismutase (SOD), glutathione peroxidase (GPx), glutathione reductase (GR), glutathione transferase (GST), and malondialdehyde (MDA) were estimated in the liver homogenate. BHE treatment significantly inhibited the CCl4-induced increase in ALT (44 and 64%), AST (36 and 46%), ALP (28 and 42%), and MDA (39 and 51%) levels at the tested doses, respectively. Moreover, BHE treatment markedly increased the activity of antioxidant parameters GSH, GPx, GR, GST, and SOD. Histological observations confirmed the strong hepatoprotective activity. These results suggest that a dietary supplement of BHE could exert a beneficial effect against oxidative stress and various liver diseases by enhancing the antioxidant defense status, reducing lipid peroxidation, and protecting against the pathological changes of the liver. The hepatoprotective activity of BHE is mediated, at least in part, by the antioxidant effect of its constituents. The active constituents of BHE were identified by HPLC-PDA-ESI/MS/MS.

  4. Determination and production of antimicrobial compounds by Aspergillus clavatonanicus strain MJ31, an endophytic fungus from Mirabilis jalapa L. using UPLC-ESI-MS/MS and TD-GC-MS analysis.

    Directory of Open Access Journals (Sweden)

    Vineet Kumar Mishra

    Full Text Available Endophytic fungi associated with medicinal plants are reported as potent producers of diverse classes of secondary metabolites. In the present study, an endophytic fungi, Aspergillus clavatonanicus strain MJ31, exhibiting significant antimicrobial activity was isolated from roots of Mirabilis jalapa L., was identified by sequencing three nuclear genes i.e. internal transcribed spacers ribosomal RNA (ITS rRNA, 28S ribosomal RNA (28S rRNA and translation elongation factor 1- alpha (EF 1α. Ethyl acetate extract of strain MJ31displayed significant antimicrobial potential against Bacillus subtilis, followed by Micrococccus luteus and Staphylococcus aureus with minimum inhibitory concentrations (MIC of 0.078, 0.156 and 0.312 mg/ml respectively. In addition, the strain was evaluated for its ability to synthesize bioactive compounds by the amplification of polyketide synthase (PKS and non ribosomal peptide synthetase (NRPS genes. Further, seven antibiotics (miconazole, ketoconazole, fluconazole, ampicillin, streptomycin, chloramphenicol, and rifampicin were detected and quantified using UPLC-ESI-MS/MS. Additionally, thermal desorption-gas chromatography mass spectrometry (TD-GC-MS analysis of strain MJ31 showed the presence of 28 volatile compounds. This is the first report on A. clavatonanicus as an endophyte obtained from M. jalapa. We conclude that A. clavatonanicus strain MJ31 has prolific antimicrobial potential against both plant and human pathogens and can be exploited for the discovery of new antimicrobial compounds and could be an alternate source for the production of secondary metabolites.

  5. Pistachio oil (Pistacia vera L. cv. Uzun): Characterization of key odorants in a representative aromatic extract by GC-MS-olfactometry and phenolic profile by LC-ESI-MS/MS.

    Science.gov (United States)

    Sonmezdag, Ahmet Salih; Kelebek, Hasim; Selli, Serkan

    2018-02-01

    Volatile, aroma-active, and phenolic compounds of pistachio oil obtained from cv. Uzun were investigated in the current study. To obtain a representative aromatic extract, three of the most widely used extraction methods were compared using a representative test; the solvent-assisted flavour extraction (SAFE) aromatic extract from pistachio oil was found to be the most representative. A total of 50 aroma compounds were determined in pistachio oil and it was found that terpenes, aldehydes, and alcohols were the most abundant volatile compounds. Applying GC-MS-olfactometry and aroma extract dilution analysis (AEDA) resulted in a total of 14 aroma-active areas being detected in the extract of pistachio oil. In the phenolic fraction obtained by the LC-ESI-MS/MS method, a total of 12 phenolic compounds was found in the pistachio oil, of which seven compounds were reported for the first time. Eriodictyol-7-O-glucoside and protocatechuic acid were the most dominant phenolic compounds. Copyright © 2017 Elsevier Ltd. All rights reserved.

  6. Insights on the mechanism of thioredoxin reductase inhibition by gold N-heterocyclic carbene compounds using the synthetic linear selenocysteine containing C-terminal peptide hTrxR(488-499): an ESI-MS investigation.

    Science.gov (United States)

    Pratesi, Alessandro; Gabbiani, Chiara; Michelucci, Elena; Ginanneschi, Mauro; Papini, Anna Maria; Rubbiani, Riccardo; Ott, Ingo; Messori, Luigi

    2014-07-01

    Gold-based drugs typically behave as strong inhibitors of the enzyme thioredoxin reductase (hTrxR), possibly as the consequence of direct Gold(I) coordination to its active site selenocysteine. To gain a deeper insight into the molecular basis of enzyme inhibition and prove gold-selenocysteine coordination, the reactions of three parent Gold(I) NHC compounds with the synthetic C-terminal dodecapeptide of hTrxR containing Selenocysteine at position 498, were investigated by electrospray ionization mass spectrometry (ESI-MS). Formation of 1:1 Gold-peptide adducts, though in highly different amounts, was demonstrated in all cases. In these adducts the same [Au-NHC](+) moiety is always associated to the intact peptide. Afterward, tandem MS experiments, conducted on a specific Gold-peptide complex, pointed out that Gold is coordinated to the selenolate group. The relatively large strength of the Gold-selenolate coordinative bond well accounts for potent enzyme inhibition typically afforded by these Gold(I) compounds. In a selected case, the time course of enzyme inhibition was explored. Interestingly, enzyme inhibition turned out to show up very quickly and reached its maximum just few minutes after mixing. Overall, the present results offer some clear insight into the process of thioredoxin reductase inhibition by Gold-based compounds. Copyright © 2014 Elsevier Inc. All rights reserved.

  7. Ultrasonic-assisted extraction combined with sample preparation and analysis using LC-ESI-MS/MS allowed the identification of 24 new phenolic compounds in pecan nut shell [Carya illinoinensis (Wangenh) C. Koch] extracts.

    Science.gov (United States)

    Hilbig, Josiane; Alves, Victor Rodrigues; Müller, Carmen Maria Olivera; Micke, Gustavo Amadeu; Vitali, Luciano; Pedrosa, Rozangela Curi; Block, Jane Mara

    2018-04-01

    Ultrasonic-assisted extraction combined with statistical tools (factorial design, response surface methodology and kinetics) were used to evaluate the effects of the experimental conditions of temperature, solid-to-solvent ratio, ethanol concentration and time for the extraction of the total phenolic content from pecan nut shells. The optimal conditions for the aqueous and hydroalcoholic extract (with 20% v/v of ethanol) were 60 and 80 °C; solid to solvent ratio of 30 mL·g -1 (for both) and extraction time of 35 and 25 min, respectively. Using these optimize extraction conditions, 426 and 582 mg GAE·g -1 of phenolic compounds, from the aqueous and hydroalcoholic phases respectively, were obtained. In addition, the analysis of the phenolic compounds using the LC-ESI-MS/MS system allowed the identification of 29 phenolic compounds, 24 of which had not been reported in literature for this raw material yet. Copyright © 2018. Published by Elsevier Ltd.

  8. Identification of C-geranylated flavonoids from Paulownia catalpifolia Gong Tong fruits by HPLC-DAD-ESI-MS/MS and their anti-aging effects on 2BS cells induced by H2O2.

    Science.gov (United States)

    Tang, Wen-Zhao; Wang, Ying-Ai; Gao, Tian-Yang; Wang, Xiao-Jing; Zhao, Yun-Xue

    2017-05-01

    The fruits of Paulownia catalpifolia Gong Tong are used as a Chinese folk herbal medicine for the treatment of enteritis, tonsillitis, bronchitis, and dysentery, etc. Our previous study has identified new C-geranylated flavanones with obvious anti-proliferative effects in lung cancer A549 cells. In the present study, a new C-geranylated flavone, paucatalinone C (1) and five known C-geranylated flavanones (2-6) were isolated. In addition, a total of 34 C-geranylated flavonoids were detected by HPLC-DAD-ESI-MS/MS coupling techniques from the CH 2 Cl 2 extract of P. catalpifolia. Futhermore, anti-aging effects of isolated compounds were evaluated in vitro with premature senescent 2BS cells induced by H 2 O 2 . Phytochemical results indicated that P. catalpifolia was a natural resource of abundant C-geranylated flavonoids. Diplacone (3) and paucatalinone A (5) were the potent anti-aging agents in the premature senescent 2BS cells induced by H 2 O 2 and the C-geranyl substituent may be an important factor because of its lipophilic character. Copyright © 2017 China Pharmaceutical University. Published by Elsevier B.V. All rights reserved.

  9. 77 FR 75628 - STS Hydropower, Ltd., Dan River, Inc., and City of Danville, VA; Notice of Application for...

    Science.gov (United States)

    2012-12-21

    ..., Ltd., Dan River, Inc., and City of Danville, VA; Notice of Application for Partial Transfer of License... Bankruptcy Trustee for Dan River, Inc. and STS Hydropower, Ltd (co-licensees) transferors and the City of... Project from Dan River, Inc. and STS Hydropower, Ltd. to STS Hydropower, Ltd. and the City of Danville...

  10. Box-Behnken design for optimum extraction of biogenetic chemicals from P. lanceolata with an energy audit (thermal × microwave × acoustic): a case study of HPTLC determination with additional specificity using on-line/off-line coupling with DAD/NIR/ESI-MS.

    Science.gov (United States)

    Srivastava, Pooja; Ajayakumar, P V; Shanker, Karuna

    2014-01-01

    The genus Pluchea comprises about 80 species distributed worldwide, out of them, only Pluchea lanceolata (DC.) Oliv. & Hiern, is used extensively in the traditional system of India. No chromatographic method is available for its quality. To perform the energy audit for the extraction of biogenetic pentacyclic triterpene, its acetate and sterol from P. lanceolata utilising organic and four alternative solvents. Additionally to resolve the uncertainty of TLC determination, on-line/off-line coupling with a diode-array detector (DAD), and near-infrared (NIR) and electrospray ionisation (ESI) MS was introduced. The extraction of taraxasterol (Tx), taraxasterol acetate (TxAc) and stigmasterol (St) from P. lanceolata was performed using three energy modes. The effects of different operating parameters were studied for optimum extraction yield using the design of experiments, that is, the central composite design and Box-Behnken design. In addition to the retention factor (Rf ) and visible spectral matching, two additional optical spectroscopic techniques, that is, NIR and ESI-MS, were applied for extended specificity. The method was developed for Tx, TxAc and St determination using HPTLC at 645 nm. The optimum extraction yield of targeted compounds was found to be higher with organic solvents than eco-friendly surfactants. The pulse ultrasonic assisted extraction (PUAE) has resulted in optimum extraction of compounds comparable to hot extraction. Both NIR and ESI-MS provided extended specificity in determination. The 5/1-PUAE was determined to be effective, reproducible, simple and energy efficient for the determination of Tx, TxAc and St in P. lanceolata. The offline coupling of NIR and ESI-MS with HPTLC led to considerable improvement in specificity. Copyright © 2014 John Wiley & Sons, Ltd.

  11. Studies on the metabolism of five model drugs by fungi colonizing cadavers using LC-ESI-MS/MS and GC-MS analysis.

    Science.gov (United States)

    Martínez-Ramírez, Jorge A; Voigt, Kerstin; Peters, Frank T

    2012-09-01

    It is well-known that cadavers may be colonized by microorganisms, but there is limited information if or to what extent these microbes are capable of metabolizing drugs or poisons, changing the concentrations and metabolic pattern of such compounds in postmortem samples. The aim of the present study was to develop a fungal biotransformation system as an in vitro model to investigate potential postmortem metabolism by fungi. Five model drugs (amitriptyline, metoprolol, mirtazapine, promethazine, and zolpidem) were each incubated with five model fungi known to colonize cadavers (Absidia repens, Aspergillus repens, Aspergillus terreus, Gliocladium viride, and Mortierella polycephala) and with Cunninghamella elegans (positive control). Incubations were performed in Sabouraud medium at 25 °C for 5 days. After centrifugation, a part of the supernatants was analyzed by liquid chromatography-tandem mass spectrometry with product ion scanning. Another part was analyzed by full scan gas chromatography-mass spectrometry after extraction and derivatization. All model drugs were metabolized by the control fungus resulting in two (metoprolol) to ten (amitriptyline) metabolites. Of the model fungi, only Abs. repens and M. polycephala metabolized the model drugs: amitriptyline was metabolized to six and five, metoprolol to two and two, mirtazapine to five and three, promethazine to six and nine, and zolpidem to three and four metabolites, respectively. The main metabolic reactions were demethylation, oxidation, and hydroxylation. The presented in vitro model is applicable to studying drug metabolism by fungi colonizing cadavers.

  12. Development of a new analytical tool for assessing the mutagen 2-methyl-1,4-dinitro-pyrrole in meat products by LC-ESI-MS/MS.

    Science.gov (United States)

    Molognoni, Luciano; Daguer, Heitor; de Sá Ploêncio, Leandro Antunes; Yotsuyanagi, Suzana Eri; da Silva Correa Lemos, Ana Lucia; Joussef, Antonio Carlos; De Dea Lindner, Juliano

    2018-08-01

    The use of sorbate and nitrite in meat processing may lead to the formation of 2-methyl-1,4-dinitro-pyrrole (DNMP), a mutagenic compound. This work was aimed at developing and validating an analytical method for the quantitation of DNMP by liquid chromatography-tandem mass spectrometry. Full validation was performed in accordance to Commission Decision 2002/657/EC and method applicability was checked in several samples of meat products. A simple procedure, with low temperature partitioning solid-liquid extraction, was developed. The nitrosation during the extraction was monitored by the N-nitroso-DL-pipecolic acid content. Chromatographic separation was achieved in 8 min with di-isopropyl-3-aminopropyl silane bound to hydroxylated silica as stationary phase. Samples of bacon and cooked sausage yielded the highest concentrations of DNMP (68 ± 3 and 50 ± 3 μg kg -1 , respectively). The developed method proved to be a reliable, selective, and sensitive tool for DNMP measurements in meat products. Copyright © 2018 Elsevier B.V. All rights reserved.

  13. Rapid Screening of Carboxylic Acids from Waste and Surface Waters by ESI-MS/MS Using Barium Ion Chemistry and On-Line Membrane Sampling

    Science.gov (United States)

    Duncan, Kyle D.; Volmer, Dietrich A.; Gill, Chris G.; Krogh, Erik T.

    2016-03-01

    Negative ion tandem mass spectrometric analysis of aliphatic carboxylic acids often yields only non-diagnostic ([M - H]-) ions with limited selective fragmentation. However, carboxylates cationized with Ba2+ have demonstrated efficient dissociation in positive ion mode, providing structurally diagnostic product ions. We report the application of barium adducts followed by collision induced dissociation (CID), to improve selectivity for rapid screening of carboxylic acids in complex aqueous samples. The quantitative MS/MS method presented utilizes common product ions of [M - H + Ba]+ precursor ions. The mechanism of product ion formation is investigated using isotopically labeled standards and a series of structurally related carboxylic acids. The results suggest that hydrogen atoms in the β and γ positions yield common product ions ([BaH]+ and [BaOH]+). Furthermore, the diagnostic product ion at m/z 196 serves as a qualifying ion for carboxylate species. This methodology has been successfully used in conjunction with condensed phase membrane introduction mass spectrometry (CP-MIMS), with barium acetate added directly to the methanol acceptor phase. The combination enables rapid screening of carboxylic acids directly from acidified water samples (wastewater effluent, spiked natural waters) using a capillary hollow fiber PDMS membrane immersion probe. We have applied this technique for the direct analysis of complex naphthenic acid mixtures spiked into natural surface waters using CP-MIMS. Selectivity at the ionization and tandem mass spectrometry level eliminate isobaric interferences from hydroxylated species present within the samples, which have been observed in negative electrospray ionization.

  14. Rapid Screening of Carboxylic Acids from Waste and Surface Waters by ESI-MS/MS Using Barium Ion Chemistry and On-Line Membrane Sampling.

    Science.gov (United States)

    Duncan, Kyle D; Volmer, Dietrich A; Gill, Chris G; Krogh, Erik T

    2016-03-01

    Negative ion tandem mass spectrometric analysis of aliphatic carboxylic acids often yields only non-diagnostic ([M - H](-)) ions with limited selective fragmentation. However, carboxylates cationized with Ba(2+) have demonstrated efficient dissociation in positive ion mode, providing structurally diagnostic product ions. We report the application of barium adducts followed by collision induced dissociation (CID), to improve selectivity for rapid screening of carboxylic acids in complex aqueous samples. The quantitative MS/MS method presented utilizes common product ions of [M - H + Ba](+) precursor ions. The mechanism of product ion formation is investigated using isotopically labeled standards and a series of structurally related carboxylic acids. The results suggest that hydrogen atoms in the β and γ positions yield common product ions ([BaH](+) and [BaOH](+)). Furthermore, the diagnostic product ion at m/z 196 serves as a qualifying ion for carboxylate species. This methodology has been successfully used in conjunction with condensed phase membrane introduction mass spectrometry (CP-MIMS), with barium acetate added directly to the methanol acceptor phase. The combination enables rapid screening of carboxylic acids directly from acidified water samples (wastewater effluent, spiked natural waters) using a capillary hollow fiber PDMS membrane immersion probe. We have applied this technique for the direct analysis of complex naphthenic acid mixtures spiked into natural surface waters using CP-MIMS. Selectivity at the ionization and tandem mass spectrometry level eliminate isobaric interferences from hydroxylated species present within the samples, which have been observed in negative electrospray ionization.

  15. Rapid analysis of bile acids in different biological matrices using LC-ESI-MS/MS for the investigation of bile acid transformation by mammalian gut bacteria.

    Science.gov (United States)

    Wegner, Katrin; Just, Sarah; Gau, Laura; Mueller, Henrike; Gérard, Philippe; Lepage, Patricia; Clavel, Thomas; Rohn, Sascha

    2017-02-01

    Bile acids are important signaling molecules that regulate cholesterol, glucose, and energy homoeostasis and have thus been implicated in the development of metabolic disorders. Their bioavailability is strongly modulated by the gut microbiota, which contributes to generation of complex individual-specific bile acid profiles. Hence, it is important to have accurate methods at hand for precise measurement of these important metabolites. Here, a rapid and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for simultaneous identification and quantitation of primary and secondary bile acids as well as their taurine and glycine conjugates was developed and validated. Applicability of the method was demonstrated for mammalian tissues, biofluids, and cell culture media. The analytical approach mainly consists of a simple and rapid liquid-liquid extraction procedure in presence of deuterium-labeled internal standards. Baseline separation of all isobaric bile acid species was achieved and a linear correlation over a broad concentration range was observed. The method showed acceptable accuracy and precision on intra-day (1.42-11.07 %) and inter-day (2.11-12.71 %) analyses and achieved good recovery rates for representative analytes (83.7-107.1 %). As a proof of concept, the analytical method was applied to mouse tissues and biofluids, but especially to samples from in vitro fermentations with gut bacteria of the family Coriobacteriaceae. The developed method revealed that the species Eggerthella lenta and Collinsella aerofaciens possess bile salt hydrolase activity, and for the first time that the species Enterorhabdus mucosicola is able to deconjugate and dehydrogenate primary bile acids in vitro.

  16. Zirconium silicate assisted removal of residual proteins after organic solvent deproteinization of human plasma, enhancing the stability of the LC–ESI-MS response for the bioanalysis of small molecules

    Energy Technology Data Exchange (ETDEWEB)

    Hussain, Shah; Pezzei, Cornelia [Institute of Analytical Chemistry and Radiochemistry, CCB-Center for Chemistry and Biomedicine, Leopold-Franzens University, Innrain 80/82, 6020 Innsbruck (Austria); Güzel, Yüksel [Institute of Analytical Chemistry and Radiochemistry, CCB-Center for Chemistry and Biomedicine, Leopold-Franzens University, Innrain 80/82, 6020 Innsbruck (Austria); ADSI-Austrian Drug Screening Institute, Innrain 66a, 6020 Innsbruck (Austria); Rainer, Matthias [Institute of Analytical Chemistry and Radiochemistry, CCB-Center for Chemistry and Biomedicine, Leopold-Franzens University, Innrain 80/82, 6020 Innsbruck (Austria); Huck, Christian W., E-mail: Christian.W.Huck@uibk.ac.at [Institute of Analytical Chemistry and Radiochemistry, CCB-Center for Chemistry and Biomedicine, Leopold-Franzens University, Innrain 80/82, 6020 Innsbruck (Austria); Bonn, Günther K. [Institute of Analytical Chemistry and Radiochemistry, CCB-Center for Chemistry and Biomedicine, Leopold-Franzens University, Innrain 80/82, 6020 Innsbruck (Austria); ADSI-Austrian Drug Screening Institute, Innrain 66a, 6020 Innsbruck (Austria)

    2014-12-10

    Highlights: • A novel sample preparation technique for isolation of small molecules from human plasma. • Effectiveness of zirconium silicate for the removal of residual proteins after protein precipitation. • Abolishing the consumption of salts for the depletion of residual proteins after protein precipitation. • More than 99.6% removal of plasma proteins. - Abstract: An efficient blood plasma clean-up method was developed, where methanol protein precipitation was applied, followed by zirconium silicate assisted exclusion of residual proteins. A strong binding of zirconium (IV) silicate to the proteins enabled the elimination of remaining proteins after solvent deproteinization through a rapid solid-phase extraction (SPE) procedure. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI/TOF MS) was used for monitoring the proteins during clean-up practice applied to human plasma samples. The proteins were quantified by colorimetric detection using the bicinchoninic acid (BCA) assay. The presented analytical strategy resulted in the depletion of >99.6% proteins from human plasma samples. Furthermore, high-performance liquid chromatography hyphenated to diode-array and electrospray ionization mass spectrometric detection (HPLC–DAD/ESI MS) was applied for qualitative and quantitative analysis of the caffeoylquinic acids (CQAs) and their metabolites in human plasma. The procedure demonstrated high recoveries for the standard compounds spiked at different concentrations. Cynarin and chlorogenic acid were recovered in the range of 81–86% and 78–83%, respectively. Caffeic acid was extracted in the excess of 89–92%, while ferulic acid and dihydroxyhydrocinnamic acid showed a recovery of 87–91% and 92–95%, respectively. The method was partially validated in accordance with FDA-Industry Guidelines for Bioanalytical Method Validation (2001). The presented scheme improves the clean-up efficacy of the methanol deproteinization

  17. Liquid Chromatography Electrospray Ionization Tandem Mass Spectrometric (LC/ESI-MS/MS) Study for the Identification and Characterization of In Vivo Metabolites of Cisplatin in Rat Kidney Cancer Tissues: Online Hydrogen/Deuterium (H/D) Exchange Study.

    Science.gov (United States)

    Bandu, Raju; Ahn, Hyun Soo; Lee, Joon Won; Kim, Yong Woo; Choi, Seon Hee; Kim, Hak Jin; Kim, Kwang Pyo

    2015-01-01

    In vivo rat kidney tissue metabolites of an anticancer drug, cisplatin (cis-diamminedichloroplatinum [II]) (CP) which is used for the treatment of testicular, ovarian, bladder, cervical, esophageal, small cell lung, head and neck cancers, have been identified and characterized by using liquid chromatography positive ion electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) in combination with on line hydrogen/deuterium exchange (HDX) experiments. To identify in vivo metabolites, kidney tissues were collected after intravenous administration of CP to adult male Sprague-Dawley rats (n = 3 per group). The tissue samples were homogenized and extracted using newly optimized metabolite extraction procedure which involves liquid extraction with phosphate buffer containing ethyl acetate and protein precipitation with mixed solvents of methanol-water-chloroform followed by solid-phase clean-up procedure on Oasis HLB 3cc cartridges and then subjected to LC/ESI-HRMS analysis. A total of thirty one unknown in vivo metabolites have been identified and the structures of metabolites were elucidated using LC-MS/MS experiments combined with accurate mass measurements. Online HDX experiments have been used to further support the structural characterization of metabolites. The results showed that CP undergoes a series of ligand exchange biotransformation reactions with water and other nucleophiles like thio groups of methionine, cysteine, acetylcysteine, glutathione and thioether. This is the first research approach focused on the structure elucidation of biotransformation products of CP in rats, and the identification of metabolites provides essential information for further pharmacological and clinical studies of CP, and may also be useful to develop various effective new anticancer agents.

  18. Zirconium silicate assisted removal of residual proteins after organic solvent deproteinization of human plasma, enhancing the stability of the LC–ESI-MS response for the bioanalysis of small molecules

    International Nuclear Information System (INIS)

    Hussain, Shah; Pezzei, Cornelia; Güzel, Yüksel; Rainer, Matthias; Huck, Christian W.; Bonn, Günther K.

    2014-01-01

    Highlights: • A novel sample preparation technique for isolation of small molecules from human plasma. • Effectiveness of zirconium silicate for the removal of residual proteins after protein precipitation. • Abolishing the consumption of salts for the depletion of residual proteins after protein precipitation. • More than 99.6% removal of plasma proteins. - Abstract: An efficient blood plasma clean-up method was developed, where methanol protein precipitation was applied, followed by zirconium silicate assisted exclusion of residual proteins. A strong binding of zirconium (IV) silicate to the proteins enabled the elimination of remaining proteins after solvent deproteinization through a rapid solid-phase extraction (SPE) procedure. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI/TOF MS) was used for monitoring the proteins during clean-up practice applied to human plasma samples. The proteins were quantified by colorimetric detection using the bicinchoninic acid (BCA) assay. The presented analytical strategy resulted in the depletion of >99.6% proteins from human plasma samples. Furthermore, high-performance liquid chromatography hyphenated to diode-array and electrospray ionization mass spectrometric detection (HPLC–DAD/ESI MS) was applied for qualitative and quantitative analysis of the caffeoylquinic acids (CQAs) and their metabolites in human plasma. The procedure demonstrated high recoveries for the standard compounds spiked at different concentrations. Cynarin and chlorogenic acid were recovered in the range of 81–86% and 78–83%, respectively. Caffeic acid was extracted in the excess of 89–92%, while ferulic acid and dihydroxyhydrocinnamic acid showed a recovery of 87–91% and 92–95%, respectively. The method was partially validated in accordance with FDA-Industry Guidelines for Bioanalytical Method Validation (2001). The presented scheme improves the clean-up efficacy of the methanol deproteinization

  19. Effects of N source concentration and NH4(+)/NO3(-) ratio on phenylethanoid glycoside pattern in tissue cultures of Plantago lanceolata L.: a metabolomics driven full-factorial experiment with LC-ESI-MS(3.).

    Science.gov (United States)

    Gonda, Sándor; Kiss-Szikszai, Attila; Szűcs, Zsolt; Máthé, Csaba; Vasas, Gábor

    2014-10-01

    Tissue cultures of a medicinal plant, Plantago lanceolata L. were screened for phenylethanoid glycosides (PGs) and other natural products (NPs) with LC-ESI-MS(3). The effects of N source concentration and NH4(+)/NO3(-) ratio were evaluated in a full-factorial (FF) experiment. N concentrations of 10, 20, 40 and 60mM, and NH4(+)/NO3(-) ratios of 0, 0.11, 0.20 and 0.33 (ratio of NH4(+) in total N source) were tested. Several peaks could be identified as PGs, of which, 16 could be putatively identified from the MS/MS/MS spectra. N source concentration and NH4(+)/NO3(-) ratio had significant effects on the metabolome, their effects on individual PGs were different despite these metabolites were of the same biosynthethic class. Chief PGs were plantamajoside and acteoside (verbascoside), their highest concentrations were 3.54±0.83% and 1.30±0.40% of dry weight, on media 10(0.33) and 40(0.33), respectively. NH4(+)/NO3(-) ratio and N source concentration effects were examined on a set of 89 NPs. For most NPs, high increases in abundance were observed compared to Murashige-Skoog medium. Abundances of 42 and 10 NPs were significantly influenced by the N source concentration and the NH4(+)/NO3(-) ratio, respectively. Optimal media for production of different NP clusters were 10(0), 10(0.11) and 40(0.33). Interaction was observed between NH4(+)/NO3(-) ratio and N source concentration for many NPs. It was shown in simulated experiments, that one-factor at a time (OFAT) experimental designs lead to sub-optimal media compositions for production of many NPs, and alternative experimental designs (e.g. FF) should be preferred when optimizing medium N source for optimal yield of NPs. If using OFAT, the N source concentration is to be optimized first, followed by NH4(+)/NO3(-) ratio, as this reduces the likeliness of suboptimal yield results. Copyright © 2014 Elsevier Ltd. All rights reserved.

  20. On-Line 1D and 2D PLOT/LC-ESI-MS Using 10 μm i.d. Poly(styrene–divinylbenzene) Porous Layer Open Tubular (PLOT) Columns For Ultrasensitive Proteomic Analysis

    Science.gov (United States)

    Luo, Quanzhou; Yue, Guihua; Valaskovic, Gary A; Gu, Ye; Wu, Shiaw-Lin; Karger, Barry L.

    2008-01-01

    Following on our recent work, on-line one dimensional (1D) and two dimensional (2D) PLOT/LC-ESI-MS platforms using 3.2 m × 10 μm i.d. poly(styrenedivinylbenzene) (PS-DVB) porous layer open tubular (PLOT) columns have been developed to provide robust, high performance and ultrasensitive proteomic analysis. Using a PicoClear tee, the dead volume connection between a 50 μm i.d. PS-DVB monolithic microSPE column and the PLOT column was minimized. The microSPE/PLOT column assembly provided a separation performance similar to that obtained with direct injection onto the PLOT column at a mobile phase flow rate of 20 nL/min. The trace analysis potential of the platform was evaluated using an in-gel tryptic digest sample of a gel fraction (15 to 40 kDa) of a cervical cancer (SiHa) cell line. As an example of the sensitivity of the system, ∼2.5 ng of protein in 2 μL solution, an amount corresponding to 20 SiHa cells, was subjected to on-line microSPE-PLOT/LC-ESIMS/MS analysis using a linear ion trap MS. 237 peptides associated with 163 unique proteins were identified from a single analysis when using stringent criteria associated with a false positive rate less than 1% . The number of identified peptides and proteins increased to 638 and 343, respectively, as the injection amount was raised to ∼45 ng of protein, an amount corresponding to 350 SiHa cells. In comparison, only 338 peptides and 231 unique proteins were identified (false positive rate again less than 1%) from 750 ng of protein from the identical gel fraction, an amount corresponding to 6000 SiHa cells, using a typical 15 cm × 75 μm i.d. packed capillary column. The greater sensitivity, higher recovery, and higher resolving power of the PLOT column resulted in the increased number of identifications from only ∼5% of the injected sample amount. The resolving power of the microSPE/PLOT assembly was further extended by 2D chromatography via combination of the high-efficiency reversed phase PLOT column

  1. MOBILE APPLICATION SISTEM MONITORING KONDISI PASIEN SERANGAN JANTUNG BERBASIS GOOGLE MAPS DAN ANDROID

    Directory of Open Access Journals (Sweden)

    Musfirah Putri Lukman

    2017-09-01

    Full Text Available Many people with heart disease who do not detect recurrent heart attacks because they do not feel chest pain, shortness of breath and cold sweat. Recorded 45% of cases in the journal Circulation America Heart Association published heart attacks that did not start with symptoms to make deaths due to heart triples. Therefore, continuous monitoring of vital signs of the body such as heart rate, breathing frequency and body temperature, especially for fast, slow and unnecessary activity functions need to reduce the risk of paralysis, coma, and even death. The method used in mobile applications based on Google Maps and android uses a waterfall model. This application is designed with the purpose of protecting patients, especially with elderly risk factors from sudden death at the location of recurrent heart attacks by identifying the functional abnormalities of the body's vital activity in real-time that alarm the family against the alarm signals that occur in patients. A monitoring system using a microcontroller and sensors mounted on the patient will send the location of a recurrent attack of the patient with the help of google maps technology and the value of the body's vital tool will be displayed on the smartphone screen without limitation of location, distance, and time. Applications built with java programming language, and using web service and MySQL for database. The results of this study the application has been able to display the parameter values measured by the right and can display the location of the occurrence of recurrent attacks of the heart. Techno-biomedical devices with GPS technology can also provide a quick response to the initial rescue handling of patients who suddenly experience recurrent attacks by sending alarm alerts as alarms in the form of phone calls. Keywords: Application, Monitoring, Heart, breath and temperature Banyak penderita penyakit jantung yang tidak mendeteksi terjadinya serangan jantung berulang sebab tidak

  2. PERBEDAAN TOPICAL FLUORIDE APPLICATION DAN FISSURE SEALANT DALAM MENCEGAH KARIES PADAGIGI MOLAR SATU

    Directory of Open Access Journals (Sweden)

    Pawarti Pawarti

    2017-07-01

    Full Text Available Abstract: Topical Fluoride Application And Fissure Sealant To Prevent Dental Caries Permanent First Molars. Anatomy pits and fissures of teeth are caries initiation vulnerable areas of the permanent molars that grow at the age of 6 years where children can not perform oral hygiene. Caries prevention can be done by closing the pits and fissures or application of fluoride (topical fluoride application on the surface of the teeth. The purpose of this study was to analyze the difference fissure sealants and topical application of fluoride to prevent dental caries of first permanent molars. This study was a quasi-experimental study with time series, a sample was taken by purposive 117-second grade students of SDN District of North Pontianak. Data were analyzed using t-test. The result showed that fissure sealant more effective in caries prevention of first permanent molar than topical fluoride application where there were none caries teeth after and month fissure sealant, 25% sealant partially off and 11% fully off. Teeth that have done fluoride after 6 months of 3.9% of dental caries, the eighth month of 5.4% of dental caries. There was a significant difference between the effectiveness of fissure sealants with topical application of fluoride to prevent dental caries in first permanent molars p-value < 0.05, after 6-month p-value: 0.004 and after 8-month p-value: 0.001. Abstrak: Topical Fluoride Application Dan Fissure Sealant Untuk Mencegah Karies Pada Gigi Molar Satu Permanen. Anatomi pit dan fisura gigi merupakan daerah rentan inisiasi karies gigi molar satu permanen yang tumbuh pada usia 6 tahun anak belum bisa melakukan kebersihan mulutnya. Pencegahan karies dapat dilakukan dengan cara menutup pit dan fissure atau pengolesan fluor (topical fluoride application pada permukaan gigi. Tujuan penelitian ini untuk menganalisis perbedaan efektivitas fissure sealant dan topical fluoride application untuk mencegah karies gigi molar satu permanen anak

  3. Peningkatan Efisiensi dan Efektifitas Layanan Dosen dalam Pemanfaatan Web Application

    Directory of Open Access Journals (Sweden)

    Reina Reina

    2013-06-01

    Full Text Available This study aims to determine the benefits of a web application in improving the efficiency and effectiveness of services to lecturers. The research method consists of literature study and data collection analysis based on observations. Implementing a web application, an observation is conducted followed by a comparison on data prior to the implementation. The evaluation results show that the implementation of a web application improves efficiency and effectiveness in the use of time and resources in providing services to lecturers in information access.

  4. Uso da técnica de espectrometria de massas com ionização por eletrospray (ESI-MS) para o estudo do mecanismo de reações orgânicas e avaliação do perfil de fragmentação de bis-hidroxiiminas aromáticas

    OpenAIRE

    Maria Elisa Romanelli Diniz

    2011-01-01

    A Espectrometria de Massas com Ionização por Eletrospray (ESI-MS) foi utilizada na investigação dos mecanismos de duas reações orgânicas: Reação de Zincke e Reação de Aza Diels Alder. Um estudo sistemático sobre a fragmentação das formas protonadas de alguns ligantes do tipo Salofen (bis-hidroxiiminas aromáticas) foi conduzido também neste trabalho. No monitoramento da reação de Zincke foram observados, além dos produtos tradicionais, intermediários inéditos, cujas estruturas foram propostas ...

  5. Applications of implicit restarting in optimization and control Dan Sorensen

    Energy Technology Data Exchange (ETDEWEB)

    Sorensen, D. [Rice Univ., Houston, TX (United States)

    1996-12-31

    Implicit restarting is a technique for combining the implicitly shifted QR mechanism with a k-step Arnoldi or Lanczos factorization to obtain a truncated form of the implicitly shifted QR-iteration suitable for large scale eigenvalue problems. The software package ARPACK based upon this technique has been successfully used to solve large scale symmetric and nonsymmetric (generalized) eigenvalue problems arising from a variety of applications.

  6. Analysis of phenolic compounds in different parts of pomegranate (Punica granatum) fruit by HPLC-PDA-ESI/MS and evaluation of their antioxidant activity: application to different Italian varieties.

    Science.gov (United States)

    Russo, Marina; Fanali, Chiara; Tripodo, Giusy; Dugo, Paola; Muleo, Rosario; Dugo, Laura; De Gara, Laura; Mondello, Luigi

    2018-06-01

    The analysis of pomegranate phenolic compounds belonging to different classes in different fruit parts was performed by high-performance liquid chromatography coupled with photodiode array and mass spectrometry detection. Two different separation methods were optimized for the analysis of anthocyanins and hydrolyzable tannins along with phenolic acids and flavonoids. Two C 18 columns, core-shell and fully porous particle stationary phases, were used. The parameters for separation of phenolic compounds were optimized considering chromatographic resolution and analysis time. Thirty-five phenolic compounds were found, and 28 of them were tentatively identified as belonging to four different phenolic compound classes; namely, anthocyanins, phenolic acids, hydrolyzable tannins, and flavonoids. Quantitative analysis was performed with a mixture of nine phenolic compounds belonging to phenolic compound classes representative of pomegranate. The method was then fully validated in terms of retention time precision, expressed as the relative standard deviation, limit of detection, limit of quantification, and linearity range. Phenolic compounds were analyzed directly in pomegranate juice, and after solvent extraction with a mixture of water and methanol with a small percentage of acid in peel and pulp samples. The accuracy of the extraction method was also assessed, and satisfactory values were obtained. Finally, the method was used to study identified analytes in pomegranate juice, peel, and pulp of six different Italian varieties and one international variety. Differences in phenolic compound profiles among the different pomegranate parts were observed. Pomegranate peel samples showed a high concentration of phenolic compounds, ellagitannins being the most abundant ones, with respect to pulp and juice samples for each variety. With the same samples, total phenols and antioxidant activity were evaluated through colorimetric assays, and the results were correlated among them.

  7. Development and validation of a highly sensitive LC-ESI-MS/MS method for estimation of IIIM-MCD-211, a novel nitrofuranyl methyl piperazine derivative with potential activity against tuberculosis: Application to drug development.

    Science.gov (United States)

    Magotra, Asmita; Sharma, Anjna; Gupta, Ajai Prakash; Wazir, Priya; Sharma, Shweta; Singh, Parvinder Pal; Tikoo, Manoj Kumar; Vishwakarma, Ram A; Singh, Gurdarshan; Nandi, Utpal

    2017-08-15

    In the present study, a simple, sensitive, specific and rapid liquid chromatography (LC) tandem mass spectrometry (MS/MS) method was developed and validated according to the Food and Drug Administration (FDA) guidelines for estimation of IIIM-MCD-211 (a potent oral candidate with promising action against tuberculosis) in mice plasma using carbamazepine as internal standard (IS). Bioanalytical method consisted of one step protein precipitation for sample preparation followed by quantitation in LC-MS/MS using positive electrospray ionization technique (ESI) operating in multiple reaction monitoring (MRM) mode. Elution was achieved in gradient mode on High Resolution Chromolith RP-18e column with mobile phase comprised of acetonitrile and 0.1% (v/v) formic acid in water at the flow rate of 0.4mL/min. Precursor to product ion transitions (m/z 344.5/218.4 and m/z 237.3/194.2) were used to measure analyte and IS, respectively. All validation parameters were well within the limit of acceptance criteria. The method was successfully applied to assess the pharmacokinetics of the candidate in mice following oral (10mg/kg) and intravenous (IV; 2.5mg/kg) administration. It was also effectively used to quantitate metabolic stability of the compound in mouse liver microsomes (MLM) and human liver microsomes (HLM) followed by its in-vitro-in-vivo extrapolation. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Identification of some chemical constituents of Indigofera hirsuta Linn. (Fabaceae) by HPLC-ESI-MS (TOF) and evaluation of the anti radical activity; Identificacao de alguns constituintes quimicos de Indigofera hirsuta Linn. (Fabaceae) por de alguns constituintes quimicos de Indigofera hirsuta Linn. (Fabaceae) por CLAE-IES-EM (TOF) e avaliacao da atividade antirradicalar

    Energy Technology Data Exchange (ETDEWEB)

    Moura, Adriana Candido da Silva; Vilegas, Wagner; Santos, Lourdes Campaner dos [Universidade Estadual Paulista (UNESP), Araraquara, SP (Brazil). Inst. de Quimica.Dept. de Quimica Organica

    2011-07-01

    A rapid analytical approach, suitable to characterize the compounds present in the aqueous and methanol extracts prepared from the aerial parts of Indigofera hirsute, was developed. The method based on high-performance liquid chromatography coupled to mass spectrometry, electrospray positive ionization and detection by time of flight (HPLC-ESI-MS-TOF) identified, tryptophan, uracil, rutin, kempferol-3-O{beta}{sub -}-D-glucopyranoside, gallic acid and methyl gallate. The antiradical activity of this extract was evaluated using DPPH assay, with gallic acid as antiradical pattern. The study revealed the antiradical activity of methyl galatte (EC{sub 50} = 5 {+-} 0.3 {mu}g mL{sup -1}) gallic acid (EC{sub 50} = 5 {+-} 0.2 {mu}g mL{sup -1}) and rutin (EC{sub 50} = 21.6 {+-} 0.6 {mu}g m L{sup -1}), isolated from methanol extract (EC{sub 50} = 67.7 {+-} 0.9 {mu}g mL{sup -1}), which showed strong antiradical activity. (author)

  9. Optimization of the Extraction of Anthocyanins from the Fruit Skin of Rhodomyrtus tomentosa (Ait. Hassk and Identification of Anthocyanins in the Extract Using High-Performance Liquid Chromatography-Electrospray Ionization-Mass Spectrometry (HPLC-ESI-MS

    Directory of Open Access Journals (Sweden)

    Yuan-Ming Sun

    2012-05-01

    Full Text Available Anthocyanins are naturally occurring polyphenols that impart bright color to fruits, vegetables and plants. In this study, the extraction of anthocyanins from freeze-dried fruit skin of downy rose-myrtle (Rhodomyrtus tomentosa (Ait. Hassk var. Gangren was optimized using response surface methodology (RSM. Using 60% ethanol containing 0.1% (v/v hydrochloric acid as extraction solvent, the optimal conditions for maximum yields of anthocyanin (4.358 ± 0.045 mg/g were 15.7:1 (v/w liquid to solid ratio, 64.38 °C with a 116.88 min extraction time. The results showed good fits with the proposed model for the anthocyanin extraction (R2 = 0.9944. Furthermore, the results of high-performance liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS analysis of the anthocyanins extracted from the fruit skin of downy rose-myrtle revealed the presence of five anthocyanin components, which were tentatively identified as delphinidin-3-glucoside, cyanidin-3-glucoside, peonidin-3-glucoside, petunidin-3-glucoside and malvidin-3-glucoside.

  10. Application of liquid chromatography-electrospray ionization mass spectrometry for study of steroid-converting enzymes.

    Science.gov (United States)

    Miksík, Ivan; Mikulíková, Katerina; Pácha, Jirí; Kucka, Marek; Deyl, Zdenek

    2004-02-05

    A high-performance liquid chromatography-atmospheric pressure ionization-electrospray ionization mass spectrometry (HPLC-API-ESI-MS) method was developed for the analysis of steroids in a study of steroid-converting enzymes. Separations ware done on a Zorbax Eclipse XDB-C18 column (eluted with a linear methanol-water-acetic acid gradient) and identification of the steroids involved was done by API-ESI-MS using positive ion mode and extracted ion analysis. The applicability of the present method for studying steroid metabolism was proven in assaying two steroid-converting enzymes (20beta-hydroxysteroid dehydrogenase and 11beta-hydroxysteroid dehydrogenase) in various biological samples (rat and chicken intestine, chicken oviduct).

  11. Détermination des radionucléides dans le repas. Application aux ...

    African Journals Online (AJOL)

    40 sont des radionucléides naturels présents dans les riz, les tubercules, les bouillons et les friandises. Dans les quatre échantillons des repas du Riz analysés, les activités spécifiques en potassium-40 sont différentes. Cette différence est ...

  12. Enantioselective extraction of (+)-(S)-citalopram and its main metabolites using a tailor-made stir bar chiral imprinted polymer for their LC-ESI-MS/MS quantitation in urine samples.

    Science.gov (United States)

    Unceta, Nora; Gómez-Caballero, Alberto; García, Deiene; Díaz, Goretti; Guerreiro, Antonio; Piletsky, Sergey; Goicolea, M Aránzazu; Barrio, Ramón J

    2013-11-15

    This paper reports the application of a chiral imprinted polymer (CIP)-coated stir bar for the selective extraction of (+)-(S)-citalopram (SCIT) and its main metabolites, (+)-(S)-desmethylcitalopram (SDCIT) and (+)-(S)-didesmethylcitalopram (SDDCIT), from urine samples. The developed device has been demonstrated to be capable of selectively extracting the three target analytes from urine samples without saturating the imprinted sites. A CIP-coated stir bar sorptive extraction procedure (CIP-SBSE) is proposed for the isolation of SCIT, SDCIT and SDDCIT followed by their subsequent analysis using liquid chromatography ion trap mass spectrometry (LC-ITMS). Deuterated SCIT-d6 was used as an internal standard. The method was validated using a standard procedure, which revealed that a quantification of 5 ng mL(-1) was obtained in urine samples and that the accuracy and precision were within the established values while no matrix effect was observed. Copyright © 2013 Elsevier B.V. All rights reserved.

  13. Rock-Eval 6 Applications in Hydrocarbon Exploration, Production, and Soil Contamination Studies Les applications de Rock-Eval 6 dans l'exploration et la production des hydrocarbures, et dans les études de contamination des sols

    Directory of Open Access Journals (Sweden)

    Lafargue E.

    2006-12-01

    Full Text Available Successful petroleum exploration relies on detailed analysis of the petroleum system in a given area. Identification of potential source rocks, their maturity and kinetic parameters, and their regional distribution are best accomplished by rapid screening of rock samples (cores and/or cuttings using the Rock-Eval apparatus. The technique has been routinely used for about fifteen years and has become a standard tool for hydrocarbon exploration. This paper describes how the new functions of the latest version of Rock-Eval (Rock-Eval 6 have expanded applications of the method in petroleum geoscience. Examples of new applications are illustrated for source rock characterization, reservoir geochemistry, and environmental studies, including quantification. Le succès d'une exploration pétrolière repose sur l'analyse détaillée du système pétrolier dans une zone donnée. L'identification des roches mères potentielles, la détermination de leur maturité, de leurs paramètres cinétiques et de leur répartition sont réalisées au mieux à partir d'examens rapides d'échantillons de roches (carottes ou déblais au moyen de la pyrolyse Rock-Eval. Cette technique a été utilisée en routine pendant une quinzaine d'années et elle est devenue un outil standard pour l'exploration des hydrocarbures. Cet article décrit comment les nouvelles fonctionnalités de la dernière version de l'appareil Rock-Eval (Rock-Eval 6 ont permis une expansion des applications de la méthode en géosciences pétrolières. Des exemples d'applications nouvelles sont illustrés dans les domaines de la caractérisation des roches mères, de la géochimie de réservoir et des études environnementales incluant la quantification et la description des hydrocarbures dans des sols contaminés.

  14. Spectrophotometric titrations: Application to the determination of some elements in uranium solutions; Les titrages spectrophotometriques: Application a la determination de quelques elements dans les solutions d'uranium

    Energy Technology Data Exchange (ETDEWEB)

    L' Her, M [Commissariat a l' Energie Atomique, Fontenay-aux-Roses (France). Centre d' Etudes Nucleaires

    1967-01-01

    The aim of this work is the application of spectrophotometric titrations to the analysis of uranium-containing solutions. We have been led to examine the general principles involved in these titrations, and we give a brief outline of these principles. In the first part we deal therefore with spectrophotometric titrations from a general point of view, examining their fundamental principle, their practical execution as well as the various possibilities of the method. The advantage of the titration are examined, in particular that of lending itself simultaneous determination of two species. The possibility of applying these spectrophotometric titrations to the analysis of uranium-containing solutions is the subject of the second part of this report: the dosage of a few species in uranium (VI) solutions is described. To this second part is added an experimental appendix consisting of a description of the apparatus, as well as of the operational techniques used for certain titrations, in particular those involving solutions containing uranium. (author) [French] Le but de ce travail est l'application des titrages spectrophotometriques a l'analyse des solutions uraniferes. Nous avons ete amenes a examiner les principes generaux de ces titrages, principes qu'il nous est apparu necessaire de rappeler. Dans une premiere partie nous traiterons donc d'une facon generale des titrages spectrophotometriques, en examinant leur principe fondamental, leur mise en oeuvre ainsi que les possibilites diverses de dosage. Nous examinerons aussi les avantages de la methode de titrage, en insistant notamment sur la possibilite de faire des dosages successifs. La possibilite d'application de ces titrages spectrophotometriques a l'analyse des solutions uraniferes sera le sujet de la deuxieme partie: nous y decrivons le dosage de quelques especes, dans les solutions d'uranium (VI). A cette deuxieme partie nous joindrons une annexe experimentale comportant une description de l'appareillage que

  15. Pengaruh Pemberian Margarin terhadap Sifat Fisiko Kimiawi dan Sensoris Sosis Ayam Petelur Afkir (The Effect of Margarine Application on Physicochemical and Sensory Properties of Culled Hens Layer Sausages

    Directory of Open Access Journals (Sweden)

    Hendronoto Arnoldus Walewengko Lengkey

    2016-12-01

    Full Text Available Research was aimed to determine the effect of margarine application on the physicochemical and sensory properties of culled layer hens sausages. In addition to utilizing the culled layer hens meat as a source of animal protein, as well as to diversify food, so that the resulting product can be accepted by consumers. This study was conducted in a completely randomized experimental design with four treatments unidirectional pattern with margarine giving addition 0.0 %; 2.5 %; 5.0 % and 7.5 % with four replications. The data obtained were statistically tested by analysis of variance (ANOVA, if there is a noticeable difference, then it continued to Duncan's multiple range test. The analysis showed that the water content, fat content, and pH sausage has significant effect, but the protein content was not significantly between the sausages were not given margarine (P-1 and the sausages are given margarine (P-2, P-3 and P-4. The sausage produced will increase the protein content, fat content, and pH with increasing percentage of margarine given, otherwise the moisture content will decrease. Based on sensory testing (appearance, color, flavor, texture and total acceptance, culled layer hens sausage can be accepted by consumers. Sausages were given margarine value ranges between 7.0 to 8.4 (just like - really like and were not given margarine has lower value ranging from 5.2 to 6.9 (neutral - just like.   ABSTRAK Penelitian mengenai pengaruh pemberian margarin terhadap sifat fisiko kimiawi dan sensoris sosis ayam petelur afkir adalah untuk mengetahui penambahan margarin terhadap kualitas sosis ayam petelur afkir, selain itu untuk memanfaatkan daging ayam petelur afkir sebagai sumber protein hewani, dan untuk melakukan penganekaragaman pangan, sehingga produk yang dihasilkan dapat diterima oleh konsumen. Penelitian ini dilakukan secara eksperimental dengan rancangan acak lengkap pola searah dengan empat perlakuan pemberian margarin 0,0 %; 2,5 %; 5

  16. Trends in the choice of refrigerants according to the applications; Tendances dans le choix des frigorigenes selon les applications

    Energy Technology Data Exchange (ETDEWEB)

    Billiard, F.

    2002-07-01

    No general rules exist in the choice of refrigerants but five classical criteria: thermo-physical, technological, economical, safety, environmental, some regulations and local standards, and the 'cultural' criteria linked with the professional habits and with the personnel training. The best approach to present the evolutions and trends in this domain consists in reasoning application by application. In this document, 8 applications are analyzed: domestic, commercial, and industrial refrigeration, terrestrial and maritime refrigerating transport, air conditioning and heat pumps, air conditioning with water cooling groups, and mobile air conditioning. For each application, national and worldwide statistical data are given which allow to characterize the economical importance of the sector of application and the trends in the choice of refrigerants (HFC, ammonia, hydrocarbons, CO{sub 2} etc..). Finally, some future trends are briefly evoked. (J.S.)

  17. Application de la gestion intégrale de l'innovation dans les petites et ...

    International Development Research Centre (IDRC) Digital Library (Canada)

    'application d'un cadre de gestion intégrale de l'innovation destiné exclusivement aux PME. Les capacités de recherche et de mise en oeuvre seront améliorées au moyen d'une formation aux cycles supérieurs ou d'une autre nature.

  18. Determinatin dúne application des betons de balles de riz dans le ...

    African Journals Online (AJOL)

    The obtained concretes are light and have compressive strength between 1 and 8 MPa. An application of these concretes is their use for the manufacture of masonry blocks and interjoists entering in the realization of walls and coffer floor. Key words: Rice husks, lightweight concrete, compressive strength, Masonry blocks, ...

  19. Penerapan Aplikasi Program Penjualan Dan Pembelian Menggunakan Model Rapid Application Development

    Directory of Open Access Journals (Sweden)

    Annisa Febriani

    2017-09-01

    Abstract The development of information technology at the moment quickly and rapidly, supported by one means namely computer. Of course the computer has been equipped with a particular application is used to help facilitate the work of the man to manage the data of an organization or company so that getting accurate results and according to needs. The results of the observations that have been made, showed a sales and purchase activities are still using manual systems, one of them at a clothing store. Starting from the data processing of the goods, the difficulty of checking stock, purchase transaction, sales transactions, as well as other data storage associated with all types of such activities, so that it could make a loss for the store owner, errors in the logging and less akuratnya the report is made. Judging from the large number of transactions done on clothing stores, required system information more quickly and accurately. Thus, the author makes the program architecture-based computer, use the Microsoft Visual Basic.net programming language and the MySQL database, so that the information and activities that occur can be done quickly and accurately. The methods used in making architecture the program using the model of Rapid Application Development (RAD. This RAD model is an adaptation of the waterfall model for high speed version of the development of each component of its software. Results achieved from the discussion of this theme is the form of the application program selling and buying the ready-made. In this case, the use of the application program is the best solution to solve the existing problems, as well as with the use of application programs can be reached by an activity which is effective and efficient in supporting that activity, especially for addressing the problem of the sale and purchase of.   Keywords: Sales Program, Purchasing Program.

  20. CanDan 2, phase 2. Final report. [Fuel cell systems for back-up power and materials handling applications]; CanDan 2, fase 2. Slutrapport

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2012-11-01

    CanDan 2 Phase 2 is the second phase of a research and demonstration project for fuel cell backup power systems and fuel cell powered material handling equipment. In the Backup Power segment the fuel cell units have been developed, certified and delivered. A total of 32 fuel cell backup power systems have been delivered for EnergiMidt and in operation since early 2011. Following this project EnergiMidt has purchased another 31 systems in order to make a full transition from battery backup to fuel cell backup in their entire broadband network. In the material handling segment a 10 kW fuel cell system has been fully integrated in the fork lift truck, Dantruck 3000 Power Hydrogen. The result was a much more commercially mature product than expected from the beginning of the project. The result is a finished 2,5T fork lift truck which was presented at the CE-mat fair in April 2011. (LN)

  1. Formation et application des nanoparticules dans les fibres optiques en silice

    OpenAIRE

    Blanc , Wilfried; Dussardier , Bernard

    2016-01-01

    International audience; Optical fibers are the basis for applications that have grown considerably in recent years (telecommunications, sensors, fiber lasers, etc). Despite undeniable successes, it is necessary to develop new generations of amplifying optical fibers that will overcome some limitations typical of silica glass. In this sense, the amplifying Transparent Glass Ceramics (TGC), and particularly the fibers based on this technology, open new perspectives that combine the mechanical a...

  2. CORPORATE IDENTITY SEJARAH DAN APLIKASINYA

    Directory of Open Access Journals (Sweden)

    Christine Suharto Cenadi

    1999-01-01

    Full Text Available In the recent globalization era%2C and the developed market%2C many companies compete to attract consumers to buy their products. One of the keys to compete and survive in this developing market is by creating an image and graphic identity. This paper will discuss about corporate identity%2C image%2C its purpose and applications. Abstract in Bahasa Indonesia : Dalam era globalisasi dewasa ini%2C dan dengan berkembangnya pasar (market%2C banyak perusahaan bersaing untuk menarik perhatian konsumen untuk membeli produknya. Salah satu cara untuk bersaing dan dapat bertahan di dalam pasar yang terus berkembang ini adalah dengan menciptakan suatu image dan identitas graphic. Tulisan ini akan membahas tentang corporate identity%2C image%2C fungsi dan aplikasinya

  3. Aplikasi teori belajar sosial dalam penatalaksanaan rasa takut dan cemasan anak pada perawatan gigi (Application of social learning theory in the management of children dental fear and anxiety

    Directory of Open Access Journals (Sweden)

    Arlette Suzy Setiawan

    2014-06-01

    Full Text Available Background: Dental anxiety is a prevalent problem faced by dentists till nowadays, especially in treating child patients. Several methods in managing anxiety are available, but there is no single method can be applied extensively. Purpose: This article was aimed to describe the application of social learning theory in preventing or reducing dental anxiety in children. Literature review: Anxiety and fear are psych feelings that is experienced by a person. A child developed these feelings by learning from their own past experienced or by information obtained from their environment. If fear and anxiety can be learned by a child, thus the opposite term which is preventing the feelings is assumed can be also offered to learned. This application actually being applied in the field of dentistry as modeling, but the exploration of how this process is due is often being ignored. Conclusion: Social learning theory provides an easy preventive approach and effective intervention that can be applied to children in 4-9 years old to reduce dental anxiety.Latar belakang: Kecemasan pada perawatan gigi merupakan hal yang paling sering dijumpai dan merupakan masalah yang dihadapi oleh dokter gigi sampai saat ini, terutama pada pasien anak. Berbagai metode penatalaksanaan kecemasan banyak tersedia, namun tidak satu pun metode yang dapat diterapkan secara luas. Tujuan: Makalah ini disusun untuk membahas mengenai aplikasi teori belajar sosial dalam mencegah kecemasan pada anak saat perawatan gigi. Tinjauan pustaka: Rasa cemas dan takut merupakan perasaan psikis yang dialami seorang individu. Perasaan ini pada seorang anak lebih banyak didapat dari proses belajar dalam menyerap informasi berdasarkan pengalaman pribadi ataupun informasi dari lingkungan sekitar. Bila rasa cemas dan takut dapat dipelajari oleh seorang anak, maka diasumsikan bahwa menghindari timbulnya perasaan ini dapat pula diajarkan pada anak. Aplikasi hal tersebut sebenarnya telah diterapkan di bidang

  4. ANALYSE RIGOUREUSE D’IRIS METALLIQUES EPAIS ET LEUR APPLICATION DANS LES FILTRES A CAVITES RECTANGULAIRES DIRECTEMENT COUPLEES

    Directory of Open Access Journals (Sweden)

    M BELMEGUENAI

    2000-12-01

    Full Text Available Une technique générale, basée sur l’analyse modale, est utilisée pour la modélisation de discontinuités et de filtres en guides d’ondes rectangulaires. Dans notre étude où l’épaisseur de l’obstacle métallique (iris épais est prise en compte, nous déterminons d’abord la matrice de diffraction de l’iris par utilisation de l’analyse en modes symétriques et asymétriques, puis en considérant le principe d’association de quadripôles en cascade, nous obtenons la réponse du filtre. Nos différents résultats sont comparés avec ceux publiés dans la littérature.

  5. Kekerasan mikro enamel gigi permanen muda setelah aplikasi bahan pemutih gigi dan pasta remineralisasi (Enamel micro hardness of young permanent tooth after bleaching and remineralization paste application

    Directory of Open Access Journals (Sweden)

    Budianto Liwang

    2014-12-01

    Full Text Available Background: Studies showed that bleaching agent had demineralization effect to enamel, and encourage use of remineralization paste after bleaching treatment especially in young permanent tooth which in post-eruptive enamel maturation. Purpose: The study ere aimed to determine the bleaching agent effect on enamel surface micro hardness, and to determine the effect of remineralization paste application on enamel surface micro hardness of young permanent tooth after bleaching treatment. Methods: Fourteen young permanent teeth were placed in a block of resin with a window on the buccal surface enamel. The initial enamel surface hardness was measured using Microvickers Hardness Tester. Then the application of hydrogen peroxide bleaching materials 30% was done three times for 15 minutes and followed by surface hardness of enamel measurement. Samples were divided into 2 groups; the first group was applied paste of Hydroxy apatite + NaF 1450ppm , and the second group was applied paste of CPP–ACP + NaF 900ppm. Each paste was applied for 30 minutes for 7 days, then the enamel surface hardness of samples were measured. Results: The enamel surface micro hardness decreased after bleaching from 333.09 ± 10.49 VHN to 299.15±5.70 VHN. Micro hardness after application of Hidroxy apatite + NaF 1450ppm was 316.61±5.87 VHN and after application of CPP-ACP + NaF 900ppm was 319.94±3.25 VHN, however the micro hardness still lower than initial micro hardness. Conclusion: Tooth bleaching agent caused a decrease of enamel surface micro hardness in young permanent tooth. The use of remineralization paste enabled to increase the enamel surface micro hardness young permanent tooth.Latar belakang: Penelitian-penelitian sebelumnya menunjukkan bahwa produk pemutih gigi memiliki efek demineralisasi enamel gigi, dan mendorong penggunaan pasta remineralisasi setelah pemutihan gigi terutama di gigi muda permanen yang enamelnya masih dalam proses maturasi pasca-erupsi. Tujuan

  6. Probes and their application to the study of H.F. plasmoids; Les sondes et leur application dans l'etude des plasmoides H.F

    Energy Technology Data Exchange (ETDEWEB)

    Brunet, A; Geller, R [Commissariat a l' Energie Atomique, Saclay (France).Centre d' Etudes Nucleaires

    1960-07-01

    In the first part of this paper, we study the single Langmuir probe and the double-probe method. In the second part, we describe the probe-technique in connection with R.F. plasmoids. (author) [French] Dans la premiere partie de cet article, nous rappelons les principes d'utilisation de la sonde simple de Langmuir ainsi que la methode de la sonde double. La seconde partie est consacree a la pratique des sondes dans l'etude des plasmoides H.F. (auteur)

  7. La Loi sur le tabac (décembre 1999 et les paradoxes de son application dans les milieux usiniers

    Directory of Open Access Journals (Sweden)

    Julie Dussault

    2005-05-01

    Full Text Available La Loi sur le tabac (1999 visant à réduire le tabagisme interdit notamment l’usage du tabac au travail. Se pose aujourd’hui l’urgence d’un questionnement sur les répercussions de cette dernière dans les différents milieux de travail.Un examen de la littérature portant sur les restrictions tabagiques au travail indique que les recherches récentes, essentiellement de nature quantitative, visent à mesurer l’efficacité des interdictions et restrictions, ou à identifier les caractéristiques du travail en lien avec le tabagisme. La plus forte prévalence du tabagisme chez les travailleurs d’usines (cols bleus suggère de porter un regard particulier sur cette population.Dans une perspective exploratoire, deux études de cas originales ont été menées (été 2002 dans deux usines syndiquées.Les résultats de la recherche mettent en perspective la perception qu’ont les travailleurs vis-à-vis de la Loi dans les usines. Pour eux, il fait non-sens qu’une Loi visant l’amélioration de la santé soit appliquée dans des milieux considérés laxistes en matière de qualité de l’environnement de travail. La recherche révèle l’importance d’envisager la question de la qualité de l’environnement de travail de manière globale.The Tobacco Act (1999, which is intended to reduce smoking by banning the use of tobacco at work, has emphasized the urgent need to question the Act’s repercussions in various workplaces.A review of the literature on restrictions on the use of tobacco at work shows that recent, primarily quantitative studies are designed to measure the efficiency of bans and restrictions, or to identify work characteristics related to smoking. A greater prevalence of smoking among plant workers (blue collar workers suggests the focus should be on this population.Two original exploratory case studies were conducted (summer 2002 in two unionized plants.The research findings show how plant workers perceive the Act

  8. Application of paper chromatography to the determination of some elements in minerals and rocks; Application de la chromatographie sur papier a la determination de certains elements dans les mineraux et les roches

    Energy Technology Data Exchange (ETDEWEB)

    Agrinier, H [Commissariat a l' Energie Atomique, Fontenay-aux-Roses (France). Centre d' Etudes Nucleaires

    1964-11-01

    This publication describes our work in applying paper chromatography to the fields of mineralogy and geology. We have studied the separation and determination of the following elements: Nb, Ta, Ti, Co, Cu, Mn, Sn, Ge, As, Sb, Bi, U, Th, Be, Au, Pb, Zn, V and Mo. The development of separation methods for these various elements has led us to solve many interference problems. These methods make it possible to separate and measure mineral components. They also enable us to search for trace elements in ores, rocks soils and carbonaceous materials. Finally let us point out that this technique may equally be used for analysis in very radioactive environment. (author) [French] Dans cette etude, nous etendons le champ d'application de la chromatographie sur papier aux domaines de la mineralogie et de la geologie. Nous avons etudie la separation et la determination des elements suivants: Nb, Ta, Ti, Co, Cu, Mn, Sn, Ge, As, Sb, Bi, U, Th, Be, Au, Pb, Zn, V et Mo. La mise au point des methodes de separation concernant ces differents elements nous a amenes a resoudre de nombreux problemes d'interference. Ces methodes permettent la separation et le dosage des constituants des mineraux, ainsi que la recherche d'elements en traces dans les minerais, les roches, les sols et les materiaux carbonnes. Signalons pour terminer que cette technique peut egalement trouver son utilisation dans le domaine de l'analyse en milieu tres radio-actif. (auteur)

  9. Calculation of control rods in rectangular reactor, and applications (1960); Calcul des barres de conteole dans un reacteur rectangulaire et applications (1960)

    Energy Technology Data Exchange (ETDEWEB)

    Goshen, S; Pazy, A [Commissariat a l' Energie Atomique, Saclay (France).Centre d' Etudes Nucleaires

    1960-07-01

    The aim of this report is to find a method for estimating the anti-reactivity of control rods perpendicular to the axis in a cylindrical pile. The paper is divided into two parts. In the first is given a method of calculating control rods in a rectangular pile, similar to the Nordheim-Scalettar method for cylindrical piles. As an example the formulas are given for the theories of one and two neutron groups, the generalisation for several groups being evident. In the second part we find by a variation method a formula for estimating the Laplacian of a pile, which may be divided into parallelepipeds for which the Laplacian are given. Finally, this formula is used to calculate the anti-reactivity of rods perpendicular to the axis in a cylindrical pile. (author) [French] Le but de ce rapport est de trouver une methode pour estimer l'antireactivite des barres de controle perpendiculaires a l'axe dans pile cylindrique. Le rapport se divise en deux parties. Dans la premiere nous donnons une methode de calcul des barres de controle dans une pile rectangulaire, analogue a la methode de Nordheim-Scalettar pour les piles cylindriques. A titre d'exemple, nous donnons les formules de theories a un et deux groupes de neutrons, la generalisation pour plusieurs groupes est evidente. Dans la deuxieme partie, nous trouvons, par une methode de variation, une formule qui permet d'estimer le laplacien d'une pile, qui peut etre divisee en parallelepipedes dont les laplaciens sont donnes. Nous utilisons enfin, cette formule pour calculer l'antireactivite des barres perpendiculaires a l'axe dans une pile cylindrique. (auteur)

  10. Proceedings of the Scientific Meeting on Application of Isotopes and Radiation, Book I, Agricultural, Animal and Biology; Risalah Pertemuan Ilmiah Penelitian Dan Pengembangan Aplikasi Isotop Dan Radiasi. Buku 1, Pertanian, Peternakan dan Biologi

    Energy Technology Data Exchange (ETDEWEB)

    Suhadi, F; Sisworo, E L; Maha, M; Ismachin, M; Hilmy, N; Sumatra, M; Mugiono,; Wandowo,; Soebianto, Y S [Center for Application of Isotopes and Radiation, National Atomic Energy Agency, Serpong (Indonesia)

    1998-07-01

    The aim of the 10{sup t}h Meeting of the Isotope and Radiation Application is to disseminate the result of research on application of nuclear techniques on agriculture, animal, biology, chemistry, environment, radiation process and industry. The meeting was held in Jakarta, 18-19 February 1998, and there were 6 invited papers and 52 papers indexed individually. This proceeding is divided by two volumes. Volume I and volume II consists of agriculture, animal, biology and chemistry, environment, radiation process and industry, respectively.(ID)

  11. Artificial Intelligence in the Petroleum World Une enquête sur les applications de l'Intelligence Artificielle dans le monde pétrolier

    Directory of Open Access Journals (Sweden)

    Braunschweig B. L.

    2006-11-01

    Full Text Available This paper shows the main results of a survey conducted by the Institut Français du Pétrole (IFP on the applications of artificial intelligence (AI in the oil industry. The survey was made in 1989 by interviews with specialists from the petroleum industry and from the academic world. This investigation produced as a result a synthetic document which presents, on an anonymous and statistical basis, the major trends of research and applications involving artificial intelligence in the oil industry. All organizations which agreed to participate in this study are in possession of one copy of this document. This paper will try to highlight the major trends identified by the survey, and show some detailed results. The figures present the interview data base, which consists in 150+ application questionnaires and 30+ questionnaires on organizations. Début 1989, la Direction de Recherches Informatique Mathématiques Appliquées de l'Institut Français du Pétrole entamait une enquête destinée à faire le point sur l'intelligence artificielle (IA dans le monde pétrolier, afin de positionner les recherches effectuées à L'IFP par rapport au reste de la profession et définir de nouvelles orientations. Au cours de l'année 1989, nous avons rencontré lors de visites individuelles ou à l'occasion de congrès, journées spécialisées, une centaine de praticiens appliquant ou souhaitant appliquer les techniques IA dans toutes les facettes du métier pétrolier. Nous avons également fait remplir à ces personnes, la plupart du temps en notre présence, mais dans certains cas par courrier, des questionnaires sur l'état de l'IA au sein de leurs organisations. Le questionnaire pour une organisation se composait d'une part, d'une page sur la place de MA dans l'organisation, le nombre de projets, d'installations, leur nature, les outils mis en oeuvre et les personnes concernées; d'autre part, d'un questionnaire de quatre pages sur chaque application

  12. Prinsip Transparansi dalam Perjanjian TBT dan SPS

    Directory of Open Access Journals (Sweden)

    Dina Widyaputri Kariodimedjo

    2012-02-01

    Full Text Available Transparency principle in the TBT and SPS Agreement is implemented by notification. Its application is prepared by related agencies through the making of regulations, establishment of enquiry points, building capacity and infrastructure. It guarantees certainty, predictability and credibility of Indonesia in international trade, and its application should not undermine national trade policy. Prinsip transparansi dalam Perjanjian TBT dan SPS diterapkan melalui notifikasi. Penerapan prinsip ini dilakukan oleh instansi-instansi terkait melalui pembuatan peraturan, upaya terkait kelembagaan, SDM dan infrastruktur. Prinsip yang bertujuan menciptakan kepastian, konsistensi bagi perdagangan dan kredibilitas Indonesia dalam perdagangan internasional, harus dilakukan tanpa mengorbankan kepentingan untuk mengamankan kebijakan impor nasional.

  13. Meet EPA's Dan Nelson

    Science.gov (United States)

    EPA’s Dan Nelson is the Director of the Human Research Protocol Office at the National Health and Environmental Effect Research Laboratory, Dan works to protect the rights and welfare of EPA’s research participants.

  14. LC-ESI-MS-MS Method for Monitoring Dopamine, Serotonin and Their Metabolites in Brain Tissue

    Czech Academy of Sciences Publication Activity Database

    Najmanová, V.; Rambousek, Lukáš; Syslová, K.; Bubeníková, V.; Šlamberová, R.; Valeš, Karel; Kačer, P.

    2011-01-01

    Roč. 73, Suppl.1 (2011), s. 143-149 ISSN 0009-5893 R&D Projects: GA MZd(CZ) NS10365 Grant - others:GA ČR(CZ) GAP303/10/0580; GA ČR(CZ) GA305/09/0126; GA ČR(CZ) GD203/08/H032 Program:GD Institutional research plan: CEZ:AV0Z50110509 Keywords : dopamine * microdialyses * liquid chromatography * tandem mass spectrometry Subject RIV: FH - Neurology Impact factor: 1.195, year: 2011

  15. High throughput microfabricated CE/ESI-MS: automated sampling from a microwell plate

    Czech Academy of Sciences Publication Activity Database

    Zhang, B.; Foret, František; Karger, B. L.

    2001-01-01

    Roč. 73, č. 11 (2001), s. 2675-2681 ISSN 0003-2700 Institutional research plan: CEZ:AV0Z4031919 Keywords : electrospray mass-spectrometry * dead volume * electrophoresis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.532, year: 2001

  16. Identification of atractyloside by LC-ESI-MS in alleged herbal poisoning

    CSIR Research Space (South Africa)

    Steenkamp, PA

    2006-11-01

    Full Text Available , approximately 3000 species are used as medicines, and of these, some 350 species are commonly used and traded medicinal plants [3,11]. One of these more commonly used plants is Callilepis laureola DC. (Asteraceae), also called ??Ox-eye daisy?? or ??Wildemagriet... by hand and drawn through the cartridges at approximately 1 ml/min by applying a mild vacuum. The cartridges were washed with 3 ml extracting buffer and dried under vacuum for 10 min. They were then eluted with 3 ml methanol, 3 ml acidic methanol (10 ml...

  17. Lipidomics analysis of follicular fluid by ESI-MS reveals potential biomarkers for ovarian endometriosis.

    Science.gov (United States)

    Cordeiro, Fernanda Bertuccez; Cataldi, Thais Regiani; Perkel, Kayla Jane; do Vale Teixeira da Costa, Lívia; Rochetti, Raquel Cellin; Stevanato, Juliana; Eberlin, Marcos Nogueira; Zylbersztejn, Daniel Suslik; Cedenho, Agnaldo Pereira; Turco, Edson Guimarães Lo

    2015-12-01

    The aim of the present study was to analyze the lipid profile of follicular fluid from patients with endometriosis and endometrioma who underwent in vitro fertilization treatment (IVF). The control group (n = 10) was composed of women with tubal factor or minimal male factor infertility who had positive pregnancy outcomes after IVF. The endometriosis group consisted of women with endometriosis diagnosed by videolaparoscopy (n = 10), and from the same patients, the endometriomas fluids were collected, which composed the endometrioma group (n = 10). From the follicular fluid and endometriomas, lipids were extracted by the Bligh and Dyer method, and the samples were analyzed by tandem mass spectrometry. We observed phosphatidylglycerol phosphate, phosphatidylcholine, phosphatidylserine, and phosphatidylnositol bisphosphate in the control group. In the endometriosis group, sphingolipids and phosphatidylcholines were more abundant, while in the endometrioma group, sphingolipids and phosphatidylcholines with different m/z from the endometriosis group were found in high abundance. This analysis demonstrated that there is a differential representation of these lipids according to their respective groups. In addition, the lipids found are involved in important mechanisms related to endometriosis progress in the ovary. Thus, the metabolomic approach for the study of lipids may be helpful in potential biomarker discovery.

  18. Chemical profile of mango (Mangifera indica L.) using electrospray ionisation mass spectrometry (ESI-MS).

    Science.gov (United States)

    Oliveira, Bruno G; Costa, Helber B; Ventura, José A; Kondratyuk, Tamara P; Barroso, Maria E S; Correia, Radigya M; Pimentel, Elisângela F; Pinto, Fernanda E; Endringer, Denise C; Romão, Wanderson

    2016-08-01

    Mangifera indica L., mango fruit, is consumed as a dietary supplement with purported health benefits; it is widely used in the food industry. Herein, the chemical profile of the Ubá mango at four distinct maturation stages was evaluated during the process of growth and maturity using negative-ion mode electrospray ionisation Fourier transform ion cyclotron resonance mass spectrometry (ESI(-)FT-ICR MS) and physicochemical characterisation analysis (total titratable acidity (TA), total soluble solids (TSS), TSS/TA ratio, and total polyphenolic content). Primary (organic acids and sugars) and secondary metabolites (polyphenolic compounds) were mostly identified in the third maturation stage, thus indicating the best stage for harvesting and consuming the fruit. In addition, the potential cancer chemoprevention of the secondary metabolites (phenolic extracts obtained from mango samples) was evaluated using the induction of quinone reductase activity, concluding that fruit polyphenols have the potential for cancer chemoprevention. Copyright © 2016 Elsevier Ltd. All rights reserved.

  19. Chemotaxonomic Differentiation of Bacteria Using Sugar/Nucleotide Markers Identified by ESI MS-MS

    National Research Council Canada - National Science Library

    Fox, Alvin

    1999-01-01

    .... A scheme for characterization of brucella (following our earlier work with bacilli) was developed. The feasibility of detecting markers for bacteria in environmental samples was demonstrated by developed...

  20. Derivatization of peptides as quaternary ammonium salts for sensitive detection by ESI-MS.

    Science.gov (United States)

    Cydzik, Marzena; Rudowska, Magdalena; Stefanowicz, Piotr; Szewczuk, Zbigniew

    2011-06-01

    A series of model peptides in the form of quaternary ammonium salts at the N-terminus was efficiently prepared by the solid-phase synthesis. Tandem mass spectrometric analysis of the peptide quaternary ammonium derivatives was shown to provide sequence confirmation and enhanced detection. We designed the 2-(1,4-diazabicyclo[2.2.2] octylammonium)acetyl quaternary ammonium group which does not suffer from neutral losses during MS/MS experiments. The presented quaternization of 1,4-diazabicyclo[2.2.2]octane (DABCO) by iodoacetylated peptides is relatively easy and compatible with standard solid-phase peptide synthesis. This methodology offers a novel sensitive approach to analyze peptides and other compounds. Copyright © 2011 European Peptide Society and John Wiley & Sons, Ltd.

  1. Rapid UPLC-ESI-MS/MS method for the analysis of isoflavonoids and other phenylpropanoids

    Czech Academy of Sciences Publication Activity Database

    Prokudina, E. A.; Havlíček, Libor; Al-Maharik, N.; Lapčík, O.; Strnad, Miroslav; Grúz, Jiří

    2012-01-01

    Roč. 26, 1-2 (2012), s. 36-42 ISSN 0889-1575 R&D Projects: GA AV ČR KAN200380801; GA ČR GA525/09/0994 Grant - others:GA MŠk(CZ) ED0007/01/01; GA ČR(CZ) GPP503/12/P166 Program:ED; GP Institutional research plan: CEZ:AV0Z50380511 Keywords : Isoflavonoids * Isoflavones * Flavonoids Subject RIV: EC - Immunology Impact factor: 2.088, year: 2012

  2. Thermal Aging of Anions in Ionic Liquids containing Lithium Salts by IC/ESI-MS

    International Nuclear Information System (INIS)

    Pyschik, Marcelina; Kraft, Vadim; Passerini, Stefano; Winter, Martin; Nowak, Sascha

    2014-01-01

    Highlights: • Thermal aging investigation of TFSI- and FSI- based ionic liquids and their mixtures with Li salts. • PYR 13 FSI shows thermal decomposition when mixed with LiPF 6 and LiClO 4 . • PYR 13 TFSI does not show any decomposition products with the electrolyte salts. • LiPF 6 dissolved in ionic liquids suffers of thermal aging as in conventional Li-ion battery electrolytes. - Abstract: The stability of 1-methyl-1-propylpyrrolidinium bis(trifluoromethanesulfonyl)imide (PYR 13 TFSI) and 1-methyl-1-propylpyrrolidinium bis(fluorosulfonyl)imide (PYR 13 FSI) ionic liquids at elevated temperatures (60 °C) is investigated by ion chromatography. Additionally, the influence of the electrolyte salts, lithium hexafluorophosphate (LiPF 6 ), lithium bis(trifluoromethanesulfonyl)imide (LiTFSI) and lithium perchlorate (LiClO 4 ), on the decomposition of both the ionic liquids was analysed over a long term stability study. It has been found out that TFSI has a much higher thermal stability than FSI. The addition of LiTFSI did not show any effect on the aging of both ionic liquid anions. However, PYR 13 FSI degraded when mixed with the electrolyte salts LiPF 6 and LiClO 4 , while PYR 13 TFSI did not. Finally, LiPF 6 forms the same hydrolysis products in the investigated ionic liquids as in the commonly used electrolytes based on organic solvents in lithium-ion batteries

  3. Analysis of the Main Nucleosides in Cordyceps Sinensis by LC/ESI-MS

    Directory of Open Access Journals (Sweden)

    Yun-Biao He

    2010-01-01

    Full Text Available A sensitive, selective and reliable liquid chromatography-mass spectrometry coupled with electrospray ionization interface method for simultaneous separation and determination of thymine, adenine, adenosine and cordycepin in Cordyceps sinensis has been established. The optimum separation for these analytes was achieved using a gradient elution system and a 2.0 × 150 mm Shimadzu VP-ODS column. 2-Chloroadenosine was used as internal standard for this assay. [M+H]+ions at m/z 127, 136, 268, 252 and 302 were chosen and selective ion monitoring (SIM mode was used for quantitative analysis of the four main nucleosides. The regression equations were linear in the range of 1.0–117.5 μg·mL-1 for thymine, 1.8-127.0 μg·mL-1 for adenine, 0.6-114.0 μg·mL-1 for adenosine and 0.5-107.5 μg·mL-1 for cordycepin. The limits of quantitation (LOQ and detection (LOD were 1.0 and 0.2 μg·mL-1 for thymine, 1.8 and 0.6 μg·mL-1 for adenine, 0.6 and 0.1 μg·mL-1 for adenosine and 0.5 and 0.1 μg·mL-1 for cordycepin, respectively. The recoveries of the four nucleosides ranged from 98.47 to 99.32%. The developed method was successfully used to determine nucleosides in Cordyceps sinensis from different sources.

  4. Characterization of flavonoids in Millettia nitida var. hirsutissima by HPLC/DAD/ESI-MS n

    OpenAIRE

    Ye, Min; Yang, Wen-Zhi; Liu, Ke-Di; Qiao, Xue; Li, Bei-Jia; Cheng, Jun; Feng, Jie; Guo, De-An; Zhao, Yu-Ying

    2011-01-01

    Millettia nitida var. hirsutissima is a Chinese herbal medicine used for the treatment of gynecological diseases. An HPLC/DAD/ESI-MSn method was established for the rapid separation and characterization of bioactive flavonoids in M. nitida var. hirsutissima. A total of 32 flavonoids were detected, of which 14 compounds were unambiguously characterized by comparing their retention time, UV, and MS spectra with those of the reference standards, and the others were tentatively identified based o...

  5. Sensitive quantification of apomorphine in human plasma using a LC-ESI-MS-MS method.

    Science.gov (United States)

    Abe, Emuri; Alvarez, Jean-Claude

    2006-06-01

    An analytical method based on liquid chromatography coupled with ion trap mass spectrometry (MS) detection with electrospray ionization interface has been developed for the identification and quantification of apomorphine in human plasma. Apomorphine was isolated from 0.5 mL of plasma using a liquid-liquid extraction with diethyl ether and boldine as internal standard, with satisfactory extraction recoveries. Analytes were separated on a 5-microm C18 Highpurity (Thermohypersil) column (150 mm x 2.1 mm I.D.) maintained at 30 degrees C, coupled to a precolumn (C18, 5-microm, 10 mm x 2.0 mm I.D., Thermo). The elution was achieved isocratically with a mobile phase of 2 mM NH4COOH buffer pH 3.8/acetonitrile (50/50, vol/vol) at a flow rate of 200 microL per minute. Data were collected either in full-scan MS mode at m/z 150 to 500 or in full-scan tandem mass spectrometry mode, selecting the [M+H]ion at m/z 268.0 for apomorphine and m/z 328.0 for boldine. The most intense daughter ion of apomorphine (m/z 237.1) and boldine (m/z 297.0) were used for quantification. Retention times were 2.03 and 2.11 minutes for boldine and apomorphine, respectively. Calibration curves were linear in the 0.025 to 20 ng/mL range. The limits of detection and quantification were 0.010 ng/mL and 0.025 ng/mL, respectively. Accuracy and precision of the assay were measured by analyzing 54 quality control samples for 3 days. At concentrations of 0.075, 1.5, and 15 ng/mL, intraday precisions were less than 10.1%, 5.3%, and 3.8%, and interday precisions were less than 4.8%, 6.6%, and 6.5%, respectively. Accuracies were in the 99.5 to 104.2% range. An example of a patient who was given 6 mg of apomorphine subcutaneously is shown, with concentrations of 14.1 ng/mL after 30 minutes and 0.20 ng/mL after 6 hours. The method described enables the unambiguous identification and quantification of apomorphine with very good sensitivity using only 0.5 mL of sample, and is very convenient for therapeutic drug monitoring and pharmacokinetic studies.

  6. On-chip tryptic digest with indirect coupling to ESI-MS using magnetic particles

    Czech Academy of Sciences Publication Activity Database

    Le Nel, A.; Křenková, Jana; Klepárník, Karel; Smadja, C.; Taverna, M.; Viovy, J.-L.; Foret, František

    2008-01-01

    Roč. 29, č. 24 (2008), s. 4944-4947 ISSN 0173-0835 R&D Projects: GA ČR(CZ) GA203/06/1685; GA AV ČR KAN400310651 Institutional research plan: CEZ:AV0Z40310501 Keywords : magnetic beads * MS * self-organization Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.509, year: 2008

  7. A Validated, Rapid HPLC-ESI-MS/MS Method for the Determination of Lycopsamine.

    Science.gov (United States)

    Jedlinszki, Nikoletta; Csupor, Dezső

    2015-07-01

    The aim of the present work was to develop and validate an HPLC-MS/MS method for the determination of a major pyrrolizidine alkaloid of comfrey (lycopsamine) in aqueous samples as a basis for the development of a method for the determination of absorption of lycopsamine by human skin. A linear calibration curve was established in the range of 1.32-440 ng. The intraday precision during the 3-day validation period ranged between 0.57 and 2.48% while the interday precision was 1.70% and 1.95% for quality control samples. LOD was 0.014 ng and recovery was above 97%. The lycopsamine content of the samples stored for 9 and 25 days at 22 degrees C, 10 degrees C and -25 degrees C did not vary. These results underline the good repeatability and accuracy of our method and allow the analysis of samples with very low lycopsamine content.

  8. Bahasa, Simbol, dan Religi

    OpenAIRE

    Supriyadi, Supriyadi

    1999-01-01

    Manusia sering disebut sebagai makhluk sosial, makhluk berakal, makhluk berseni, dan sebagainya. Tulisan ini secara tidak langsung membicarakan manusia sebagai makhluk berbahasa, bersimbol, dan bereligi . Meskipun demikian, titik tolaknya bukan pada manusia itu sendiri, tetapi pada bahasa, simbol, dan religinya, terutama pada hubungan di antara ketiganya . Hubungan antara bahasa dan simbol tidak diragukan lagi karena bahasa merupakan jenis simbol . Demikian juga hubungan antara simbol dengan ...

  9. Shocks in magneto-reactive-gas dynamics with application to the piston problem; Sur les chocs dans un milieu magnetodynamique reactif avec application au probleme du piston

    Energy Technology Data Exchange (ETDEWEB)

    Soubbaramayer, [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1967-03-01

    This work deals with detonation and deflagration waves in magnetogasdynamics. Four types of detonations and four types of deflagration are considered. We point out that the propagation of these waves is not always completely determined by the initial boundary conditions and the conservation laws across the discontinuity. To fix the ideas we consider the piston problem and we show that in some cases more conditions must be added to the conservation laws in order to provide sufficient data for the unique determination of the propagation process. We then show that the needed additional conditions may be derived from an investigation of the internal structure of the detonation and deflagration process in magneto gas dynamics. This internal structure is investigated for the eight types of process under the influence of the combustion mechanism and the dissipative coefficients (viscosities, electrical and thermal conductivity). Finally all the possible solutions for the piston problem are discussed in a simple case. The methods developed here may be extended to ionizing shocks. (author) [French] On considere dans ce travail les ondes de detonation et de deflagration en magneto-dynamique. Quatre types de detonation et quatre types de deflagration sont etudies. On montre d'abord que la propagation de ces ondes n'est pas toujours completement determinee par les conditions initiales, les conditions aux limites et les conditions de choc. Pour fixer les idees nous considerons le probleme du piston et nous montrons que, dans certains cas, des conditions supplementaires doivent etre jointes aux conditions de choc pour determiner l'ecoulement d'une facon unique. Nous montrons ensuite que ces conditions supplementaires peuvent etre deduites de l'analyse de la structure interne des detonations et des deflagrations magnetodynamiques. Cette structure interne est etudiee en tenant compte du mecanisme de combustion et des coefficients de dissipation (viscosites, conductivites

  10. Magnetic rotational polarisation in plasmas. Application to the measurement of electronic density; Polarisation rotatoire magnetique dans les plasmas. Application a la mesure de la densite electronique

    Energy Technology Data Exchange (ETDEWEB)

    Consoli, Terenzio; Dagai, Michel [Commissariat a l' energie atomique et aux energies alternatives - CEA (France)

    1960-07-01

    The rotation of a linearly polarised wave passing through a layer of plasma is determined. A network of curves enables these results to be applied to the electronic density measurement in a plasma during its evolution. Reprint of a paper published in Comptes rendus des seances de l'Academie des Sciences, t. 250, p. 1010-1012, sitting of 8 February 1960 [French] On determine la rotation d'une onde polarisee lineairement, traversant une couche de plasma. Un reseau de courbes permet d'appliquer ces resultats a la mesure de la densite electronique d'un plasma en evolution. Reproduction d'un article publie dans les Comptes rendus des seances de l'Academie des Sciences, t. 250, p. 1010-1012, seance du 8 fevrier 1960.

  11. APLIKASI SIG UNTUK PEMETAAN INDEKS KEPEKAAN LINGKUNGAN: STUDI KASUS DI PESISIR CILACAP DAN SEGARA ANAKAN (GIS Application for Environmental Sensitivity Index Mapping Case Study in Cilacap Coastal Area and Segara Anakan

    Directory of Open Access Journals (Sweden)

    Utantyo Utantyo

    2015-01-01

    Full Text Available ABSTRAK Sumberdaya pesisir dapat menerima dampak dari kecelakaan tumpahan minyak. Polusi minyak dapat terjadi dalam berbagai situasi lingkungan. Dalam hal ini, inventarisasi pesisir secara detil dikombinasikan dengan indeks sensitivitas memungkinkan ketersediaan informasi pada tingkat yang lebih baik bagi perencana pengelolaan tumpahan minyak. Sistem Informasi Geografis (SIG=Geographic Information System dapat meningkatkan penggunaan data yang dibutuhkan dalam menanggapi adanya tumpahan minyak tersebut serta perencanaan darurat. Studi ini dilakukan untuk mempelajari sensitivitas lingkungan dan mengkombinasikannya untuk membentuk prototipe sistem informasi sensitivitas lingkungan. Dengan menggunakan SIG di daerah pesisir Segara Anakan dan Cilacap. Salah satu strategi yang penting di dalam perencanaan darurat adanya tumpahan minyak adalah memprioritaskan respons tumpahan. Lingkungan pesisir dapat dikuantitatifkan dengan menetapkan skema klasifikasi indeks sensitivitas lingkungan (ISE=Environmemntal Sensitivity Index: ESI. Sensitivitas lingkungan mencerminkan derajad reaksi dari wilayah pesisir untuk bertatran dan pulih ketika terjadi bencana tumpahan minyak. Metode untuk menetapkan ISE adalah dengan mengkombinasikan factor-faktor yang terkait dari suatu sensitivitas lingkungan, antara lain (a paparan terhadap energi gelombang dan pasut, (b pelerengan garis pantai, (c jenis substrata, dan (d produktivitas biologi. Studi ini menekankan kemampuan SIG untuk memvisualisasikan dan memodernkan faktor-faktor sensitivitas lingkungan secara spasial. Hasil penelitian menunjukkan bahwa aplikasi SIG untuk mengelola memanipulasi dan menayangkan data pesisir yang relevan dapat dilaksanakan dan dapat dicatat keunggulannya di dalam upaya pemetaan sensitivitas lingkungan. Dalam penelitian ini wilayah pesisir Cilacap memiliki sensitivitas medium, karena daerah tersebut dibatasi oleh garis pantai ESI 5 (dengan panjang 11,6 km, dan dengan ESI 6 Sungai Donan (12,3 km

  12. Analisis Kebijakan dan Efektivitas Organisasi

    Directory of Open Access Journals (Sweden)

    Amir Syarifudin Kiwang

    2015-05-01

    Full Text Available Penerapan Peraturan Gubernur Nusa Tenggara Timur Nomor 8 Tahun 2011 tentang Organisasi dan Tata Kerja Unit Pelaksana Teknis Pendidikan dan Pelatihan Koperasi dan Usaha Mikro Kecil dan Menengah pada Dinas Koperasi dan Usaha Mikro Kecil dan Menengah Provinsi Nusa Tenggara Timur adalah dalam rangka untuk meningkatkan efektivitas kerja organisasi pada UPT Diklat Koperasi dan UMKM. Penelitian ini berusaha untuk melihat dampak kebijakan organisasi terhadap efektivitas organisasi dengan menggunakan enam elemen variabel dari kebijakan dan praktik manajemen. Keenam elemen tersebut adalah penetapan tujuan strategis, pencarian dan pemanfaatan sumber daya, lingkungan prestasi, proses komunikasi, kepemimpinan dan pengambilan keputusan, serta adaptasi dan inovasi organisasi. Penelitian kualitatif ini menggunakan pendekatan studi kasus. Teknik analisis data yang digunakan adalah analisis data model Miles dan Huberman, yang terdiri atas reduksi data, display/penyajian data, dan kesimpulan/verifikasi. Hasil penelitian menunjukkan bahwa efektivitas organisasi pada UPT Diklat koperasi dan UMKM belum berjalan secara baik, hal ini dapat dilihat dari beberapa hal antara lain, belum adanya tenaga spesialisasi pengelola diklat dan tenaga khusus (sarjana di bidang perkoperasian dan kondisi lingkungan kerja (lingkungan prestasi pada UPT Diklat koperasi dan UMKM yang belum efektif. Penempatan pegawai juga belum tepat, mutasi ke UPT Diklat Koperasi dan UMKM tidak memperhatikan latar belakang pendidikan dan spesialisasi/keahlian pegawai sehingga membutuhkan waktu dalam proses penyesuaian serta menurunkan jumlah pelaksanaan diklat dikarenakan keterbatasan alokasi dana.

  13. Sistem Pakar Diagnosis Hama dan Penyakit Tanaman Hortikultura dengan Teknik Inferensi Forward dan Backward Chaining

    Directory of Open Access Journals (Sweden)

    Ginanjar Wiro Sasmito

    2017-05-01

    Full Text Available One of the obstacles to doing cultivation of horticulture plant is to overcome pest and disease. Pest and disease attack can decrease productivity and even causes harvest fail that influence toward one of income sources the country. Therefore the diagnose on pest and disease must be done fastly and accurately. One of horticulture plant is red onion and chili plant. An expert system is offered as the second choice after expert on consultation. Using Expert System Development Life Cycle (ESDLC method, combination inference engine of and backward chaining for diagnosing pest and horticulture plant disease created as giving the solution. The technique of reasoning used in this research is the rule-based. The result of the research is an application that can be used to diagnosis pest and disease horticulture plant, that are red onion and chili. By this application, the farmer can determine quick action should be taken if the farm pests and diseases, without waiting for a consultation with an expert to do the handling. The application result also could be a learning system to the farmer about pest and disease horticulture plant. Salah satu kendala melakukan budidaya tanaman hortikultura adalah dalam mengatasi hama dan penyakit. Serangan hama dan penyakit dapat menurunkan produktivitas dan bahkan menyebabkan gagal panen yang berpengaruh terhadap salah satu sumber devisa negara. Oleh karena itu, diagnosis terhadap hama dan penyakit harus dilakukan dengan cepat dan akurat. Tanaman hortikultura tersebut salah satunya adalah bawang merah dan cabai. Sistem pakar dihadirkan sebagai pilihan kedua setelah pakar dalam melakukan konsultasi. Dengan menggunakan metode Expert System Development Life Cycle (ESDLC, penggabungan teknik inferensi forward dan backward chaining untuk diagnosis hama dan penyakit tanaman hortikultura dibuat sebagai solusi atas permasalahan yang ada. Teknik penalaran yang digunakan dalam penelitian ini yakni rule-based reasoning. Hasil

  14. TANGKI SEPTIK DAN MASALAHNYA

    Directory of Open Access Journals (Sweden)

    Sri Soewasti Soesanto

    2012-10-01

    Full Text Available Manusia yang sehat tiap hari membuang tinja yang harus ditampung dan/atau diolah secara saniter. Meskipun Indonesia telah 55 tahun merdeka dan telah memiliki banyak ahli sanitasi/teknik penyehatan baik lulusan dalam maupun luar negeri, namun cara pengelolaan tinja yang ada kebanyakan masih belum memenuhi syarat kesehatan. Tangki septik dianggap sebagai cara penampungan tinja yang terbaik, padahal sebenarnya masih terjadi pencemaran tanah dan air melalui saluran perembesan.Tangki septik (septic tank merupakan salah satu macam sarana pengolahan tinja manusia yang pada garis besarnya terdiri dari sebuah tangki pembusukan lumpur (sludge digester dan saluran perembesan efluen. Tangki pembusukan harus memenuhi syarat mengenai perbandingan panjang dan lebar serta syarat kedalaman maksimum dan minimum, agar pembusukan lumpur dari tinja manusia dapat berjalan sempurna malahan tidak berbau busuk lagi.

  15. Specific determination of clinical and toxicological important substances in biological samples by LC-MS

    International Nuclear Information System (INIS)

    Mitulovic, G.

    2001-02-01

    This thesis of this dissertation is the specific determination of clinical and toxicological important substances in biological samples by LC-MS. Nicotine was determined in serum after application of nicotine plaster and nicotine nasal spray with HPLC-ESI-MS. Cotinine was determined direct in urine with HPLC-ESI-MS. Short time anesthetics were determined in blood and cytostatics were determined in liquor with HPLC-ESI-MS. (botek)

  16. DEPRESI DAN GANGGUAN TIDUR

    Directory of Open Access Journals (Sweden)

    Wayan Eko Radityo

    2012-12-01

    Full Text Available Depresi merupakan gangguan mood berupa kesedihan yang intens, berlangsung dalamwaktu lama, dan mengganggu kehidupan normal yang insidennya semakin meningkatseiring dengan meningkatnya tekanan hidup. Tahun 2020, depresi diperkirakanmenempati urutan kedua penyakit di dunia. Gejala-gejala depresi terdiri dari gangguanemosi, gangguan kognitif, keluhan somatik, gangguan psikomotor, dan gangguanvegetatif. Salah satu gejala depresi yang muncul adalah gangguan tidur yang bisaberupa insomnia, bangun secara tiba-tiba, dan hipersomnia. Hal ini disebabkan olehgangguan neurotransmiter dan regulasi hormon. Selain sebagai gejala depresi, gangguantidur juga bisa merupakan penyebab depresi. Beberapa penelitian memberikanhubungan gangguan tidur dapat meningkatkan risiko depresi di kemudian hari.

  17. Improvement of the heat exchanges by application of an electric field in the boiling freon 12; Amelioration des echanges thermiques par application d'un champ electrique dans le freon 12 bouillant

    Energy Technology Data Exchange (ETDEWEB)

    Bonjour, Emmanuel; Verdier, Jacques; Weil, Louis [Commissariat a l' energie atomique et aux energies alternatives - CEA, Centre d' Etudes Nucleaires de Grenoble (France)

    1960-07-01

    lt was already known that the heat exchanges by simple convection are considerably improved by the application of an electric field, but no study about the effect of this field when there is ebullition has been issued until now. The authors indicate the result of their experimental investigations which present a very great interest for the increase of the efficiency of the refrigeration cycles. Reprint of a paper published in Revue generale du froid, Sep 1960 [French] On savait deja qu'il etait possible d'ameliorer sensiblement les echanges thermiques dus a la simple convection par l'application d'un champ electrique, mais jusqu'a present, il n'existait pas de resultats concernant l'effet de ce champ en presence d'ebullition. Les auteurs indiquent les resultats de leur investigation experimentale qui presente un tres grand interet pour l'accroissement de l'efficacite du cycle de refrigeration. Reproduction d'un article publie dans Revue generale du froid, Sep 1960.

  18. Superhydrophilic poly (styrene co acrylonitrile)-ZnO nanocomposite surfaces for UV shielding and self-cleaning applications

    Science.gov (United States)

    Singh, Rajender; Sharma, Ramesh; Barman, P. B.; Sharma, Dheeraj

    2017-11-01

    UV shielding based super hydrophilic material is developed in the present formulation by in situ emulsion polymerization of poly (styrene-acrylonitrile) with ZnO nanoparticles. The ESI-MS technique confirms the structure of polymer nanocomposite by their mass fragments. The XRD study confirms the presence of ZnO phase in polymer matrix. PSAN/ZnO nanocomposite leads to give effective UV shielding (upto 375 nm) and visible luminescence with ZnO content in polymer matrix. The FESEM and TEM studies confirm the symmetrical, controlled growth of PNs. The incorporation of ZnO nanofillers into PSAN matrix lead to restructuring the PNs surfaces into superhydrophilic surfaces in water contact angle (WCA) from 70° to 10°. We believe our synthesized PSAN/ZnO nanocomposite could be potential as UV shielding, luminescent and super hydrophilic nature based materials in related commercial applications.

  19. PERANCANGAN SISTEM INFORMASI AKUNTANSI KOPERASI DAN UMKM BERBASIS TECHNOPRENEUR

    Directory of Open Access Journals (Sweden)

    Dony Waluya Firdaus

    2017-08-01

    Full Text Available Abstract. The design of Accounting Information System of Cooperatives and UMKM based on Technopreneur can assist Cooperative and UMKM in presenting Financial Statement and produce accountable financial statements Accounting system development method using Rapid Application Development (RAD adjust the pace Software Development Life Cycle (SDLC in design using DFD and flowchart. UMKM and Cooperative accounting information system using Enterprise Resource Planning. Keywords: Design; Accounting information system; Cooperative; UMKM; ERP Abstrak. Perancangan Sistem Informasi Akuntansi Koperasi dan UMKM berbasis technopreneur dapat membantu Koperasi dan UMKM dalam menyajikan Laporan Keuangan dan menghasilkan laporan keuangan yang akuntabel. Metode pengembangan sistem informasi akuntansi menggunakan Rapid Application Development (RAD menyesuaikan pase Software Development Life Cycle (SDLC dalam perancangan menggunakan DFD dan flowchart. Sistem informasi akuntansi UMKM dan Koperasi menggunakan Enterprise Resources Planning. Keywords: Perancangan; Sistem Informasi Akuntansi; Koperasi; UMKM; ERP

  20. Radiant heat transfers in turbojet engines. Two applications, three levels of modeling; Transferts radiatifs dans les foyers de turboreacteurs. Deux applications, trois niveaux de modelisation

    Energy Technology Data Exchange (ETDEWEB)

    Schultz, J L; Desaulty, M [SNECMA, Centre de Villaroche, 77 - Moissy-Cramayel (France); Taine, J [Ecole Centrale de Paris, Laboratoire EM2C. CNRS, 92 - Chatenay-Malabry (France)

    1997-12-31

    Several applications linked with the dimensioning of turbojet engines require the use of modeling of radiant heat transfers. Two different applications are presented in this study: the modeling of heat transfers in the main combustion chamber, and modeling of the infrared signature of the post-combustion chamber of a military engine. In the first application, two types of radiant heat transfer modeling are presented: a global modeling based on empirical considerations and used in rapid pre-dimensioning methods, and a modeling based on a grey gases concept and combined to a ray shooting type technique allowing the determination of local radiant heat flux values. In the second application, a specific modeling of the radiant heat flux is used in the framework of a ray shooting method. Each model represents a different level of successive approximations of the radiant heat transfer adapted to flow specificities and to the performance requested. (J.S.) 16 refs.

  1. Radiant heat transfers in turbojet engines. Two applications, three levels of modeling; Transferts radiatifs dans les foyers de turboreacteurs. Deux applications, trois niveaux de modelisation

    Energy Technology Data Exchange (ETDEWEB)

    Schultz, J.L.; Desaulty, M. [SNECMA, Centre de Villaroche, 77 - Moissy-Cramayel (France); Taine, J. [Ecole Centrale de Paris, Laboratoire EM2C. CNRS, 92 - Chatenay-Malabry (France)

    1996-12-31

    Several applications linked with the dimensioning of turbojet engines require the use of modeling of radiant heat transfers. Two different applications are presented in this study: the modeling of heat transfers in the main combustion chamber, and modeling of the infrared signature of the post-combustion chamber of a military engine. In the first application, two types of radiant heat transfer modeling are presented: a global modeling based on empirical considerations and used in rapid pre-dimensioning methods, and a modeling based on a grey gases concept and combined to a ray shooting type technique allowing the determination of local radiant heat flux values. In the second application, a specific modeling of the radiant heat flux is used in the framework of a ray shooting method. Each model represents a different level of successive approximations of the radiant heat transfer adapted to flow specificities and to the performance requested. (J.S.) 16 refs.

  2. Keragaman dan Peran Biologi Arthrophoda pada Sawah Irigasi dan Tegalan

    OpenAIRE

    Suwarno, Suwarno

    2016-01-01

    Penelitian ini bertujuan untuk mengetahui keragaman arthropoda dan peran biologinya pada tanah sawah irigasi dan tegalan. Penelitian ini dilaksanakan di daerah persawahan di daerah Sragen pada bulan Maret – Mei 2016. Metode Penelitian dengan menggunakan pitfall trap atau perangkap jebakan yang diletakkan area persawahan dan tegalan. Teknik pengumpulan data dengan menggunakan purposive sampling. Sampel arthropoda yang diperoleh diidentifikasi dan dianalisis di Laboratorium pendidikan Biologi. ...

  3. Pengaruh Konsentrasi Subletal Deltametrin terhadap Nutrisi dan Pertumbuhan Tanaman Padi

    Directory of Open Access Journals (Sweden)

    Yuni Ratna

    2011-12-01

    Full Text Available Increasing the reproductive capacity through increasing plant growth and nutrition is one plausible mechanism of resurgence. This research was intended to determine the effect of deltamethrin on plant vigor and nutrition contents. The experiment was carried out outdoor. The treatments tested were deltamethrin (50 ppm, buprofezin (100 ppm, and control (water. Insecticide applications were applied one time (at age 26 d or 50 d and two times (at age 26 and 50 d. Deltamethrin applications as many as two times did not increase the total chlorophyll and the photosynthesis rate, nutrients (total nitrogen, total protein, total sugar, total reducing sugar at aged 26 d, and sucrose, growth (plant height and number of tillers, and yield (number of panicles. However, application of deltamethrin at aged 26 d increased the amount of asparagine. Asparagine is known to be associated with the feeding rate of Nilaparvata lugens stimulation. Therefore, increasing level of asparagine after application of deltamethrin at sublethal concentration was considered as one of the factors that might be involved in the mechanism of N. lugens resurgence. Salah satu mekanisme resurjensi adalah peningkatan reproduksi hama melalui peningkatan nutrisi dan pertumbuhan tanaman. Penelitian ini dimaksudkan untuk melihat pengaruh deltametrin terhadap kandungan nutrisi dan vigor tanaman. Pengujian dilakukan di lapangan. Perlakuan yang diuji adalah deltametrin 50 ppm, buprofezin 100 ppm, dan kontrol (air. Aplikasi insektisida dilakukan satu kali masing-masing pada umur tanaman 26 dan 50 hst dan dua kali pada umur 26 dan 50 hst. Aplikasi deltametrin sebanyak dua kali tidak meningkatkan total klorofil dan laju fotosintesis, nutrisi (total nitrogen, total protein, total gula, total gula reduksi pada 26 hst, dan sukrosa kecuali asparagin, pertumbuhan (tinggi tanaman dan jumlah anakan, dan hasil (jumlah malai tanaman. Oleh karena asparagin berperan sebagai pemacu laju makan Nilaparvata

  4. Evaluasi Sifat Morpologi dan Teknologi Pengolahan pada Gabah dan Beras

    OpenAIRE

    Santosa, Susilo

    2017-01-01

    Penelitian evaluasi dan beras terhadap mutu dan jumlah hasil ditekankan pada lr36 , lr38 dan Cisadane. Penelitian dilakukan di laboratorium Balai Penelitian Tanaman Pangan Karawang. Hasil studi menunjukkan diantara ketiga varitas, Cisadane mempunyai ukuran dimensi butiran yang lebih besar daripada Ir36 dan Ir38. Di antara ketiga varitas, persen kulit sekam yang tertinggi didapat 23,57 % pada lr38 diikuti 22,32% pada Ir36 dan 19,5% pada Cisadane. Persen beras pecah kulit tertinggi diperoleh pa...

  5. Evaluasi Sifat Morpologi Dan Teknologi Pengolahan Pada Gabah Dan Beras

    OpenAIRE

    Santosa, Susilo

    1982-01-01

    Penelitian evaluasi dan beras terhadap mutu dan jumlah hasil ditekankan pada lr36 , lr38 dan Cisadane. Penelitian dilakukan di laboratorium Balai Penelitian Tanaman Pangan Karawang. Hasil studi menunjukkan diantara ketiga varitas, Cisadane mempunyai ukuran dimensi butiran yang lebih besar daripada Ir36 dan Ir38. Di antara ketiga varitas, persen kulit sekam yang tertinggi didapat 23,57 % pada lr38 diikuti 22,32% pada Ir36 dan 19,5% pada Cisadane. Persen beras pecah kulit tertinggi diperoleh pa...

  6. Chrono-potentiometry in molten chlorides. Application to the study of the electrochemical properties of uranium and plutonium in the LiCl-KCl eutectic; Chronopotentiometrie dans les chlorures fondus. Application a l'etude des proprietes electrochimiques de l'uranium et du plutonium dans l'eutectique LiCl-KCl

    Energy Technology Data Exchange (ETDEWEB)

    Leseur, A. [Commissariat a l' Energie Atomique, Fontenay-aux-Roses (France). Centre d' Etudes Nucleaires

    1969-05-01

    Using solutions of cadmium chloride in the eutectic LiCl-KCl, a chrono-potentiometric method has been developed with a view to its application to the study of molten solutions. Particular attention has been paid to the choice of the indicator electrodes. The method makes it possible to analyze molten solutions quantitatively and to determine diffusion coefficients and their activation energies; it yields furthermore information about the nature and the behaviour of ionic species in solution. The method has been applied to the study of solutions of uranium and plutonium chloride in the eutectic LiCl-KCl. Linear chrono-amperometry has been used for studying these solutions quantitatively, but chrono-potentiometry, of which the theory is better developed, is better suited to a quantitative study. The results obtained have made it possible to determine the diffusion coefficients of the ions Cd{sup 2+}, U{sup 3+}, U{sup 4+} and U(IV) in the presence of F{sup -} and Pu{sup 3+} ions, as well as the activation energy of the diffusion coefficients. (author) [French] La mise au point de la chronopotentiometrie comme moyen d'etude des solutions fondues a ete effectuee avec des solutions de chlorure de cadmium dans l'eutectique LiCl-KCl. Le probleme du choix des electrodes indicatrices a ete particulierement etudie. La methode permet l'analyse quantitative des solutions fondues ainsi que la determination des coefficients de diffusion et de leurs energies d'activation: elle donne en outre des renseignements sur la nature et le comportement des especes ioniques en solution. Elle a ete appliquee a l'etude des solutions des chlorures d'uranium et de plutonium dans l'eutectique LiCl-KCl. La chronoamperometrie lineaire a ete utilisee pour l'etude qualitative de ces solutions, mais la chronopotentiometrie, dont la theorie est plus complete, convient mieux pour l'etude quantitative. Les resultats obtenus ont permis de determiner les

  7. Modification de la surface du cuivre par implantation ionique par source plasma (IISP): applications à l’érosion cathodique dans les systèmes à arcs

    OpenAIRE

    Roy, F

    2006-01-01

    L’érosion cathodique est un phénomène bien connu qui limite la durée de vie de l’électrode négative dans les systèmes à arcs. Dans le présent mémoire, nous avons tenté de voir si la formation de précipités nanométriques d’oxyde de cuivre pouvait réduire l’érosion cathodique nécessaire au maintien de l’arc en mode thermo-champ (T-F). Les dits précipités ont été produits par implantation ionique par source plasma (IISP). Avec l’aide de techniques de caractérisation telle que la microscopie à fo...

  8. Liever kraanwater dan bronwater

    NARCIS (Netherlands)

    Kole, A.P.W.

    2011-01-01

    Een test in het Restaurant van de Toekomst van de invloed van CO2-labels op het aankoopgedrag van consumenten, heeft nog geen duidelijk beeld opgeleverd. Wel pakten mensen vaker kraanwater dan bronwater.

  9. Dan Performer Mei Lanfang

    DEFF Research Database (Denmark)

    Risum, Janne

    2010-01-01

    The convention of performing female characters (dan characters) in Beijing opera, as practised by its most prominent male performer of female characters Mei Lanfang, and its and his cultural context and aesthetic aim...

  10. Consumption estimation in system design for real time embedded applications; Estimation de la consommation dans la conception systeme des applications embarquees temps reel

    Energy Technology Data Exchange (ETDEWEB)

    Laurent, J.

    2002-12-15

    Today, power and energy consumption have become, as time and area, an important constraint when you design a system. Indeed modern applications use more and more processing and memory resources so these lead a significant increase of consumption. Furthermore, embedded software impact is preponderant in real time system so the code optimisation has a great impact onto the consumption constraint. Several research teams have already developed estimation methodologies for processor but almost are at instruction level (ILPA). With this kind of method you have to measure the consumption of each instruction of the instruction set and also the inter-instruction consumption overhead. For complex architecture, this kind of methodology is not adapted due to the prohibitive number of consumption measures. So the characterisation time of this kind of architecture is too important furthermore with this method is very difficult to take into account the external environment. For actual architecture another method is needed to reduce the characterisation time while preserving the accuracy. The reduction of the characterisation time have to be realized by increasing the abstraction level. So, we propose here a new approach based on a functional and architectural analysis of the target in consumption point of view (FLPA). Our methodology has two steps: the first one is a modeling step and the second is estimation step. (author)

  11. Long term modelling in a second rank world: application to climate policies; Modeliser le long terme dans un monde de second rang: application aux politiques climatiques

    Energy Technology Data Exchange (ETDEWEB)

    Crassous, R

    2008-11-15

    This research aims at the identification of the dissatisfaction reasons with respect to the existing climate models, at the design of an innovating modelling architecture which would respond to these dissatisfactions, and at proposing climate policy assessment pathways. The authors gives a critique assessment of the modelling activity within the field of climate policies, outlines the fact that the large number and the scattering of existing long term scenarios hides a weak control of uncertainties and of the inner consistency of the produced paths, as well as the very low number of modelling paradigms. After a deepened analysis of modelling practices, the author presents the IMACLIM-R modelling architecture which is presented on a world scale and includes 12 areas and 12 sectors, and allows the simulation of evolutions by 2050, and even 2100, with a one-year time step. The author describes a scenario without any climate policy, highlights reassessment possibilities for economical trajectories which would allow greenhouse gas concentration stabilisation on a long term basis through the application of IMACLIM-R innovations. He outlines adjustment and refinement possibilities for climate policies which would robustly limit the transition cost risks.

  12. ANALISIS PENERAPAN AKUNTANSI ZAKAT DAN INFAK/SHADAQAH PADA LEMBAGA AMIL ZAKAT DI KOTA MAKASSAR (Studi Kasus LAZ Masjid Al-Markaz, LAZ Rumah Zakat, LAZISMU dan BAZNAS)

    OpenAIRE

    HAMBALI, MUHAMAD

    2017-01-01

    2017 ABSTRAK ANALISIS PENERAPAN AKUNTANSI ZAKAT DAN INFAK/SHADAQAH PADA LEMBAGA AMIL ZAKAT DI KOTA MAKASSAR (Studi Kasus LAZ Masjid Al-Markaz, LAZ Rumah Zakat, LAZISMU dan BAZNAS) Analysis of Accounting Application Of Zakat and Infak / Shadaqah on Amil Zakat Institute In Makassar City (The object of this study is Masjid Al Markaz, LAZ Rumah Zakat, LAZISMU dan BAZNAS) Muhamad Hambali Abdul Hamid Habbe Abdul Rahman Penelitian...

  13. Aplikasi web promosi kuliner dan rumah makan online

    Directory of Open Access Journals (Sweden)

    Khairus Suhada

    2017-05-01

    Full Text Available AbstrakKemajuan teknologi mendorong pertumbuhan dan perkembangan sektor perdagangan, usaha dan pemasaran. Tingginya tingkat keberhasilan dalam perdagangan didorong oleh berbagai faktor pendukung termasuk promosi dan periklanan. Melalui promosi dan periklanan yang tepat, perdagangan dibidang kuliner dapat  tumbuh dengan baik. Memanfaatkan teknologi melalui aplikasi promosi kuliner dan rumah makan secara online dapat menjadi media promosi yang tepat. Aplikasi Web Promosi Kuliner dan Rumah Makan Online dibangun menggunakan metode System Development Life Cycle(SDLC. Perancangan sistem menggunakan Konteks diagram dan Data Flow Diagram (DFD dan diterapkan menggunakan bahasa pemrograman PHP serta database MySQL. Aplikasi memberikan fasilitas berupa pencarian informasi seperti harga menu, alamat rumah makan, lokasi rumah makan serta kontak rumah makan. Fasilitas unggulan berupa fitur peta lokasi rumah makan yang terhubung dengan google map. Kata kunci: aplikasi web, promosi kuliner dan rumah makan, google map Abstract               Technological advances promote the growth and development of the trade, business and marketing sector. The high level of success in trading is driven by various supporting factors including promotion and advertising. Through proper promotion and advertising, culinary trade can grow well. Utilizing technology through culinary promotion apps and restaurants online can be the right promotional media. Web Application Culinary Promotion and Online Restaurant is built using System Development Life Cycle (SDLC method. System design using Context diagrams and Data Flow Diagrams (DFD and applied using PHP programming language as well as MySQL database. Application provides facilities in the form of information search such as menu price, restaurant address, restaurant location and restaurant contact. Excellent facility in the form of map location map of restaurant that connected with google map.  Keywords: web

  14. APLIKASI BUSINESS INTELLIGENCE UNTUK ANALISA DAN PRAKIRAAN CUACA MARITIM

    Directory of Open Access Journals (Sweden)

    Subekti Mujiasih

    2015-01-01

    Full Text Available Salah satu teknologi yang dapat mewujudkan kecepatan dan kemudahan analisa data adalah Business Intelligence (BI. Teknologi ini dapat menampilkan data dalam bentuk grafik yang bersifat multidimensi, sehingga dapat dilakukan pemilihan informasi sesuai kebutuhan. Aplikasi BI yang dibangun tidak hanya membuat tampilan berbagai komponen cuaca dalam bentuk grafik/dashboard, tetapi juga suatu gudang data. Dalam proses pembuatan informasi prakiraan cuaca maritim diperlukan banyak komponen data, diantaranya arah dan tinggi gelombang, arah dan kecepatan angin, pasang surut dan swell. Data tersebut diintegrasikan dalam bentuk data warehouse secara multidimensi melalui dimensi waktu dan lokasi. Data warehouse yang dikembangkan untuk mendukung model BI hanya yang bersifat deparmental, yaitu berbentuk datamart. Aplikasi BI yang dikembangkan meliputi aplikasi ETL dan aplikasi Dashboard dengan memanfaatkan perangkat lunak Visual Studio 2008, SQL Server Database dan Analysis Services 2008. Aplikasi ini menyediakan kemudahan dan kecepatan dalam melakukan pencarian, pemilihan dan analisa data. Trend data yang dihasilkan dari proses tersebut menjadi pengontrol range nilai prediksi cuaca maritim.   One technology that can realize rapidity and simplicity of data analysis is Business Intelligence. This technology can present multidimensional data both in graphical and spatial form, so selecting the information as needed will easily be done. The developed BI is not only graphical product but also data warehouse. In the process of providing marine weather forecast information it requires many components of data including wave direction and height, wind direction and speed, tides and swell. These data are integrated in a multidimensional form of Data warehouse through the dimension of time and location. The developed data warehouse for supporting the model of Business Intelligence is datamart that covers only one division. The resulted BI includes ETL application and

  15. Les réacteurs à membranes : possibilités d'application dans l'industrie pétrolière et pétrochimique Membrane Reactors: Possibilities of Application in the Petroleum and Petrochemical Industry

    Directory of Open Access Journals (Sweden)

    Guy C.

    2006-11-01

    Full Text Available Cet article fait le point sur l'état de la recherche dans le domaine des réacteurs chimiques avec séparation par membrane intégrée et de leur applications dans le domaine du raffinage et de la pétrochimie. Trois applications potentiellement intéressantes sont identifiées et, pour chacune, les avantages de l'utilisation d'un réacteur à membrane sont discutés. Ce sont : la déshydrogénation du propane en propylène, la déshydrogénation d'un naphtène cyclohexanique et le vaporéformage du gaz naturel. Pour ces réactions, les membranes à base de palladium apparaissent les plus performantes compte tenu de leur tenue en température, de leur sélectivité et de leur perméabilité à l'hydrogène. Quelques éléments relatifs à leur développement sont présentés en conclusion. Recently, the use of membrane in reaction engineering has been more and more advocated. The selective separation of the products from the reaction mixture allows to achieve higher conversion or better selectivity or to operate under less severe conditions or with smaller units. This paper presents an update on the recent advances in the field of chemical membrane reactors and on their applications in refining and petrochemistry. Previous work. Most of the possible applications of membrane reactors in petroleum and petrochemical industry concern gaseous catalytic reactions. For this reason, gas permeation membranes are the primary component of membrane reactors. Gas permeation membranes present different types of physical structure : dense, microporous or asymmetric which is a combination of the two. Separating properties of dense membranes are function of the solubility and diffusivity of each gaseous component in the membrane material. For microporous membranes, they follow four mechanisms : Knudsen diffusion, surface diffusion, capillary condensation or molecular sieving. Although organic polymers are the common constituent of gas permeation membrane, their

  16. La mobilité quotidienne dans les grandes villes du monde : application de la théorie des réseaux bayésiens

    Directory of Open Access Journals (Sweden)

    Giovanni Fusco

    2004-02-01

    Full Text Available À la frontière entre statistiques multivariées et intelligence artificielle, les réseaux bayésiens sont un puissant outil de modélisation de connaissance systémique. Une utilisation particulièrement intéressante est celle de la recherche des liens causaux entre variables dans une base de données. Dans cet article, nous analysons une base de données urbaines sur la mobilité quotidienne couvrant plus de cent grandes villes mondiales. À l'aide d'algorithmes de génération de réseaux bayésiens, nous avons produit deux réseaux reliant les variables et traduisant deux hypothèses différentes sur la hiérarchie causale entre elles. Si l’on introduit l’hypothèse que la mobilité détermine la structure urbaine, on crée alors un réseau qui  identifie la motorisation de la population comme étant une variable cruciale. Ce réseau s’avère plus probable que celui résultant de l’hypothèse opposée. En revanche, les deux réseaux concordent sur l’importance de l’offre de voirie rapide urbaine et de la vitesse moyenne du réseau routier dans l’explication du partage modal et des coûts et des externalités des transports urbains.

  17. Application d'une équation d'état à la simulation du comportement thermodynamique des fluides dans les gisements et dans les installations de surface Application of an Equation of State to Simulating the Thermodynamic Behaviour of Fluids in Reservoirs and Surface Installations

    Directory of Open Access Journals (Sweden)

    Jain C.

    2006-11-01

    Full Text Available La connaissance des propriétés thermodynamiques des fluides pétroliers, en particulier des masses volumiques et des coefficients d'équilibre liquide-vapeur, intervient à divers stades de la production : primaire, secondaire par in-jection de gaz (C02 ou hydrocarbures miscibles, vapeur d'eau, séparation, réseau de collecte et de transport. L'ampleur du domaine de pression et de température à l'intérieur duquel on a besoin de connaître les propriétés des huiles et des gaz à condensat, et le fait que la compo-sition d'ensemble des mélanges diphasiques ne cesse de varier au cours de leur déplacement soit dans les gisements, soit dans les installations d'exploitation, rendent mani-feste l'intérêt de pouvoir calculer ces propriétés, en évi-tant d'avoir recours à des travaux de laboratoire beaucoup trop importants. Pour résoudre ces problèmes, une nouvelle équation d'état appelée Redlich-Kwong Développée (RKD a été mise au point. Au cours de cet exposé, nous verrons que cette équation restitue les enveloppes diphasiques de l'équilibre liquide-vapeur avec une qualité au moins égale à celles des méthodes de Soave et de Peng-Robinson qui jouissent actuellement d'une grande notoriété. L'avantage de ce modèle sur ces dernières méthodes est l'évaluation simultanée des propriétés volumétriques des phases en présence avec une bonne précision, ce qui est d'une grande utilité pour l'application de ce modèle aux problèmes industriels. Knowing the thermodynamic properties of petroleum fluids, and in particular the density and liquid-vapor equilibrium coefficients, is important at different stages of production, i. e. primary production, secondary production by gas flooding (CO2 or miscible hydrocarbons, steam, separation, gathering network and transportation. The pressure and temperature range within which the oil and gas-condensate properties must be known coupled with the fact that the overall composition of

  18. PREFERENSI PEMBIAYAAN USAHA MIKRO DAN KECIL : PERSPEKTIF GENDER DAN ENTREPRENEURABILITY

    Directory of Open Access Journals (Sweden)

    Khaira Amalia Fachrudin

    2013-06-01

    Full Text Available Preferensi pembiayaan dalam perusahaan besar lebih didasarkan pada karakteristik perusahaan tersebut.  Namun dalam usaha mikro dan kecil hal ini mungkin berbeda dan bergantung pada karakteristik pemiliknya seperti gender dan entrepreneurability.   Perbedaan gender mungkin juga membedakan entrepreneurability dan dukungan yang diterima.  Penelitian ini akan menguji apakah terdapat perbedaan preferensi pembiayaan berdasarkan gender, entrepreneurability berdasarkan gender dan berdasarkan preferensi pembiayaan, serta perbedaan dukungan berdasarkan gender.  Sampel dari usaha mikro dan kecil yang bergerak dalam bidang kuliner  diuji dengan uji beda Independent Sample t Test dan kemudian dengan Crosstabulation untuk lebih memperinci hasilnya.  Hasil uji menunjukkan bahwa tidak terdapat perbedaan yang signifikan preferensi pembiayaan berdasarkan gender dan berdasarkan  entrepreneurability, namun entrepreneurability berbeda signifikan berdasarkan gender dan juga ditemukan bahwa dukungan moral, tenaga, dan modal yang diterima pemilik usaha pria dan wanita tidak berbeda signifikan (p value lebih kecil dari 0.05.   Hasil ini menunjukkan bahwa terdapat kesetaraan gender dalam pembiayaan usaha dan entrepreneurability lebih tinggi pada pria.  Pria pemilik usaha juga mendapatkan dukungan tenaga kerja yang lebih banyak daripada wanita.  Dukungan tenaga ini adalah salah satu bentuk  financial bootstrapping karena dapat mengurangi pembiayaan usaha

  19. ANALISIS HUBUNGAN KEMANDIRIAN KEUANGAN DAERAH DAN KETERGANTUNGAN DAERAH TERHADAP PENGANGGURAN DAN KEMISKINAN

    Directory of Open Access Journals (Sweden)

    Rosyafah Febiandani

    2017-06-01

    Full Text Available Adanya desentralisasi fiskal diharapkan dapat menciptakan kemandirian daerah dan dapat mengurangi ketergantungan pemerintah daerah terhadap pemerintah pusat. Kemandirian keuangan daerah dicerminkan dengan perbandingan besarnya PAD terhadap total pendapatan daerah. Sejak 10 tahun dilaksanakannya otonomi daerah sesuai UU No 32 Tahun 2004, kemandirian keuangan daerah di Provinsi Jawa Tengah masih berada di level yang kurang baik dibandingkan dengan provinsi lainnya di Pulau Jawa. Jumlah pengangguran dan jumlah penduduk miskin di Provinsi Jawa Tengah juga masih terhitung tinggi. Penelitian ini bertujuan untuk mengetahui hubungan dari tingkat kemandirian keuangan daerah dan tingkat ketergantungan daerah terhadap tingkat pengangguran dan tingkat kemiskinan di kabupaten/kota Provinsi Jawa Tengah Tahun 2013. Data yang digunakan dalam penelitian ini adalah data sekunder. Metode analisis yang digunakan adalah Analisis Korelasi Kanonikal menggunakan bantuan program SPSS. Hasil penelitian menunjukkan kemandirian keuangan daerah mempunyi hubungan yang signifikan, kuat, dan tidak searah dengan pengangguran dan kemiskinan. Sedangkan hubungan antara ketergantungan daerah terhadap kemiskinan dan pengangguran mempunyai hubungan yang signifikan, tidak kuat, dan tidak searah. Peningkatan kemandirian keuangan daerah guna mengurangi tingkat ketergantungan terhadap pemerintah pusat dapat dilakukan dengan cara menggali dan mengelola sumber daya atau potensi daerah yang dimilikinya secara efektif dan efisien sebagai sumber utama pendapatan keuangan daerahnya. Fiscal decentralization is expected to create independency regional financial and to reduce the dependence of local governments to the central government. Independency regional financial can be result by the ratio of PAD to total local revenue. Since 10 years the implementation of regional autonomy based on UU No. 32 of 2004, independency regional financial in Central Java is still unwell compared to the other

  20. DETEKSI DAN MANAJEMEN REFEEDING SYNDROME

    OpenAIRE

    Darmadi Darmadi; Riska Habriel Ruslie

    2012-01-01

    AbstrakRefeeding syndrome (RFS) dideskripsikan sebagai perubahan biokimiawi, manifestasi klinis dan komplikasi sebagai konsekuensi pemberian nutrisi pada pasien kurang gizi. Refeeding syndrome ini menyebabkan dampak buruk dan kematian. Sindroma ini lebih sering terjadi pada kelompok risiko. Refeeding syndrome merupakan suatu sindroma yang sering tak terdiagnosis oleh karena itu perlu peningkatan pengetahuan dan kesadaran dari tenaga medis untuk mengurangi morbiditas dan mortalitas dari RFS. K...

  1. Synthèse bibliographique sur le comportement de recherche de l’hôte chez la punaise de lit (Cimex lectularius) et applications dans le cadre de la lutte intégrée

    OpenAIRE

    Legrand, Pauline; Verheggen, François; Haubruge, Eric; Francis, Frédéric

    2016-01-01

    Cette étude analyse le comportement de recherche de l’hôte chez la punaise de lit, Cimex lectularius, en portant une attention particulière sur les stimuli émis par l’Homme et impliqués dans ce processus d’orientation. Elle met également en évidence les applications possibles en matière de lutte intégrée. La punaise de lit est un ectoparasite exclusivement hématophage étroitement lié à l’Homme depuis des millénaires. Lors de sa recherche alimentaire, cet insecte utilise des stimuli émis pa...

  2. INOVASI DAN STRATEGI PENCAPAIANNYA

    Directory of Open Access Journals (Sweden)

    Liem Ferryanto

    2009-01-01

    Full Text Available Innovation is the way of life of any institution to profitably sustain its life. It starts with empathy, the ability to reach outside of ourselves and walk in someone else’s shoes, and optimal implementation of the newly advanced technology. Innovation shows its results through continuously hard working efforts known as "10 Thousand Hours Rule". As world uncertainty creates complexity we, instead of predicting, should therefore anticipate the future by creating and managing real options on contingent projects or elements of alternative optimal strategies. This should reflect into our portfolio strategy. Abstract in Bahasa Indonesia: Inovasi merupakan darah bagi suatu institusi untuk bisa hidup berkelanjutan serta menguntungkan. Inovasi berupa penemuan baru secara sistematis yang berawal dari empati, kemampuan untuk melihat dunia melalui mata orang lain, dan pemanfaatan secara optimal kemajuan teknologi yang ada. Inovasi baru menghasilkan buahnya melalui kerja keras, yaitu dengan mengikuti “Aturan 10 Ribu Jam” secara berkesinambungan. Ketidakpastian, interaksi, keterbatasan dan degradasi menciptakan kompleksitas tentang kebutuhan dan solusi di masa depan. Oleh sebab itu daripada meramalkan risiko yang bakal terjadi, kita sebaiknya memasang strategi berupa skenario untuk mereduksi akibat dari risiko masa depan yang tidak kita mengerti. Skenario ini dapat diperoleh lewat penciptaan dan penanganan beberapa pilihan nyata atas semua proyek antisipatif yang ada. Kata kunci: Inovasi, ketidakpastian dan kompleksitas, aturan 10 ribu jam, paradoks strategi, peta jalan, empati, kerja berkesinambungan.

  3. PENGELOLAAN PENELITIAN DAN PENGEMBANGAN KESEHATAN DI THAILAND, MYANMAR, DAN INDIA

    Directory of Open Access Journals (Sweden)

    Anorital, SKM Anorital, SKM

    2012-09-01

    Full Text Available Dalam bulan Januari 1991 yang lalu, Sdr. Anorital, SKM (Ka. Subbag. Pengumpulan dan PengolahanData Badan Litbangkes dan H. Syafwani Mirin, SKM (Ka. Bag. Keuangan Badan Litbangkes memperoleh fellowship dari WHO untuk melakukan studi perbandingan ke institusi-institusi penelitian kesehatan di Thailand,Myanmar, dan India.Berikut di bawah ini tulisan bersangkutan yang menggambarkan secara garis besar pengelolaan penelitian dan pengembangan kesehatan pada masing-masing negara obyek studi. Semoga informasi yang terkandung pada tulisan ini dapat bermanfaat bagi pengembangan Badan Penelitian dan Pengembangan Kesehatan.

  4. Une stratégie adaptive au changement climatique dans le Moyen ...

    International Development Research Centre (IDRC) Digital Library (Canada)

    Des pratiques d'adaptation et de gestion de risques dans le secteur de l'eau sont en voie d'application dans différents pays et régions du monde à la lumière des impacts de changement climatique prévus. Dans la région MENA, la sensibilisation de toutes les parties prenantes sur la signification du changement climatique ...

  5. Le phosphore limite-t-il la production intensive du riz dans la plaine ...

    African Journals Online (AJOL)

    admin

    Le phosphore (P) est un élément important dans la nutrition minérale du riz et dans l'élaboration du rendement paddy. Des essais soustractifs ont été conduits en milieu paysan dans la plaine rizicole de Bagré au cours de trois campagnes successives pour évaluer l'effet de l'application de P sur le rendement paddy. La.

  6. Application of radioisotope techniques to the study of endemic goitre on Idjwi Island; Utilisation de methodes radioisotopiques dans l' etude du goitre endemique de l'Ile Idjwi

    Energy Technology Data Exchange (ETDEWEB)

    Delange, F.; Thilly, C.; Pourbadc, P.; Ermans, A. M. [CEMUBAC auprès de l' IRSAC, Lwiro (Congo, The Democratic Republic of the); Université libre de Bruxelles, Brussels (Belgium)

    1970-01-15

    On a world-wide scale endemic goitre represents one of the major problems of public health inasmuch as at least 200 million people are affected by this disease. Endemic goitre is particularly prevalent in Africa. The authors have recently undertaken a study of endemic goitre on Idjwi Island (Lake Kivu). The inhabitants of this island comprise an isolated population group. The island is geographically divided into a north and south zone with only occasional contact between the populations of the two zones. The entire population of the island has been examined and three zones can be distinguished as far as the prevalence of goitre is concerned: in the north of the island the number of cases is very high (averaging 54.4% of the population), whereas it drops to 5.3% in a limited region in the south-west; in the south and south-east of the island it is somewhere between the two. Radioisotope techniques have been applied to the study of three basic public health aspects of the disease. (author) [French] Le goitre endémique constitue à l’échelle mondiale un des problèmes majeurs de la santé publique puisque 200 millions de sujets au moins sont atteints par la maladie. Les endémies goitreuses sont particulièrement importantes en Afrique. Les auteurs ont entrepris récemment l'étude de l’endémie goitreuse de l'îleIdjwi (lac Kivu). Cette île constitue un groupe isolé de population. Elle est séparée géographiquement en deux zones: nord et sud. Les contacts entre les populations de ces deux zones sont épisodiques. La totalité de la population de l’île a été examinée. Trois zones peuvent être distinguées en ce qui concerne la prévalence du goitre: dans le nord de l’île elle est très élevée (valeur moyenne 54,4% de la population); par contre elle tombe à 5,3% dans une région limitée du sud-ouest; dans le sud et le sud-est de l’île elle est intermédiaire entre les deux premières. Des méthodes radioisotopiques ont été appliquées à l

  7. Kinerja Dan Efisiensi Bank Pemerintah (Bumn) Dan Busn Yang Go Publik Di Indonesia

    OpenAIRE

    Haryanto, Sugeng

    2012-01-01

    Penelitian ini menganalisis kinerja dan tingkat efisiensi bank-bank BUMN dan BUSN yang go Publik di Bursa Efek Indonesia. Sample penelitian ini mengambil tiga bank BUMN Bank BNI 46, Bank Mandiri dan Bank BRI) dan tiga bank BUSN (Bank BCA, Bank Niaga dan Bank Panin) dengan periode analisis tahun 2005-2011. Varibael yang digunakan meliputi ROA, ROE, LAR. LDR, NPL dan BOPO. Tujuan dari penelitian ini adalah melihat dan menganalisis perbedaan kinerja antara Bank BUMN dan BUSN yang go public di...

  8. Kondisi oral higiene dan karies gigi pada vegetarian dan non vegetarian di Maha Vihara Maitreya Medan

    OpenAIRE

    Prawira, Albert

    2011-01-01

    Perbedaan pola makan antara vegetarian dan non vegetarian dapat mempengaruhi kesehatan gigi dan mulut. Tujuan penelitian adalah untuk mengetahui kondisi oral higiene dan karies gigi pada umat vegetarian dan non vegetarian di Maha Vihara Maitreya Medan. Jenis penelitian adalah survei deskriptif. Sampel terdiri atas 74 vegetarian dan 65 non vegetarian. Pemeriksaan oral higiene dan karies gigi masing-masing menggunakan indeks OHIS Greene dan Vermillion dan indeks DMFT Klein, se...

  9. Modélisation des processus physiques et biologiques dans des fosses septiques et voies de valorisation des boues de vidange:Application à Bujumbura-Burundi

    OpenAIRE

    Nsavyimana, Gaston

    2014-01-01

    Dans les pays en développement (PED) en général et au Burundi en particulier, la problématique de gestion des eaux usées et des déchets solides constitue un enjeu majeur pour les spécialistes et les autorités locales. En effet, suite à un manque des stations d'épuration collectives au Burundi, les fosses septiques sont les plus utilisées pour gérer les eaux usées produites. Cependant, les processus qui s'y déroulent ne sont pas encore maîtrisés et la gestion des boues de vidange lorsque c...

  10. Pengembangan Model dan Media Pembelajaran Matematika Ekonomi dan Bisnis dengan Aplikasi Microsoft Mathematics

    Directory of Open Access Journals (Sweden)

    Mohammad Arief

    2015-09-01

    Full Text Available The purpose of this research was to produce: 1 Computer-assisted learning model (Computer Assisted Instruction/CAI using Microsoft Mathematics Application for task completion in the Economic Mathematic and Business course; 2 the development (production interactive multimedia for learning in Economic Mathematic and Business course; 3 Dissemination of results model development and learning media CAI into learning of the Economic Mathematic and Business course in the department of management Economics Faculty UM. The research method that used in this study is qualitative method with Class Action Research (CAR. To collecting data observation that are; 1 observation; 2 questionnaire; 3 photo documentation; 4 application. Research subject was student Management S-1 of academic years 2011/2012 on the odd semester of 2011/2012 who are taking Economic Mathematic and Business courses that are 43 students. The result of development model activities and learning media of Economic Mathematic and Business shown that even though they are beginner using this software, however its ease to use and better outcome expectation with the appropriate learning model, it’s very helpful to achieve learning objective of Economic Mathematic and Business course. Important suggestion is the time in mid semester examination or final semester examination in task completion should be use conventional way, because mastery concept of mathematic which associated and economic phenomena and business not all them can be explained through application program. Abstrak: Tujuan penelitian ini adalah untuk menghasilkan: 1 Model pembelajaran berbantuan komputer ( Computer Assisted Instruction / CAI dengan memanfaatkan Aplikasi Microsoft Mathematics untuk penyelesaian soal dalam mata kuliah Matematika Ekonomi dan Bisnis; 2 Pengembangan multimedia interaktif untuk pembelajaran mata kuliah Matematika Ekonomi dan Bisnis; 3 Diseminasi hasil pengembangan model dan media pembelajaran CAI ke

  11. IDE DAN DESAIN

    Directory of Open Access Journals (Sweden)

    Priscilia Yunita Wijaya

    1999-01-01

    Full Text Available We have seen many desain all around our everyday living. Design exist in the form of brochures%2C posters%2C banners%2C signages%2C book covers%2C and etcetera. Some are nice and easy to understand%2C some are ok%2C and some look like they are not fully develop and thought. A word that run across our mind whrn we enjoying a design is idea . A good design almost always associated with a good idea%2C is it tru? This paper is going to discuss about desain and its relationship to idea. Abstract in Bahasa Indonesia : Banyak desain yang diamati dalam kehidupan kita sehari-hari. Desain hadir dalam bentuk brosur%2C poster%2C spanduk%2C tanda-tanda%2C sampul buku%2C dan lain sebagainya. Ada beberapa yang bagus dan mudah untuk dimengerti%2C beberapa yang biasa%2C dan beberapa yang tampak asal dibuat. Sebuah kata yang terlintas dalam pemikiran kita dalam menikmati sebuah desain adalah ide . Sebuah desain yang baik selalu di identikan dengan ide yang baik%2C benarkah hal ini? Apakah desain dan apa hubungannya dengan ide akan dibahas pada tulisan ini.

  12. Application of neutron activation analysis to the study of impurities in molybdenum, tungsten and nuclear graphite; Application de l'analyse par activation neutronique a l'etude des impuretes dans le molybdene, le tungstene et le graphite nucleaire

    Energy Technology Data Exchange (ETDEWEB)

    Pinte, G [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1967-10-15

    A neutron activation method is described for the analysis of a maximum number of foreign elements in molybdenum, tungsten and graphite. The various elements are isolated using a systematic separation programme; the elements are subsequently analysed qualitatively and quantitatively using {gamma}-spectrometry. By this method are dosed 27 elements in molybdenum and tungsten, and 20 elements in graphite to which can be added those elements which are already the object of routine analysis: V, Mn, Si, P, S, Cl and 14 rare earths. (author) [French] On decrit une methode d'analyse par activation neutronique permettant de doser un maximum d'elements etrangers dans le molybdene, le tungstene et le graphite. En suivant un schema de separation systematique, on isole les differents elements dont les analyses qualitatives et quantitatives sont ensuite effectuees par spectrometrie {gamma}. Par cette methode, on dose 27 elements dans le molybdene et le tungstene, 20 elements dans le graphite, auxquels on peut encore ajouter les elements doses couramment: V, Mn, Si, P, S, Cl et 14 Terres Rares. (auteur)

  13. Evaluation de l'efficacité vis-à-vis du ruissellement de surface et des transferts latéraux dans le sol de différentes options de gestion utilisant (ou non) un couvert enherbé : Application en vue de limiter la contamination des eaux par les pesticides dans le contexte du Beaujolais viticole de coteaux

    OpenAIRE

    Gouy, V.; Peyrard, X.; Liger, L.

    2015-01-01

    / Cette étude apporte des éléments de réponse aux questions suivantes dans le contexte du Nord Beaujolais : - dans quelle mesure une zone tampon enherbée rivulaire recevant un ruissellement concentré de surface est-elle capable de réduire significativement le transfert des pesticides associés sans engendrer une contamination de nappe sous-jacente ? - dans quelle mesure une infiltration en amont en parcelle de vigne peut-elle contribuer à l'atténuation des transferts de pesticides ou engendrer...

  14. Danışma Hizmetlerinde Bulut Bilişim Uygulamalarının Kullanımı = Use of Cloud Computing Applications in Reference Services

    Directory of Open Access Journals (Sweden)

    Canan Tavluoğlu

    2014-12-01

    Full Text Available Bulut bilişim, herhangi bir yazılım ve depolama birimi olmaksızın, masaüstü-dizüstü bilgisayar, tablet PC veya akıllı telefonlar kullanılarak internet üzerinden bilgiye erişim sağlayan bir bilişim platformudur. Kütüphaneler gibi birçok kurum zamandan ve paradan tasarruf etmek için bu uygulamaları kullanmaktadır. Kütüphaneler danışma hizmetlerini yeni teknolojilere göre uyarlamakta ve hizmetlerini söz konusu bilişim ortamına taşımaktadır. Bu çalışmada bulut bilişimin tanımı, sunduğu fırsatlar ve zorluklardan kısaca bahsedilmekte ayrıca danışma hizmetlerinde bulut tabanlı uygulamaların nasıl kullanılabileceğine yer verilmektedir. Bu bağlamda Ankara’da bulunan üniversite kütüphanelerinde çalışan danışma kütüphanecilerinin bulut tabanlı yazılım olarak hizmet (Software as a Service - SaaS araçlarının ne ölçüde kullandıklarını belirlemek amacıyla bir anket uygulanmıştır. Anket sonuçlarına göre, danışma hizmetlerinde bu araçların kullanım oranlarının çok düşük olduğu görülmektedir. / Cloud computing is a computing platform that allows access the information over internet by using desktop computers, laptops, tablet PCs and smart phones without any software and storage unit. Many organizations use this technology and save time and money, such as libraries. Libraries have been adopting their reference services to the new technology and library services have been moving to the cloud. This paper defines cloud computing, presents the opportunities and challenges, also include how to use cloud based applications in reference services. A survey was applied to identify the use of cloud based Software as a Service (SaaS models by references librarians who work at university libraries in Ankara. According to results, the degree of usage of this tools generally low.

  15. Tekanan Metarhizium anisopliae dan Feromon terhadap Populasi dan Tingkat Kerusakan oleh Oryctes rhinoceros

    Directory of Open Access Journals (Sweden)

    Wtjaksono Witjaksono

    2015-12-01

    Full Text Available Oryctes rhinoceros is one of the most serious pests in coconut palm tree. Biological control for controlling the pest is done by applying fungal entomopathogen Metarhizium anisopliae on its breeding sites to infect the larvae. Recent development for controlling Oryctes beetle was including the use of pheromone trap baited with ethyl-4-methyl octanoic which attract both male and female of the Oryctes beetle. This research was aimed to determine the effect of combination of both entomopathogen and pheromone application on the population dynamics of rhinoceros beetle, and the intensity of leaf damage on coconut tree. For this purpose, a research was conducted in local farmer coconut tree in the Bojong Village, Panjatan District, Kulon Progo from June 2009−January 2010. Observation including leaf damage intensity before and after application, the number of adult beetle trapped by pheromone, and the number infected larvae in the breeding site. The result showed that there were significant differences among all treatments in term of intensity of leaf damage, the number of trapped adult beetle, and the number of larvae at the breeding site. Leaf damage on control, pheromone application, and combined treatment were: 4.73%; 1.08% and 0.65%. The number of trapped Rhinoceros beetle by ferotrap was 101; in combined treatment was 52. The number of M. anisopliae infected grub were 265 out of 281 total observed grub.   INTISARI Kerusakan tanaman kelapa akibat serangan Oryctes rhinoceros terjadi mulai pada tanaman muda. Mengingat besarnya kerugian yang ditimbulkan, maka perlu diupayakan cara pengendalian yang efisien, efektif dan aman bagi sumber daya alam dan lingkungan. Salah satu cara pengendalian secara hayati adalah dengan menggunakan cendawan patogenik Metarhizium anisopliae. Selain menggunakan cendawan, upaya terkini dalam mengendalikan kumbang badak adalah dengan menggunakan perangkap berferomon. Feromon dengan bahan aktif Etil-4-metil oktanoat dapat

  16. URGENSI DAN PROSPEK PENGATURAN (IUS CONSTITUENDUM UU TENTANG CONTEMPT OF COURT UNTUK MENEGAKKAN MARTABAT DAN WIBAWA PERADILAN

    Directory of Open Access Journals (Sweden)

    Lilik Mulyadi

    2015-07-01

    Full Text Available UU Contempt of Court merupakan kebutuhan yang bersifat urgent, segera dan mendesak, sehingga perlu dilakukan kajian dan penelitian secara kritis, akademis dan bersifat komprehensif untuk menjaga keluhuran dan menegakkan martabat dan wibawa peradilan.

  17. Capillary isotachophoresis with ESI-MS detection: Methodology for highly sensitive analysis of ibuprofen and diclofenac in waters

    Czech Academy of Sciences Publication Activity Database

    Malá, Zdeňka; Gebauer, Petr; Boček, Petr

    2016-01-01

    Roč. 907, FEB (2016), s. 1-6 ISSN 0003-2670 R&D Projects: GA ČR(CZ) GA13-05762S Institutional support: RVO:68081715 Keywords : isotachophoresis * mass spectrometric detection * Diclofenac * Ibuprofen Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.950, year: 2016

  18. UPLC/ESI-MS/MS analysis of compositional changes for organosulfur compounds in garlic (Allium sativum L.) during fermentation.

    Science.gov (United States)

    Kim, Sunyoung; Park, So-Lim; Lee, Sanghee; Lee, So-Young; Ko, Sungho; Yoo, Miyoung

    2016-11-15

    In this study, we used liquid chromatography coupled to ion trap mass spectrometry (MS) for the quantification of 11 organosulfur compounds and analysis of their compositional changes in garlic during fermentation using 3 different microbe strains. The calibration curves of all 11 analytes exhibited good linearity (R⩾0.995), and the mean recoveries measured at three concentrations were greater than 81.63% with relative standard deviations of less than 12.79%. Investigation of the compositional changes revealed that the γ-glutamyl peptides content in fermented blanched garlic reduced, whereas the content of the compounds in biosynthesis of S-allyl-l-cysteines from γ-glutamyl peptides increased significantly. Our results also indicated that starter cultures can be used selectively in the production of fermented garlic to increase the amounts of the desired organosulfur compounds. Copyright © 2016 Elsevier Ltd. All rights reserved.

  19. LC-ESI/MS/MS method for rapid screening and confirmation of 44 exogenous anabolic steroids in human urine.

    Science.gov (United States)

    Jeon, Byoung Wook; Yoo, Hye Hyun; Jeong, Eun Sook; Kim, Ho Jun; Jin, Changbae; Kim, Dong Hyun; Lee, Jaeick

    2011-09-01

    A sensitive and rapid method based on liquid chromatography-triple-quadrupole tandem mass spectrometry (LC-MS/MS) with electrospray ionization (ESI) has been developed and validated for the screening and confirmation of 44 exogenous anabolic steroids (29 parent steroids and 15 metabolites) in human urine. The method involves an enzymatic hydrolysis, liquid-liquid extraction, and detection by LC-MS/MS. A triple-quadrupole mass spectrometer was operated in positive ESI mode with selected reaction monitoring (SRM) mode for the screening and product ion scan mode for the confirmation. The protonated molecular ions were used as precursor ions for the SRM analysis and product ion scan. The intraday and interday precisions of the target analytes at concentrations of the minimum required performance levels for the screening were 2-14% and 2-15%, respectively. The limits of detection for the screening and confirmation method were 0.1-10 ng/mL and 0.2-10 ng/mL, respectively, for 44 steroids. This method was successfully applied to analysis of urine samples from suspected anabolic steroid abusers.

  20. Stability-indicating HPLC-DAD/UV-ESI/MS impurity profiling of the anti-malarial drug lumefantrine.

    Science.gov (United States)

    Verbeken, Mathieu; Suleman, Sultan; Baert, Bram; Vangheluwe, Elien; Van Dorpe, Sylvia; Burvenich, Christian; Duchateau, Luc; Jansen, Frans H; De Spiegeleer, Bart

    2011-02-28

    Lumefantrine (benflumetol) is a fluorene derivative belonging to the aryl amino alcohol class of anti-malarial drugs and is commercially available in fixed combination products with β-artemether. Impurity characterization of such drugs, which are widely consumed in tropical countries for malaria control programmes, is of paramount importance. However, until now, no exhaustive impurity profile of lumefantrine has been established, encompassing process-related and degradation impurities in active pharmaceutical ingredients (APIs) and finished pharmaceutical products (FPPs). Using HPLC-DAD/UV-ESI/ion trap/MS, a comprehensive impurity profile was established based upon analysis of market samples as well as stress, accelerated and long-term stability results. In-silico toxicological predictions for these lumefantrine related impurities were made using Toxtree® and Derek®. Several new impurities are identified, of which the desbenzylketo derivative (DBK) is proposed as a new specified degradant. DBK and the remaining unspecified lumefantrine related impurities are predicted, using Toxtree® and Derek®, to have a toxicity risk comparable to the toxicity risk of the API lumefantrine itself. From unstressed, stressed and accelerated stability samples of lumefantrine API and FPPs, nine compounds were detected and characterized to be lumefantrine related impurities. One new lumefantrine related compound, DBK, was identified and characterized as a specified degradation impurity of lumefantrine in real market samples (FPPs). The in-silico toxicological investigation (Toxtree® and Derek®) indicated overall a toxicity risk for lumefantrine related impurities comparable to that of the API lumefantrine itself.

  1. Simultaneous Determination of Sulphur metabolites in Arabidopsis thaliana via LC-ESI-MS/MS and 34S-metabolic Labelling

    NARCIS (Netherlands)

    Hsieh, Chin-Lin; Yeh, Kai-Wun; De Kok, Luit J.; Pan, Ryh-Nan; Kuo, Yueh-Hsiung; Tseng, Mei-Hwei

    2012-01-01

    Introduction Sulphur-containing metabolites play an important role in metabolism and homeostasis. Determination of these metabolites is challenging owing to their low concentrations and the interference in mass spectrometry analysis. Objective To develop a sensitive and accurate method based on

  2. Piper betle leaves: profiling phenolic compounds by HPLC/DAD-ESI/MS(n) and anti-cholinesterase activity.

    Science.gov (United States)

    Ferreres, Federico; Oliveira, Andreia P; Gil-Izquierdo, Angel; Valentão, Patrícia; Andrade, Paula B

    2014-01-01

    Piper betle L. is a widely distributed plant in the tropical and subtropical regions, its leaves being largely consumed as a masticator and mouth freshener. The purposes of this work were to characterise the phenolic profile of this species and to improve knowledge of its anti-cholinesterase properties. The phenolic composition of P. betle leaf aqueous and ethanol extracts was characterised by HPLC coupled with a diode-array detector and combined with electrospray ionisation tandem MS, and in vitro cholinesterase inhibitory capacity of both extracts was assessed by spectrophotometric microassays. The effect on neuronal cells (SH-SY5Y) viability was evaluated by 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide reduction and lactate dehydrogenase leakage. Twelve phenolic compounds, comprising a phenylpropanoid, five cinnamoyl and six flavonoids derivatives were identified in P. betle leaves. Hydroxychavicol was the major compound in both extracts; however, the aqueous extract presented a greater diversity of compounds. Both extracts showed strong activity against both acetyl- and butyrylcholinesterase, which can be due, at least partially, to the phenolic composition. Furthermore, the aqueous extract proved to be cytotoxic to human neuroblastoma cells at concentrations higher than 500 µg/mL. The results suggest that the consumption of P. betle leaves as an infusion can have a positive impact in the prevention and treatment of neurodegenerative diseases. Apigenin and luteolin derivatives are reported for the first time in this species. Copyright © 2014 John Wiley & Sons, Ltd.

  3. Combined HILIC-ELSD/ESI-MS(n) enables the separation, identification and quantification of sugar beet pectin derived oligomers.

    Science.gov (United States)

    Remoroza, C; Cord-Landwehr, S; Leijdekkers, A G M; Moerschbacher, B M; Schols, H A; Gruppen, H

    2012-09-01

    The combined action of endo-polygalacturonase (endo-PGII), pectin lyase (PL), pectin methyl esterase (fungal PME) and RG-I degrading enzymes enabled the extended degradation of methylesterified and acetylated sugar beet pectins (SBPs). The released oligomers were separated, identified and quantified using hydrophilic interaction liquid chromatography (HILIC) with online electrospray ionization ion trap mass spectrometry (ESI-IT-MS(n)) and evaporative light scattering detection (ELSD). By MS(n), the structures of galacturonic acid (GalA) oligomers having an acetyl group in the O-2 and/or O-3 positions eluting from the HILIC column were elucidated. The presence of methylesterified and/or acetylated galacturonic acid units within an oligomer reduced the interaction with the HILIC column significantly compared to the unsubstituted GalA oligomers. The HILIC column enables a good separation of most oligomers present in the digest. The use of ELSD to quantify oligogalacturonides was validated using pure GalA standards and the signal was found to be independent of the chemical structure of the oligomer being detected. The combination of chromatographic and enzymatic strategies enables to distinguish SBPs having different methylesters and acetyl group distribution. Copyright © 2012 Elsevier Ltd. All rights reserved.

  4. Screening for Proteolytic Activities in Snake Venom by Means of a Multiplexing ESI-MS Assay Scheme

    NARCIS (Netherlands)

    Liesener, A.; Perchuc, Anna-Maria; Schöni, Reto; Wilmer, Marianne; Karst, U.

    2005-01-01

    A multiplexed mass spectrometry based assay scheme for the simultaneous determination of five different substrate/product pairs was developed as a tool for screening of proteolytic activities in snake venom fractions from Bothrops moojeni. The assay scheme was employed in the functional

  5. Characterization of Flavonoid Glycosides from Fenugreek (Trigonella foenum-graecum Crude Seeds by HPLC–DAD–ESI/MS Analysis

    Directory of Open Access Journals (Sweden)

    Zakia Benayad

    2014-11-01

    Full Text Available Fenugreek (Trigonella foenum-graecum is a medicinal plant which is widely used for its pharmacological properties. In this study the phenolic composition of fenugreek crude seeds originating from Morocco has been investigated. Extraction was performed from defatted seeds by a hydromethanolic solution using an Accelerated Solvent Extractor. HPLC technique coupled to negative ion electrospray ionization mass spectrometry and diode array detection was employed to identify the polyphenol in the obtained extract. The obtained results allowed the detection of 32 phenolic compounds among which various flavonoid glycosides and phenolic acids have been tentatively identified on the basis of their UV and MS spectra, and comparisons with standards when available, as well as with literature data. A systematic study of the obtained MS spectra and the observed fragmentation showed that most of the identified compounds were acylated and non-acylated flavonoids with apigenin, luteolin and kaempferol as aglycons. Hydroxycinnamic acids mostly dominated by caffeic acid derivatives were also detected. The quantitative analysis of the identified compounds showed that the phenolic composition of the studied crude fenugreek seeds was predominantly acylated and non-acylated flavone derivatives with apigenin as the main aglycon.

  6. A quantitative analysis of the polyamine in lung cancer patient fingernails by LC-ESI-MS/MS.

    Science.gov (United States)

    Min, Jun Zhe; Matsumoto, Akihito; Li, Gao; Jiang, Ying-Zi; Yu, Hai-Fu; Todoroki, Kenichiro; Inoue, Koichi; Toyo'oka, Toshimasa

    2014-04-01

    A quantitative analysis of polyamines in lung cancer patient fingernails by the combination of 4-(N,N-dimethylaminosulfonyl)-7-fluoro-2,1,3-benzoxadiazole derivatives and liquid chromatography-electrospray ionization tandem mass spectrometry is described. The reaction of the reagent with eight kinds of polyamines, that is, N(1) -acetylputrescine (N(1) -actPUT), N(8) -acetylspermidine, N(1) -acetylspermine, 1,3-diaminopropane, putrescine (PUT), cadaverine, spermidine and spermine (SPM) effectively occurs at 60 °C for 30 min. The detection limits (signal-to-noise ratio 5) were 5-100 fmol. A good linearity was achieved from the calibration curves, which was obtained by plotting the peak area ratios of the analytes relative to the internal standard (IS), that is, 1,6-diaminohexane, vs the injected amounts of polyamines (r(2)  > 0.996), and the intra-day and inter-day assay precisions were group, as compared with the healthy volunteers, the concentrations of SPM had a statistically significant (p < 0.05) correlation. Therefore, because the proposed method provides a good mass accuracy and the trace detection of the polyamines in human fingernails, this analytical technique could be a noninvasive technique to assist in the diagnosis and assessment of disease activity in lung cancer patients. Copyright © 2013 John Wiley & Sons, Ltd.

  7. Collagen Peptides from Crucian Skin Improve Calcium Bioavailability and Structural Characterization by HPLC-ESI-MS/MS.

    Science.gov (United States)

    Hou, Tao; Liu, Yanshuang; Guo, Danjun; Li, Bo; He, Hui

    2017-10-11

    The effects of collagen peptides (CPs), which are derived from crucian skin, were investigated in a retinoic acid-induced bone loss model. The level of serum bone alkaline phosphatase (BALP) in the model group (117.65 ± 4.66 units/L) was significantly higher than those of the other three groups (P group. In addition, the bone mineral density in the 600 mg of CPs/kg group was significantly higher (femur, 0.37 ± 0.02 g/cm 2 ; tibia, 0.33 ± 0.02 g/cm 2 ) than in the model group (femur, 0.26 ± 0.01 g/cm 2 ; tibia, 0.23 ± 0.02 g/cm 2 ). The morphology results indicated bone structure improved after the treatment with CPs. Structural characterization demonstrated that Glu, Lys, and Arg play important roles in binding calcium and promoting calcium uptake. Our results indicated that CPs could promote calcium uptake and regulate bone formation.

  8. Critical Conditions for Liquid Chromatography of Statistical Copolymers: Functionality Type and Composition Distribution Characterization by UP-LCCC/ESI-MS.

    Science.gov (United States)

    Epping, Ruben; Panne, Ulrich; Falkenhagen, Jana

    2017-02-07

    Statistical ethylene oxide (EO) and propylene oxide (PO) copolymers of different monomer compositions and different average molar masses additionally containing two kinds of end groups (FTD) were investigated by ultra high pressure liquid chromatography under critical conditions (UP-LCCC) combined with electrospray ionization time-of flight mass spectrometry (ESI-TOF-MS). Theoretical predictions of the existence of a critical adsorption point (CPA) for statistical copolymers with a given chemical and sequence distribution1 could be studied and confirmed. A fundamentally new approach to determine these critical conditions in a copolymer, alongside the inevitable chemical composition distribution (CCD), with mass spectrometric detection, is described. The shift of the critical eluent composition with the monomer composition of the polymers was determined. Due to the broad molar mass distribution (MMD) and the presumed existence of different end group functionalities as well as monomer sequence distribution (MSD), gradient separation only by CCD was not possible. Therefore, isocratic separation conditions at the CPA of definite CCD fractions were developed. Although the various present distributions partly superimposed the separation process, the goal of separation by end group functionality was still achieved on the basis of the additional dimension of ESI-TOF-MS. The existence of HO-H besides the desired allylO-H end group functionalities was confirmed and their amount estimated. Furthermore, indications for a MSD were found by UPLC/MS/MS measurements. This approach offers for the first time the possibility to obtain a fingerprint of a broad distributed statistical copolymer including MMD, FTD, CCD, and MSD.

  9. Determination of cysteinyl leukotrienes in exhaled breath condensate: Method combining immunoseparation with LC-ESI-MS/MS

    Czech Academy of Sciences Publication Activity Database

    Syslová, K.; Kačer, P.; Vilhanová, B.; Kuzma, Marek; Lipovová, P.; Fenclová, Z.; Lebedová, J.; Pelclová, D.

    2011-01-01

    Roč. 879, č. 23 (2011), s. 2220-2228 ISSN 1570-0232 R&D Projects: GA MZd NS10298 Keywords : Cysteinyl leukotriene * Exhaled breath condensate * Immunoseparation Subject RIV: CE - Biochemistry Impact factor: 2.888, year: 2011

  10. LC-PDA-ESI/MS Identification of the Phenolic Components of Three Compositae Spices: Chamomile, Tarragon, and Mexican Arnica

    Science.gov (United States)

    Chamomile (Matricaria chamomilla L.), tarragon (Artemisia dracunculus L.) and Mexican arnica (Heterotheca inuoides) are common compositae spices and herbs found in the US market. They contain flavonoids and hydroxycinnamates that are potentially beneficial to human health. A standardized LC-PDA-ESI...

  11. Frequency-Modulated Continuous Flow Analysis Electrospray Ionization Mass Spectrometry (FM-CFA-ESI-MS) for Sample Multiplexing.

    Science.gov (United States)

    Filla, Robert T; Schrell, Adrian M; Coulton, John B; Edwards, James L; Roper, Michael G

    2018-02-20

    A method for multiplexed sample analysis by mass spectrometry without the need for chemical tagging is presented. In this new method, each sample is pulsed at unique frequencies, mixed, and delivered to the mass spectrometer while maintaining a constant total flow rate. Reconstructed ion currents are then a time-dependent signal consisting of the sum of the ion currents from the various samples. Spectral deconvolution of each reconstructed ion current reveals the identity of each sample, encoded by its unique frequency, and its concentration encoded by the peak height in the frequency domain. This technique is different from other approaches that have been described, which have used modulation techniques to increase the signal-to-noise ratio of a single sample. As proof of concept of this new method, two samples containing up to 9 analytes were multiplexed. The linear dynamic range of the calibration curve was increased with extended acquisition times of the experiment and longer oscillation periods of the samples. Because of the combination of the samples, salt had little effect on the ability of this method to achieve relative quantitation. Continued development of this method is expected to allow for increased numbers of samples that can be multiplexed.

  12. The differences in matrix effect between supercritical fluid chromatography and reversed phase liquid chromatography coupled to ESI/MS.

    Science.gov (United States)

    Svan, Alfred; Hedeland, Mikael; Arvidsson, Torbjörn; Pettersson, Curt E

    2018-02-13

    For many sample matrices, matrix effects are a troublesome phenomenon using the electrospray ionization source. The increasing use of supercritical fluid chromatography with CO 2 in combination with the electrospray ionization source for MS detection is therefore raising questions: is the matrix effect behaving differently using SFC in comparison with reversed phase LC? This was investigated using urine, plasma, influent- and effluent-wastewater as sample matrices. The matrix effect was evaluated using the post-extraction addition method and through post-column infusions. Matrix effect profiles generated from the post-column infusions in combination with time of flight-MS detection provided the most valuable information for the study. The combination of both qualitative and semi-quantitative information with the ability to use HRMS-data for identifying interfering compounds from the same experiment was very useful, and has to the authors' knowledge not been used this way before. The results showed that both LC and SFC are affected by matrix effects, however differently depending on sample matrix. Generally, both suppressions and enhancements were seen, with a higher amount of enhancements for LC, where 65% of all compounds and all sample matrices were enhanced, compared to only 7% for SFC. Several interferences were tentatively identified, with phospholipids, creatinine, and metal ion clusters as examples of important interferences, with different impact depending on chromatographic technique. SFC needs a different strategy for limiting matrix interferences, owing to its almost reverse retention order compared to RPLC. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. The determination of 22 natural brassinosteroids in a minute sample of plant tissue by UHPLC-ESI-MS/MS

    Czech Academy of Sciences Publication Activity Database

    Tarkowská, Danuše; Novák, Ondřej; Oklešťková, Jana; Strnad, Miroslav

    2016-01-01

    Roč. 408, č. 24 (2016), s. 6799-6812 ISSN 1618-2642 R&D Projects: GA MŠk(CZ) LO1204; GA MŠk LK21306; GA ČR GA14-34792S Institutional support: RVO:61389030 Keywords : Brassinosteroids * Solid-phase extraction * Ultra-high performance liquid chromatography Subject RIV: EB - Genetics ; Molecular Biology Impact factor: 3.431, year: 2016

  14. Análise de fármacos em águas por SPE-UPLC-ESI-MS/MS

    Directory of Open Access Journals (Sweden)

    Vanessa de Jesus Gaffney

    2014-01-01

    Full Text Available A method was developed for the analysis of 31 pharmaceutical compounds in Lisbon's drinking water system, using solid-phase extraction (SPE and ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS. The method was validated through estimation of the linearity range, method detection and quantification limits, matrix effects, precision and accuracy. The method detection and quantification limit ranges were 0.009-10 and 0.03-33 ng/L, respectively. Analytes were quantified in water samples collected from the EPAL (Empresa Portuguesa das Águas Livres S.A. supply system. Carbamazepine, atenolol, sulfadiazine, sulfamethazine, sulfapyridine, sulfamethoxazole, acetaminophen, caffeine and erythromycin were quantified in the analysed samples.

  15. Novel tyrosine phosphorylation sites in rat skeletal muscle revealed by phosphopeptide enrichment and HPLC-ESI-MS/MS

    DEFF Research Database (Denmark)

    Zhang, Xiangmin; Højlund, Kurt; Luo, Moulun

    2012-01-01

    Tyrosine phosphorylation plays a fundamental role in many cellular processes including differentiation, growth and insulin signaling. In insulin resistant muscle, aberrant tyrosine phosphorylation of several proteins has been detected. However, due to the low abundance of tyrosine phosphorylation (...

  16. Trace analysis of antidepressant pharmaceuticals and their select degradates in aquatic matrixes by LC/ESI/MS/MS

    Science.gov (United States)

    Schultz, M.M.; Furlong, E.T.

    2008-01-01

    Treated wastewater effluent is a potential environmental point source for antidepressant pharmaceuticals. A quantitative method was developed for the determination of trace levels of antidepressants in environmental aquatic matrixes using solid-phase extraction coupled with liquid chromatography- electrospray ionization tandem mass spectrometry. Recoveries of parent antidepressants from matrix spiking experiments for the individual antidepressants ranged from 72 to 118% at low concentrations (0.5 ng/L) and 70 to 118% at high concentrations (100 ng/L) for the solid-phase extraction method. Method detection limits for the individual antidepressant compounds ranged from 0.19 to 0.45 ng/L. The method was applied to wastewater effluent and samples collected from a wastewater-dominated stream. Venlafaxine was the predominant antidepressant observed in wastewater and river water samples. Individual antidepressant concentrations found in the wastewater effluent ranged from 3 (duloxetine) to 2190 ng/L (venlafaxine), whereas individual concentrations in the waste-dominated stream ranged from 0.72 (norfluoxetine) to 1310 ng/L (venlafaxine). ?? 2008 American Chemical Society.

  17. Sunscreen Agents in the Environment: Determination by HPLC-ESI-MS/MS and GC-MS and Calculation of Phototoxicity

    Science.gov (United States)

    Ultraviolet (UV) filters, also known as sunscreen agents, are chemicals widely used in cosmetics, sunscreens, and plastics to block UV radiation from the sun. There have been studies that show some sunscreen agents demonstrate estrogenicity and multiple hormonal activities in vi...

  18. Analysis of Arsenicals and their Sulfur Analogs Using HPLC with Collision Cell ICP-MS and ESI-MS

    Science.gov (United States)

    Recent metabolic and exposure assessment studies have found sulfur analogs (thioarsenicals) of common oxoarsenicals in environmental and biological systems. The occurrence of thioarsenicals raises questions regarding their origin and transport, and their roles in metabolism of a...

  19. Identification and semi-quantification of biogenic organic nitrates in ambient particulate matters by UHPLC/ESI-MS

    Science.gov (United States)

    Li, Rui; Wang, Xinfeng; Gu, Rongrong; Lu, Chunying; Zhu, Fanping; Xue, Likun; Xie, Huijun; Du, Lin; Chen, Jianmin; Wang, Wenxing

    2018-03-01

    Particulate biogenic organic nitrates (PBONs) are important components of secondary organic aerosols and play an important role in the tropospheric atmosphere chemistry. However, the concentrations and the chemistry of PBONs remain poorly understood due to the lack of accurate measurement techniques on specific organic nitrates. In this study, ultra high performance liquid chromatography/electrospray mass spectrometry was applied in detection of individual PBONs in ambient atmosphere. Total five kinds of PBONs were identified in PM2.5 samples collected in urban Ji'nan in spring according to characteristic fragments of NO2, NO3, HNO3, CO2, and H2O, including monoterpene hydroxyl nitrate (MW = 215, MHN215), pinene keto nitrate (MW = 229, PKN229), limonene di-keto nitrate (MW = 247, LDKN247), oleic acid keto nitrate (MW = 359, OAKN359), and oleic acid hydroxyl nitrate (MW = 361, OAHN361). Among them, three kinds of PBONs originated from biogenic volatile organic compounds of pinene and limonene and two kinds of PBONs came from chemical conversion of oleic acid. The concentrations of these PBONs were roughly quantified with surrogate standards of (1R,2R,5R)-(+)-2-hydroxy-3-pinanone and ricinoleic acid. The average concentrations of MHN215, PKN229, LDKN247, OAKN359, and OAHN361 were 111.6 ± 23.0, 93.1 ± 49.6, 55.3 ± 7.4, 23.4 ± 14.5, 36.8 ± 18.3 ng m-3, respectively. The total concentration of these PBONs was 325.4 ± 116.7 ng m-3, contributing to 1.64 ± 0.34‰ of PM2.5.

  20. Characterization of Flavonoid Glycosides from Fenugreek (Trigonella foenum-graecum) Crude Seeds by HPLC–DAD–ESI/MS Analysis

    Science.gov (United States)

    Benayad, Zakia; Gómez-Cordovés, Carmen; Es-Safi, Nour Eddine

    2014-01-01

    Fenugreek (Trigonella foenum-graecum) is a medicinal plant which is widely used for its pharmacological properties. In this study the phenolic composition of fenugreek crude seeds originating from Morocco has been investigated. Extraction was performed from defatted seeds by a hydromethanolic solution using an Accelerated Solvent Extractor. HPLC technique coupled to negative ion electrospray ionization mass spectrometry and diode array detection was employed to identify the polyphenol in the obtained extract. The obtained results allowed the detection of 32 phenolic compounds among which various flavonoid glycosides and phenolic acids have been tentatively identified on the basis of their UV and MS spectra, and comparisons with standards when available, as well as with literature data. A systematic study of the obtained MS spectra and the observed fragmentation showed that most of the identified compounds were acylated and non-acylated flavonoids with apigenin, luteolin and kaempferol as aglycons. Hydroxycinnamic acids mostly dominated by caffeic acid derivatives were also detected. The quantitative analysis of the identified compounds showed that the phenolic composition of the studied crude fenugreek seeds was predominantly acylated and non-acylated flavone derivatives with apigenin as the main aglycon. PMID:25393509

  1. Simultaneous determination of phenolic acids and flavonoids in Chenopodium formosanum Koidz. (djulis) by HPLC-DAD-ESI-MS/MS.

    Science.gov (United States)

    Hsu, B Y; Lin, S W; Inbaraj, B Stephen; Chen, B H

    2017-01-05

    A high performance liquid chromatography-diode array detection-tandem mass spectrometry method (HPLC-DAD-MS/MS) was developed for simultaneous determination of phenolic acids and flavonoids in djulis (Chenopodium formosanum Koidz.), a traditional Chinese herb reported to possess vital biological activities. A high yield of phenolic acids and flavonoids was attained by employing 50% ethanol in water as the extraction solvent and shaking in a 60°C water bath for 3h. A total of 8 phenolic acids and 14 flavonoids were separated and identified within 55min by using a Poroshell 120 EC-C18 column with detection at 280nm, flow rate at 0.8mL/min, column temperature at 35°C, and a gradient solvent system of 0.1% formic acid in water and acetonitrile. Two internal standards caffeic acid and kaempferol-3-O-rutinoside were used for quantitation of phenolic acids and flavonoids in djulis respectively. The amounts of phenolic acids ranged from 11.5±0.8μg/g (caffeoyl-putrescine-derivative (2)) to 1855.3±16.9μg/g (hydroxylphenylacetic acid pentoside), while the flavonoids ranged from 19.93±2.29μg/g (quercetin-3-O-(coumaryl)-rutinoside-pentoside (1)) to 257.3±2.05μg/g (rutin-O-pentoside (2)). A high recovery (89.68-97.20%) and high reproducibility was obtained for both phenolic acids and flavonoids with the relative standard deviation (RSD) for the latter ranging from 0.09-8.22% (intra-day variability) and 0.80-8.48% (inter-day variability). This method may be applied to determination of both phenolic acids and flavonoids in food products and Chinese herbs. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Quantification of monosialogangliosides in human plasma through chemical derivatization for signal enhancement in LC–ESI-MS

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Qianyang; Liu, Danting [Clinical Chemistry Program, Department of Chemistry, Cleveland State University, 2121 Euclid Avenue, Cleveland, OH 44115 (United States); Xin, Baozhong; Cechner, Karen [DDC Clinic, Center for Special Needs Children, 14567 Madison Road, Middlefield, OH 44062 (United States); Zhou, Xiang [Clinical Chemistry Program, Department of Chemistry, Cleveland State University, 2121 Euclid Avenue, Cleveland, OH 44115 (United States); Wang, Heng, E-mail: Wang@ddcclinic.org [DDC Clinic, Center for Special Needs Children, 14567 Madison Road, Middlefield, OH 44062 (United States); Zhou, Aimin, E-mail: a.zhou@csuohio.edu [Clinical Chemistry Program, Department of Chemistry, Cleveland State University, 2121 Euclid Avenue, Cleveland, OH 44115 (United States); Center for Gene Regulation in Health and Diseases, Cleveland State University, 2121 Euclid Avenue, Cleveland, OH 44115 (United States)

    2016-07-27

    Gangliosides are found in abundance in the central nervous system of vertebrates. Their metabolic disruption and dysfunction are associated with various neurodegenerative disorders such as Alzheimer's disease and Parkinson's disease. In order to improve our understanding of the etiology of these diseases, analytical ganglioside assays with sufficient specificity and sensitivity in relevant biological matrices are required. In the present work we have developed and validated a reverse-phase ultra-performance liquid chromatography (UPLC)/tandem mass spectrometry (MS) method for determining monosialogangliosides GM1, GM2, and GM3 present in human plasma. Compared with our previous method, this method enhanced, by 15 fold, MS responses of the analytes by employing 2-(2-Pyridilamino)-ethylamine (PAEA) & 4-(4, 6-Dimethoxy-1, 3, 5-triazin-2-yl)-4-methylmorpholinium chloride (DMTMM)-based derivatization. The analytes and internal standards were derivatized with PAEA&DMTMM after extraction from plasma using a protein precipitation procedure. They were then purified using liquid–liquid partitioning. When the samples were then analyzed by UPLC-MS/MS with a multiple reaction monitoring (MRM) mode, we achieved superior sensitivity and specificity. This method was evaluated for extraction recovery, calibration linearity, precision, accuracy, and lower limit of quantification (LLOQ). The validated method was successfully applied to monitor monosialoganglioside levels in the plasma from patients with GM3 synthase deficiency. With significantly increased sensitivity, we have, for the first time, detected a significant amount of GM3 in the affected patients. - Highlights: • A UPLC/MS/MS method for analyzing monosialogangliosides GM1, GM2, and GM3 in human plasma was developed and validated. • PAEA&DMTMM-based derivatization greatly improved the sensitivity. • The method was applied to measure GM1, GM2, and GM3 in the plasma from the patients with GM3 synthase deficiency. • GM3 was detected, for the first time, at a significant amount in the patients with GM3 synthase deficiency.

  3. A Novel Approach to Detect Accelerated Aged and Surface-Mediated Degradation in Explosives by UPLC-ESI-MS.

    Energy Technology Data Exchange (ETDEWEB)

    Beppler, Christina L [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

    2015-12-01

    A new approach was created for studying energetic material degradation. This approach involved detecting and tentatively identifying non-volatile chemical species by liquid chromatography-mass spectrometry (LC-MS) with multivariate statistical data analysis that form as the CL-20 energetic material thermally degraded. Multivariate data analysis showed clear separation and clustering of samples based on sample group: either pristine or aged material. Further analysis showed counter-clockwise trends in the principal components analysis (PCA), a type of multivariate data analysis, Scores plots. These trends may indicate that there was a discrete shift in the chemical markers as the went from pristine to aged material, and then again when the aged CL-20 mixed with a potentially incompatible material was thermally aged for 4, 6, or 9 months. This new approach to studying energetic material degradation should provide greater knowledge of potential degradation markers in these materials.

  4. Characterization of the Human Skeletal Muscle Proteome by One-dimensional Gel Electrophoresis and HPLC-ESI-MS/MS

    DEFF Research Database (Denmark)

    Højlund, Kurt; Yi, Zhengping; Hwang, Hyonson

    2008-01-01

    and pathophysiological conditions. However, to date, the number of proteins identified by this approach has been limited, with 107 different proteins being the maximum reported so far. Using a combination of one-dimensional gel electrophoresis and high performance liquid chromatography electrospray ionization tandem...... muscle. Mitochondrial proteins accounted for 22% of all proteins identified, including 55 subunits of the respiratory complexes I-V. Moreover, a number of enzymes involved in endocrine and metabolic signaling pathways as well as calcium homeostasis were identified. These results provide the most...

  5. LC-ESI-MS/MS Identification of Polar Lipids of Two Thermophilic Anoxybacillus Bacteria Containing a Unique Lipid Pattern

    Czech Academy of Sciences Publication Activity Database

    Řezanka, Tomáš; Kambourova, M.; Derekova, A.; Kolouchová, I.; Sigler, Karel

    2012-01-01

    Roč. 47, č. 7 (2012), s. 729-739 ISSN 0024-4201 R&D Projects: GA ČR(CZ) GAP503/11/0215 Institutional support: RVO:61388971 Keywords : Anoxybacillus * Plasmalogens * O-Aminoacylphosphatidylglycerols Subject RIV: CE - Biochemistry Impact factor: 2.557, year: 2012

  6. Epistemologi dan Keterbatasan Teori Gravitasi

    Directory of Open Access Journals (Sweden)

    Erwin Erwin

    2017-08-01

    Full Text Available Peristiwa tentang kecenderungan jatuhnya benda-benda menuju pusat bumi dan keteraturan peredaran planet dan benda-benda langit lainnya dalam tata surya dahulu dianggap dua fenomena yang berbeda. Mekanika benda langit dan mekanika bumi yang sebelumnya merupakan dua pengetahuan yang terpisah, dianggap satu kesatuan oleh Sir Isaac Newton. Newton mengemukakan hukum gravitasi umum yaitu gaya tarik menarik antara dua benda besarnya sebanding dengan massa masing-masing benda dan berbanding terbalik dengan kuadrat jarak antara kedua benda. Hukum gravitasi ini sukses menjalaskan bagaimana benda cendrung jatuh menuju pusat bumi dan peredaran planet dan benda-benda langit lain mengelilingi matahari dalam sistem tata surya. Namun hukum gravitasi Newton ternyata tidak sepenuhnya tepat, beberapa hal dapat dijelaskan dengan hukum relativitas Einstein, namun demikian hukum relativitas Einstein juga dicurigai masih perlu diamandemen agar dapat menjelaskan fenomena alam dengan tepat.

  7. EPISTEMOLOGI DAN KETERBATASAN TEORI GRAVITASI

    Directory of Open Access Journals (Sweden)

    Erwin Erwin

    2017-08-01

    Full Text Available Peristiwa tentang kecenderungan jatuhnya benda-benda menuju pusat bumi dan keteraturan peredaran planet dan benda-benda langit lainnya dalam tata surya dahulu dianggap dua fenomena yang berbeda. Mekanika benda langit dan mekanika bumi yang sebelumnya merupakan dua pengetahuan yang terpisah, dianggap satu kesatuan oleh Sir Isaac Newton. Newton mengemukakan hukum gravitasi umum yaitu gaya tarik menarik antara dua benda besarnya sebanding dengan massa masing-masing benda dan berbanding terbalik dengan kuadrat jarak antara kedua benda. Hukum gravitasi ini sukses menjalaskan bagaimana benda cendrung jatuh menuju pusat bumi dan peredaran planet dan benda-benda langit lain mengelilingi matahari dalam sistem tata surya. Namun hukum gravitasi Newton ternyata tidak sepenuhnya tepat, beberapa hal dapat dijelaskan dengan hukum relativitas Einstein, namun demikian hukum relativitas Einstein juga dicurigai masih perlu diamandemen agar dapat menjelaskan fenomena alam dengan tepat.

  8. ISLAM DAN RADIKALISME: Upaya Antisipasi dan Penanggulangannya

    Directory of Open Access Journals (Sweden)

    Idrus Ruslan

    2017-02-01

    Full Text Available Sejak tragedi pemboman WTC tanggal 11 September 2001 yang disusul dengan rangkaian peledakan bom di sejumlah negara, banyak orang non Muslim yang berasumsi bahwa ajaran Islam identik dengan radikalisme. Walaupun assumsi yang berkembang itu dapat dimaklumi, namun keyakinan tersebut tentu saja tidak sepenuhnya benar. Karena meskipun terdapat sekelompok orang Islam yang berbuat radikal, akan tetapi mayoritas Muslim justru bertentangan dengan mereka. Lagi pula, jika dicermati secara mendalam, sesungguhnya Islam sama sekali tidak mentolerir tindakan radikal. Ia adalah agama kasih sayang yang sangat mendodrong penganutnya untuk berbuat baik terhadap orang lain, termasuk kepada orang-orang non-Muslim. Artikel ini menawarkan beberapa upaya strategis dalam mengantisipasi dan menanggulangi bahaya radikalisme-terorisme.

  9. PENERAPAN HYGIENE DAN SANITASI DI PASTRY HOTEL HILTON BANDUNG

    Directory of Open Access Journals (Sweden)

    Verena Widya Pertiwi

    2016-05-01

    Full Text Available Abstract - Application of hygiene and sanitation in Hilton Hotel Bandung is important thing to note in the process of implementation. This is done to prevent food contamination of food that cab be caused by several factors such as, human, work area, kitchen utensil, material strorage systems and product. Because of this determination of standarts personal hygiene, area and utensil must be done correcly so that each product is safe for consumption. Authors on the basis of these issues are very keen to examine and make a final project with the title “application of hygiene and sanitation in the Hilton Hotel Bandung”. Research carried out by several methode of observation, interview and the latter is the study of documents. The research was conducted at the Hilton Hotel Bandung, for 6 months. The study was conducted as one of the requiremants for the final session of college exams Bina Sarana Informatika university Bandung. Based on the result of research and discussion conducted, authors concluded that the presence of load application staandard of hygiene and sanitation in hotel can improve the standard of health, hygiene and quality of a product when it is done in accordance with existing procedures. Key word : Hygiene and sanitation pastry hotel. Abstraksi - Penerapan hygiene dan sanitasi di Hotel Hilton Bandung merupakan upaya penting yang harus diperhatikan dalam proses pelaksanannya. Hal ini dilakukan untuk mencegah terjadinya kontaminasi makanan yang dapat disebabkan oleh beberapa faktor seperti manusia, area kerja, peralatan, sistem penyimpanan bahan dan produk. Penentuan standar kebersihan personal, area kerja maupun peralatan harus dilakukan dengan tepat dan benar agar setiap produk yang dihasilkan oleh bagian pastry hotel aman untuk dikonsumsi. Atas dasar persoalan di atas penulis sangat tertarik untuk menelitinya dan membuat tugas akhir dengan judul “ Penerapan Hygiene dan Sanitasi di Hotel Hilton Bandung ”. Metode penelitian

  10. DIVERSITAS DAN KERAPATAN MANGROVE, GASTROPODA DAN BIVALVIA DI ESTUARI PERANCAK, BALI

    OpenAIRE

    Susiana; Ali, Syamsu Alam; Rukminasari, Nita

    2011-01-01

    Penelitian ini bertujuan membandingkan diversitas dan kerapatan mangrove dengan kepadatan gastropoda dan bivalvia di mangrove alami dan rehabilitasi. Pengukuran ekosistem mangrove menggunakan transek kuadrat 10 m x 10 m. Kelimpahan dan kepadatan gastropoda dan bialvia menggunakan transek kuadrat berukuran 1 m x 1 m. Analisis nMDS, cluster untuk melihat hubungan karekteristik mangrove alami dan rehabilitasi dianalisis secara deskriptif dan analisis regresi untuk mendetermi...

  11. Les possibilités des turbines de détente dans les industries gazière et pétrolière Application of Expansion Turbines in the Gas and Oil Industry

    Directory of Open Access Journals (Sweden)

    Verneau A.

    2006-11-01

    Full Text Available Utilisées depuis longtemps dans l'industrie cryogénique, les turbines de détente voient leur intérêt augmenter actuellement en tant que turbines de récupération de l'énergie des laminages. Cette énergie peut servir à l'entraînement de compresseurs, pompes ou générateurs électriques. Il existe surtout des turbines dans la gamme de 200 à 20 000 ch. Deux types principaux sont développés : les turbines axiales et les turbines radiales. Les particularités techniques et les domaines d'emploi de chaque type sont discutés. Ue intérêt particulier est porté au domaine des petites puissances (de 100 kW jusqu'à quelques centaines de watts. L'évolution du rendement en fonction de la puissance est étudiée et quelques types spéciaux bien adaptés à cette gamme, tels que les turbines périphériques, sont présentés. Quelques indications sur la récupération de l'énergie des liquides par turbines sont également données. Ensuite, plusieurs exemples d'applications sont exposés tels que : récupération de fractions condensables du gaz naturel (butane, propane, éthane, récupération de gaz perdu, récupération de l'énergie des laminages lors de la distribution et au niveau des stockages souterrains, turbine hydraulique de lavage de gaz, récupération de l'énergie des fumées de cracking catalytique, entraînement de petits générateurs électriques dans la gamme de quelques kilowatts à quelques centaines de watts. Enfin, nous abordons la technologie et les dispositions constructives particulières en nous attachant plus spécialement aux problèmes de régulation, étanchéité, paliers. Des techniques nouvelles telles que l'emploi de paliers à gaz et leurs avantages sont décrites. Les difficultés dues aux basses températures et à la condensation sont examinées. Nous terminons par quelques considérations d'ordre économique destinées à prévoir la rentabilité d'une installation de récupération d

  12. DAKWAH DAN PEMBERDAYAAN PEREMPUAN

    Directory of Open Access Journals (Sweden)

    Siti Nurmahyati

    2017-02-01

    Full Text Available Da’wah is an attempt to persuade and influence others in realizing the teachings of Islam, to achieve worldly prosperity and welfare of the hereafter. The success was fueled by propaganda aspects are interrelated, anatara preachers, propaganda material, propaganda strategy, mad’u (target da’wah. The number of women in this country nearly half of people (49.36. therefore, it is important to empower women in da’wah to build their own people in consciousness and religious activities that provide the basics of life prosperous world and hereafter.   Dakwah merupakan suatu upaya untuk mengajak dan mempengaruhi orang lain dalam merealisasikan ajaran Islam, untuk mencapai tujuan kesejahteraan duniawi maupun kesejahteraan ukhrawi. Keberhasilan tersebut pun dipicu oleh berbagai aspek dakwah yang saling terkait, antara juru dakwah, materi dakwah, strategi dakwah, mad’u (sasaran dakwah. Jumlah kaum perempuan di negara ini hampir mencapai separuh dari jumlah masyarakatnya (49,36. Oleh karena itu, sangat penting sekali pemberdayaan perempuan dalam dakwah untuk membangun kaumnya sendiri dalam kesadaran dan aktivitas-aktivitas keagamaan yang memberikan dasar kehidupan sejahtera duniawi dan ukhrawi.

  13. ASIMETRI INFORMASI DAN UNDERPRICING

    Directory of Open Access Journals (Sweden)

    Tety Anggita Safitri

    2013-03-01

    Full Text Available Tujuan penelitian ini adalah untuk menguji pengaruh asimetri informasi terhadap underpricing. Penelitian ini menggunakan sampel 63 perusahaan yang melakukan penawaran umum perdana di Bursa Efek Indonesia dalam kurun waktu 2005-2010. Analisis data menggunakan regresi linier berganda, yaitu menguji proksi asimetri informasi yang terdiri atas ukuran perusahaan, umur perusahaan, proporsi saham yang ditawarkan kepada masyarakat, reputasi underwriter dan reputasi auditor terhadap underpricing. Hasil penelitian ini mengindikasikan bahwa reputasi underwriter dan reputasi auditor berpengaruh terhadap underpricing. Ukuran perusahaan, umur perusahaan dan proporsi saham yang ditawarkan tidak berpengaruh terhadap underpricing.The aim of this research is to examine the effect of assymetric information on underpricing. This research used a sample of 63 companies that make initial public offering on the Indonesia Stock Exchange in the period of 2005-2010. The data analysis is using multiple linear regression, which is testing the proxy of asymmetric information which consists of the firm size, the firm age, the proportion of shares offered to the public, underwriter reputation and auditor reputation on underpricing. This research indicates that underwriter reputation and auditor reputation have a significant effect on underpricing. The firm size, the firm age and the proportion of shares offered to the public have no significant effect on underpricing.

  14. The application of radioactive isotopes to the study of motion of silt and pebbles in the rivers and in the sea; Application des isotopes radioactifs a l'etude des mouvements des sediments et des galets dans les cours d'eau et en mer

    Energy Technology Data Exchange (ETDEWEB)

    Hours, R [Commissariat a l' Energie Atomique, Saclay (France).Centre d' Etudes Nucleaires; Jaffry, P [Electricite de France (EDF), 78 - Chatou (France). Lab. National d' Hydraulique

    1959-07-01

    The application of radioactive tracers to the study of sediments drift has received considerable attention since 1954 in various countries. A comparative review is made of a number of techniques of labelling, immersing and detecting silts, sands, and pebbles. The influence of the burying of the active material is emphasized. The different experiments which have been so far carried out are described. (author) [French] L'application des traceurs radioactifs a l'etude des deplacements de sediments a fait depuis 1954 l'objet de travaux nombreux dans divers pays. On passe en revue et on compare differentes techniques de marquage, d'immersion et de detection des vases, sables et galets; on insiste sur l'influence de l'enfouissement du materiau actif. On decrit les differentes experiences effectuees jusqu'a ce jour. (auteur)

  15. DAMPAK NEGATIF PERKEMBANGAN TEKNOLOGI INFORMATIKA DAN KOMUNIKASI DAN CARA ANTISIFASINYA

    Directory of Open Access Journals (Sweden)

    I Gede Ratnaya

    2011-03-01

    Full Text Available Sampai saat ini perkembangan ilmu pengetahuan telah menghantarkan masyarakat menuju babak baru yaitu babak yang memanfaatkan peralatan-peralatan yang merupakan hasil dari teknologi. Penggunaan tenaga manusia yang semakin hari semakin kecil volumenya sering kali menyebabkan orang kehilangan pekerjaannya karena tugasnya telah tergantikan oleh peralatan atau mesin. Sebagai sarana penyampaian informasi dan komunikasi, komputer bisa dipakai sebagai sarana berinternetan. Lewat internet orang bisa mencari bermacam-macam informasi dan berkomunikasi. Peran yang dapat diberikan oleh aplikasi teknologi informasi ini adalah mendapatkan informasi untuk kehidupan pribadi seperti informasi tentang kesehatan, hobi, rekreasi, dan rohani. Selain memberikan keuntungan, ternyata peralatan teknologi informasi dan komunikasi juga memberikan dampak negatif bagi penggunanya. Dampak negatif tersebut muncul sebagai akibat dari penggunaan yang salah atau tidak bertanggung jawab dari yang menggunakan. Beberapa dampak negatif tersebut adalah 1. Anak lebih banyak menghabiskan waktu menonton TV ketimbang melakukan hal lainnya (seperti belajar dan olah raga, 2. Anak kehilangan kemampuan berbaur dengan masyarakat dan cenderung nyaman dengan kehidupan online, 3 Adanya pelanggaran hak cipta, 4.  Kejahatan di internet, 5. Penyebaran virus komputer, dan 6. Pornografi, perjudian, penipuan, tayangan kekerasan. Adapun cara mengatasi dampak-dampak negatif tersebut adalah : 1. Gunakan teknologi untuk menjalin hubungan dengan orang yang sudah dikenal, 2. Cari komunitas positif  yang sering melakukan pertemuan didunia nyata, 3. Perlunya penegakkan hukum yang berlaku dengan dibentuknya polisi internet, 4. Menghindari pemakaian telepon seluler yang berfitur canggih oleh anak-anak dibawah umur dan lebih mengawasi penggunaan telepon seluler, 5. Perbanyak membaca buku-buku yang bersifat edukatif dan bersifat keimanan serta aplikasi komputer yang bersifat mendidik, dan 6. Perlunya pengaturan

  16. KETERGANTUNGAN ONLINE GAME DAN PENANGANANNYA

    Directory of Open Access Journals (Sweden)

    Ridwan Syahran

    2015-06-01

    Full Text Available Penelitian ini dimaksudkan untuk mengetahui perilaku yang ditimbulkan dari kecanduan bermaian online game pada siswa SMP Negeri 1 Palu yang meliputi faktor-faktor penyebab kecanduan, keadaan psikologis yang ditimbulkan dari kecanduan bermain online game dan dampak-dampak yang ditimbulkan dari kecanduan bermain online game.Pendekatan penelitian ini adalah penelitian kualitatif dengan jenis penelitian studi kasus dengan berdasarkan responden dan informan sebagai bahan sumber data. Dalam proses pengumpulan data digunakan teknik observasi dan wawancara, dimana setelah data diperoleh selanjutnya dianalisis dengan menggunakan analisis deskriptif kualitatif.Berdasarkan hasil penelitian ini, bahwa subyek (RZ dan (MT, kedua subyek penelitian menjadi ketergantungan atau kecanduan untuk bermain online game yang dikarenakan tersedianya beberapa fasilitas pendukung untuk bermain game di rumah, adanya faktor sosial dari pertemanan dengan teman bermain dan keingintahuan yang sangat besar terhadap suatu jenis game. Penanganan ketergantungan game online dengan bantuan dari berbagai pihak terutama pihak sekolah memberikan kepercayaan kepada konselor sekolah atau guru BK untuk mengadakan seminar kepada orang tua siswa tentang game online dan masalah yang akan ditimbulkan, mengatur waktu belajar dan bermain anak, memasukkan materi tentang game online dan dampaknya kepada siswa serta memberikan penyaluran yang baik dalam memilih game yang edukatif serta Menjalin komunikasi interpersonal agar anak dapat terbuka dengan orang tua.

  17. Measurements and Application of Partition Coefficients of Compounds Suitable for Tracing Gas Injected Into Oil Reservoirs Mesures et applications des coefficients de partage de composants utilisables comme gaz traceurs injectés dans des réservoirs de pétrole

    Directory of Open Access Journals (Sweden)

    Dugstad O.

    2006-11-01

    Full Text Available Tracing of injection gas in oil reservoirs is a technique used to improve the description of permeability distributions in situ. Results from dynamic laboratory experiments of gas tracers are reported. Gas tracers are delayed when flooding through a reservoir by the partitioning into the oil phase. A knowledge of this effect is important to optimize the interpretation of field tracer tests. The partition is quantified by the partition coefficient K. Two chemical tracers perfluoromethylcyclopentane (PMCP and perfluoromethylcyclohexane (PMCH and the radioactive 14C labelled ethane have been studied here. The two chemical compounds are new as reservoir tracers and no field results with these tracers are reported in the open literature. Our group has, however, recently applied these compound successfully as tracers in a North Sea reservoir. Les traceurs représentent un outil précieux pour améliorer la description des gisements. On les a utilisés pour obtenir des renseignements sur la configuration de l'écoulement des fluides injectés et sur leur vitesse, sur l'instant de percé des venues d'eau et sur leur origine précise, sur les traitements d'amélioration du balayage, sur les hétérogénéités importantes telles que fractures, barrières d'écoulement et stratifications de la perméabilité. Dans les gisements importants comportant plusieurs puits de production et plusieurs puits d'injection, il est donc souhaitable de disposer de plusieurs traceurs afin de pouvoir injecter différents traceurs ou mélanges de traceurs dans les différents puits. L'article présenté ici est une contribution a l'effort fait pour étendre le nombre de gaz traceurs fiables applicables aux gisements. L'article présente les résultats d'essais dynamiques en laboratoires dans lesquels on injecte des traceurs à travers un milieu poreux. Lorsqu'ils traversent un réservoir, les gaz traceurs sont retardés du fait de leur ségrégation dans la phase huile. La

  18. Determination of correction coefficients for quantitative analysis by mass spectrometry. Application to uranium impurities analysis; Recherche des coefficients de correction permettant l'analyse quantitative par spectrometrie de masse. Application a l'analyse d'impuretes dans l'uranium

    Energy Technology Data Exchange (ETDEWEB)

    Billon, J P [Commissariat a l' Energie Atomique, Bruyeres-le-Chatel (France). Centre d' Etudes

    1970-07-01

    Some of basic principles in spark source mass spectrometry are recalled. It is shown how this method can lead to quantitative analysis when attention is paid to some theoretical aspects. A time constant relation being assumed between the analysed solid sample and the ionic beam it gives we determined experimental relative sensitivity factors for impurities in uranium matrix. Results being in fairly good agreement with: an unelaborate theory on ionization yield in spark-source use of theoretically obtained relative sensitivity factors in uranium matrix has been developed. (author) [French] Apres avoir rappele quelques principes fondamentaux regissant la spectrometrie de masse a etincelles, nous avons montre que moyennant un certain nombre de precautions, il etait possible d'utiliser cette methode en analyse quantitative. Ayant admis qu'il existait une relation constante dans le temps entre l'echantillon solide analyse et le faisceau ionique qui en est issu, nous avons d'abord entrepris de determiner des coefficients de correction experimentaux pour des matrices d'uranium. Les premiers resultats pratiques semblant en accord avec une theorie simple relative au rendement d'ionisation dans la source a etincelles, nous avons etudie la possibilite d'appliquer directement les coefficients theoriques ainsi definis, l'application etant toujours faite sur des matrices d'uranium. (auteur)

  19. The n,{gamma} discrimination in recoil-proton proportional counters. Application to the measurement of fast neutron spectra; Discrimination n,{gamma} dans les compteurs proportionnels a protons de recul. Application a la mesure des spectres de neutrons rapides

    Energy Technology Data Exchange (ETDEWEB)

    Jeandidier, C [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1969-07-01

    A description is given of a spectrometry chain working in the energy range of a few keV to 1 MeV, and designed for measurement of fast neutron spectra. It consists of detectors, recoil proton proportional counters built especially for this work by R. COMTE (DEG/SER) and which make it possible to cover the energy range and also associated electronic equipment. A brief description is first given of the physical processes involved: (n,p) collisions in the gas, influence of {gamma} radiation; the method of discrimination is then presented. It is based on the difference in the rise-times of the pulses. In the experiments described here the use of a bi-parametric system made it possible to employ the most simple discrimination device, based on the fact that the high frequency gamma pulse components are, at a given energy, weaker than those of the neutron pulses. Results are given of measurements carried out on the Van der Graaff (mono-energetic neutrons for testing the linearity of the chain and the resolving power of the counters), and of those made in a sub-critical system Hug at Cadarache. (author) [French] On decrit une chaine de spectrometrie travaillant dans le domaine d'energie de quelques keV a 1 MeV destinee a la mesure des spectres de neutrons rapides. Elle comprend les detecteurs, compteurs proportionnels a protons de recul, realises specialement pour cette etude par M. R. COMTE (DEG/SER), permettant de couvrir la gamme d'energie et l'electronique associee. Apres un rappel des processus physiques mis en jeu: chocs (n,p) dans les gaz, influence des rayonnements {gamma}, on expose la methode de discrimination utilisee. Celle-ci est basee sur la difference des temps de montee des impulsions. Au cours des experiences rapportees ici, la mise en oeuvre d'un ensemble bi-parametrique a permis d'utiliser le dispositif de discrimination le plus simple, base sur la remarque que les composantes a haute frequence des impulsions {gamma} sont, a energie egale, plus faibles

  20. The n,{gamma} discrimination in recoil-proton proportional counters. Application to the measurement of fast neutron spectra; Discrimination n,{gamma} dans les compteurs proportionnels a protons de recul. Application a la mesure des spectres de neutrons rapides

    Energy Technology Data Exchange (ETDEWEB)

    Jeandidier, C. [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1969-07-01

    A description is given of a spectrometry chain working in the energy range of a few keV to 1 MeV, and designed for measurement of fast neutron spectra. It consists of detectors, recoil proton proportional counters built especially for this work by R. COMTE (DEG/SER) and which make it possible to cover the energy range and also associated electronic equipment. A brief description is first given of the physical processes involved: (n,p) collisions in the gas, influence of {gamma} radiation; the method of discrimination is then presented. It is based on the difference in the rise-times of the pulses. In the experiments described here the use of a bi-parametric system made it possible to employ the most simple discrimination device, based on the fact that the high frequency gamma pulse components are, at a given energy, weaker than those of the neutron pulses. Results are given of measurements carried out on the Van der Graaff (mono-energetic neutrons for testing the linearity of the chain and the resolving power of the counters), and of those made in a sub-critical system Hug at Cadarache. (author) [French] On decrit une chaine de spectrometrie travaillant dans le domaine d'energie de quelques keV a 1 MeV destinee a la mesure des spectres de neutrons rapides. Elle comprend les detecteurs, compteurs proportionnels a protons de recul, realises specialement pour cette etude par M. R. COMTE (DEG/SER), permettant de couvrir la gamme d'energie et l'electronique associee. Apres un rappel des processus physiques mis en jeu: chocs (n,p) dans les gaz, influence des rayonnements {gamma}, on expose la methode de discrimination utilisee. Celle-ci est basee sur la difference des temps de montee des impulsions. Au cours des experiences rapportees ici, la mise en oeuvre d'un ensemble bi-parametrique a permis d'utiliser le dispositif de discrimination le plus simple, base sur la remarque que les composantes a haute frequence des impulsions {gamma} sont, a

  1. Mass spectrometer introduction line: application to the analysis of impurities in uranium hexafluoride; Ligne d'introduction pour spectrometre de masse: application a l'analyse des impuretes contenues dans l'UF{sub 6}

    Energy Technology Data Exchange (ETDEWEB)

    Besson, M. [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires. Departement de physico-chimie, service des isotopes stables, section de spectrometrie de masse

    1967-01-01

    The continuous mass-spectrometric analysis of impurities in UF{sub 6} is possible industrially if certain conditions imposed by the nature of the gas are respected. The gas introduction line arriving at the spectrometer's source makes it possible to fix the flow-rate, to control the inlet pressure and to selectively destroy the gas containing the impurities. The operational conditions for the line are defined and a description is given of the theoretical and experimental study of the various elements of which it is composed, i.e. the leak valve, the flow-meter, the chemical trap and the servo-mechanism making it possible to regulate and control the gas flow. The dynamic characteristics of the line's various components and the performance of the equipment in the case of the analyses considered are given. (author) [French] L'analyse en continu par spectrometrie de masse des impuretes contenus dans l'UF{sub 6} est possible industriellement moyennant certaines conditions imposees par la nature du gaz. La ligne d'introduction des gaz dans la source du spectrometre permet de regler le debit, de controler la pression d'introduction et de detruire selectivement le gaz porteur d'impuretes. Les conditions de fonctionnement de la ligne etant definies, on decrit l'etude theorique et experimentale des differents elements qui la composent, c'est-a-dire: le robinet a fuite, le debitmetre, le piege chimique et l'ensemble d'asservissement permettant la regulation et le controle du debit. On donne les caracteristiques dynamiques des differents constituants de la ligne et les performances de l'ensemble pour les analyses considerees. (auteur)

  2. Mass spectrometer introduction line: application to the analysis of impurities in uranium hexafluoride; Ligne d'introduction pour spectrometre de masse: application a l'analyse des impuretes contenues dans l'UF{sub 6}

    Energy Technology Data Exchange (ETDEWEB)

    Besson, M [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires. Departement de physico-chimie, service des isotopes stables, section de spectrometrie de masse

    1967-01-01

    The continuous mass-spectrometric analysis of impurities in UF{sub 6} is possible industrially if certain conditions imposed by the nature of the gas are respected. The gas introduction line arriving at the spectrometer's source makes it possible to fix the flow-rate, to control the inlet pressure and to selectively destroy the gas containing the impurities. The operational conditions for the line are defined and a description is given of the theoretical and experimental study of the various elements of which it is composed, i.e. the leak valve, the flow-meter, the chemical trap and the servo-mechanism making it possible to regulate and control the gas flow. The dynamic characteristics of the line's various components and the performance of the equipment in the case of the analyses considered are given. (author) [French] L'analyse en continu par spectrometrie de masse des impuretes contenus dans l'UF{sub 6} est possible industriellement moyennant certaines conditions imposees par la nature du gaz. La ligne d'introduction des gaz dans la source du spectrometre permet de regler le debit, de controler la pression d'introduction et de detruire selectivement le gaz porteur d'impuretes. Les conditions de fonctionnement de la ligne etant definies, on decrit l'etude theorique et experimentale des differents elements qui la composent, c'est-a-dire: le robinet a fuite, le debitmetre, le piege chimique et l'ensemble d'asservissement permettant la regulation et le controle du debit. On donne les caracteristiques dynamiques des differents constituants de la ligne et les performances de l'ensemble pour les analyses considerees. (auteur)

  3. Application of resistivity measurements to research on structural elements in the Nord-Limousin (France) uraniferous basin (1960); Application des mesures de resistivite a la recherche des elements structuraux dans le bassin uranifere du Nord-Limousin (France) (1960)

    Energy Technology Data Exchange (ETDEWEB)

    Sarcia, J A; Bonnet, J; Combe, R [Commissariat a l' Energie Atomique, Saclay (France).Centre d' Etudes Nucleaires

    1960-07-01

    The authors discuss the difficulties encountered in the exploration of a typical deposit in the Nord-Limousin, using the resistivity measurement method. In the zone in question the over-thrust was very variable and difficult to predict. The uraniferous deposits had two types of aspect, the passage from one to the other being often very sudden: long thin veins without gangue; short and thick lens-shape deposits which were strongly contaminated by clay towards their edges. After several unsatisfactory attempts, the device known as the 'rectangular map' was adopted and gave an acceptable structural representation rapidly and cheaply. For the placing of the probes however, methods are required which are more refined and sensitive. It is in any case useless to expect to obtain a satisfactory representation and a sufficient accuracy using a single technique; especially in the region under consideration. (author) [French] Les auteurs exposent les difficultes rencontrees pour l'exploration, par la methode des mesures de resistivite, d'un gisement type du Nord-Limousin: il s'agissait d'une zone a recouvrement tres variable et difficilement previsible. Les occurences uraniferes y affectaient deux facies passant brutalement de l'un a l'autre: longs filonnets minces et sans gangue; lentilles courtes et puissantes avec alteration argileuses tres etendue aux epontes. Apres plusieurs essais peu satisfaisants, le dispositif dit 'carte des rectangles' a ete adopte pour obtenir rapidement et a bon compte un schema structural suffisant. Mais des methodes plus fines et plus sensibles sont necessaires pour guider l'implantation des sondages. Il est d'ailleurs vain d'esperer trouver a la fois la representativite d'ensemble et la precision, dans l'utilisation d'une seule technique, surtout dans la region envisagee. (auteur)

  4. GAMBARAN JENIS DAN JUMLAH KONSUMSI FAST FOOD DAN SOFT DRINK PADA MAHASISWA OBESITAS DI UNIVERSITAS HASANUDDIN

    OpenAIRE

    Suryanti, Rut; Jafar, Nurhaedar; Syam, Aminuddin

    2013-01-01

    Konsumsi fast food dan soft drink dapat menyebabkan kelebihan berat badan dan obesitas.Penelitian ini bertujuan untuk mengetahui gambaran jenis dan jumlah zat gizi makro dari konsumsi fast food dan soft drink pada mahasiswa yang obesitas.Jenis penelitian adalah deskriptif, dilaksanakan pada bulan Mei-Juni 2013 di Universitas Hasanuddin dengan jumlah responden 60 orang. Instrument penelitian adalah kuesioner identitas diri dan food frekuensiSemiQuantitatif fast food dan soft drink, food pictur...

  5. PERSEPSI DAN TRANSFORMASI VISI DAN MISI PADA CIVITAS AKADEMIKA STAIN PEKALONGAN

    Directory of Open Access Journals (Sweden)

    Imam Khanafi

    2013-05-01

    Full Text Available Penelitian ini mengukur tingkat persepsi visi dan misi civitas akademika STAIN Pekalongan, dan mengukur juga tingkat implementasi sebagai transformasi visi misi tersebut serta menemukan hubungan antara persepsi dengan implementasinya. Kajian ini memiliki signifikan yang strategis dalam konteks manajemen dan pengembangan Pendidikan di STAIN Pekalongan dan lembaga pendidikan lainnya. Hal ini karena posisi visi dan misi sebagai kerangka acuan (frame of reference yang mengarahkan dan menjelaskan kepada keseluruh unsur civitas akademika dalam setiap program kerjanya.

  6. SISTEM PENGOLAHAN AIR ASAM TAMBANG PADA WATER POND DAN APLIKASI MODEL ENCAPSULATION IN-PIT DISPOSAL PADA WASTE DUMP TAMBANG BATUBARA (Acid Mine Drainage Treatment System in Water Pond and Application of Encapsulation In-Pit Disposal Model in Waste Dump

    Directory of Open Access Journals (Sweden)

    Andy R. Erwin Wijaya

    2010-03-01

    Full Text Available ABSTRAK Kegiatan pertambangan batubara umumnya dapat menimbulkan dampak negatif terhadap lingkungan di lokasi penambangan. Salah satu dampak negatif yang signifikan adalah terjadinya pencemaran air asam tambang yang dapat merusak fungsi lingkungan seperti komponen air dan tanah. Umumnya lokasi tambang batubara yang berpotensi besar sebagai sumber terbentuknya air asam tambang adalah kolam penampungan air tambang (water pond dan tempat penimbunan material buangan sulfida (waste dump. Penelitian ini bertujuan untuk mengendalikan rembesan air asam tambang yang berasal dari kolam penampungan air (water pond dan mengurangi terbentuknya air asam tambang pada tempat penimbunan material buangan sulfida (waste dunp. Sistem pengendalian pencemaran air asam tambang meliputi pengolahan air asam tambang (water pond dan pengelolaan material sulfida (waste dump. Metode pengolahan air asam tambang adalah menetralisasi air asam dengan reagen alkali. Reagen alkali yang paling efektif dan ekonomis adalah batugamping (kalsium karbonat. Jumlah batugamping yang dibutuhkan untuk menetralkan air asam lambang pada water pond (5040 m3 sebesar 104,56 kg. Pengelolaan material buangan sulfida (waste dump adalah menerapkan model encapsulation in-pit disposal. Hal ini sangat efektif untuk mencegah terbentuknya air asam tambang. Material perlapisan yang digunakan adalah lempung (clay, karena mempunyai nilai permeabilitas yang sangat kecil yaitu sebesar 2,3148 x 10-9 m/det dan ketersediaannya mencukupi.   ABSTRACT Coal mining activity generally can generate negative impact to environment on mining location. One of the negative impact is contamination of acid mine drainage which able to destroy environment and ecosystem as water and soil. High potency source of acid mine drainage formed on coal mining location are water pond and waste dump. This aim of the research are control of acid mine drainage from water pond and prevention of acid mine drainage formed on the waste dump

  7. Perancangan dan Analisis Redistribution Routing Protocol OSPF dan EIGRP

    Directory of Open Access Journals (Sweden)

    DWI ARYANTA

    2016-02-01

    Full Text Available Abstrak OSPF (Open Shortest Path First dan EIGRP (Enhanced Interior Gateway Routing Protocol adalah dua routing protokol yang banyak digunakan dalam jaringan komputer. Perbedaan karakteristik antar routing protokol menimbulkan masalah dalam pengiriman paket data. Teknik redistribution adalah solusi untuk melakukan komunikasi antar routing protokol. Dengan menggunakan software Cisco Packet Tracer 5.3 pada penelitian ini dibuat simulasi OSPF dan EIGRP yang dihubungkan oleh teknik redistribution, kemudian dibandingkan kualitasnya dengan single routing protokol EIGRP dan OSPF. Parameter pengujian dalam penelitian ini adalah nilai time delay dan trace route. Nilai trace route berdasarkan perhitungan langsung cost dan metric dibandingkan dengan hasil simulasi. Hasilnya dapat dilakukan proses redistribution OSPF dan EIGRP. Nilai delay redistribution lebih baik 1% dibanding OSPF dan 2-3% di bawah EIGRP tergantung kepadatan traffic. Dalam perhitungan trace route redistribution dilakukan 2 perhitungan, yaitu cost untuk area OSPF dan metric pada area EIGRP. Pengambilan jalur utama dan alternatif pengiriman paket berdasarkan nilai cost dan metric yang terkecil, hal ini terbukti berdasarkan perhitungan dan simulasi. Kata kunci: OSPF, EIGRP, Redistribution, Delay, Cost, Metric. Abstract OSPF (Open Shortest Path First and EIGRP (Enhanced Interior Gateway Routing Protocol are two routing protocols are widely used in computer networks. Differences between the characteristics of routing protocols pose a problem in the delivery of data packets. Redistribution technique is the solution for communication between routing protocols. By using the software Cisco Packet Tracer 5.3 in this study were made simulating OSPF and EIGRP redistribution linked by technique, then compared its quality with a single EIGRP and OSPF routing protocols. Testing parameters in this study is the value of the time delay and trace route. Value trace route based on direct calculation of cost

  8. Pembuatan Aplikasi Web Manajemen Laundry dan Integrasi Data dengan Web Service

    Directory of Open Access Journals (Sweden)

    Refika Khoirunnisa

    2016-01-01

    Full Text Available Selama ini banyak dari perusahaan di bidang jasa laundry masih menggunakan pencatatan secara manual seperti menggunakan buku, sehingga setiap data tidak terintegrasi secara waktu-nyata. Oleh sebab itu, perlu dibuat penelitian untuk merancang sebuah sistem terkomputerisasi yang dapat mempermudah pencatatan dan pengolahan data keuangan laundry. Pembuatan Aplikasi Web Manajemen Laundry menggunakan bahasa pemrograman PHP, HTML, CSS, JavaScript dan basisdata MySQL sebagai tempat penyimpanan data. Aplikasi ini merupakan aplikasi yang terintegrasi dengan aplikasi melalui sebuah teknologi yang disebut web service. Aplikasi Web Manajemen Laundry dikembangkan dengan menggunakan metode RAD (Rapid Application Development yang terdiri dari tahap perencanaan kebutuhan, proses perancangan, implementasi, dan tahap pengujian. Dari hasil penelitian dapat disimpulkan bahwa Aplikasi Web Manajemen Laundry memiliki fitur yang berfungsi untuk mempermudah pencatatan dan pengolahan data secara akurat dan waktu-nyata. Fitur-fitur utama dari aplikasi ini diantaranya adalah pengolahan data transaksi, pengeluaran, dan laporan laba/rugi. Dalam menunjang fitur-fitur utama agar dapat bekerja dengan baik maka terdapat fitur pendukung yaitu pengolahan data pelanggan dan data pengguna aplikasi. Berdasarkan pengujian dengan menggunakan metode black-box, seluruh fungsi menu yang ada dalam aplikasi web telah berhasil dan berjalan sesuai dengan kebutuhan.

  9. REENGINEERING PROSES BISNIS : TINJAUAN KONSEPTUAL DAN METODOLOGI

    Directory of Open Access Journals (Sweden)

    Lena Ellitan

    1999-01-01

    Full Text Available Business process reengineering is fundamental rethinking and radical redesign of an organization's business processes that leads the organization to achieve dramatic improvement in business performance. Many firms have successfully embraced this new innovation paradigm to achieve orders of magnitude improvements in cost, eficiency, quality and value. Even more firms are seeking opportunities to apply reengineering and methodologies to assist them in doing so. The recognition of reengineering as a new management paradigm emerged in the 1990's, though it may be argued that the principle of reengineering has been applied well before then. The early 1990's saw world wide interest in reengineering. Consequently, many organizations have reported their first-cycle experiences in reengineering. Reengineering practices in the period of the 1990's was largerly characterized by application to operational processes and emphasis on operational measure of time, cost, and quality. Quite recently, a more strategic flavor of reengineering has been advocated. One of the hopes of new thinking is that by trancending microscopic concern of operational strategy, it would help the organization derive significantly greater value out of the reengineering effort. This paper presents: 1. The concept of reengineering 2. Various problems in business process reengineering. 3. The rigorous methodology for organizing reengineering activities. Abstract in Bahasa Indonesia : Reengineering proses bisnis adalah pemikiran ulang fundamental dan disain ulang radikal suatu proses bisnis organisasi yang akan mengarahkan organisasi untuk mencapai peningkatan kinerja bisnis secara dramatis. Beberapa perusahaan telah menerapkan paradigma inovasi baru ini untuk mencapai berbagai perbaikan dalam biaya, kualitas, dan efisiensi. Bahkan makin banyak perusahaan yang mencari peluang untuk menerapkan proyek reengineering dan metodologi-metodologi yang membantu mereka dalam mencapai usaha

  10. Computer Applications in Counselor Education: Developing Cultural Competencies Through Online Collaboration of Future School Counselors / L’informatique dans l’éducation des orienteurs : le développement du savoir-faire culturel par la collaboration en

    Directory of Open Access Journals (Sweden)

    Vessela Ilieva

    2012-07-01

    Full Text Available This study examined the applications of computer-mediated student collaboration in a graduate multicultural counseling course. The course work included a reflective cultural competency building assignment that utilized online communication and collaboration using a wiki to extend and improve students’ multicultural counseling and social justice advocacy skills. The online assignment design was aligned with the current call for utilizing technology in the counseling profession. It further considered the needs of the future counselors, the current levels of exposure to and experience with available technology of the class members, and the opportunities for utilization of a variety of online-based tools to extend in-class and out-of-class discussions. Students’ response to this new form of class work and communication confirmed the potential of the online component to other aspects of counselor preparation, and the data analysis showed that the computer-mediated assignment was a valuable addition to developing students’ skills as multiculturally competent professionals. Cette étude a examiné les applications de la collaboration entre étudiants par l’entremise de l’informatique dans le cadre d’un cours d’études supérieures sur l’orientation en contexte multiculturel. Les travaux du cours comprenaient un travail de réflexion pour renforcer le savoir-faire culturel grâce à la communication et à la collaboration en ligne, en utilisant un wiki pour accroître et améliorer les aptitudes des étudiants en orientation en contexte multiculturel et en défense de la justice sociale. La conception du travail en ligne s’alignait sur la tendance actuelle pour une utilisation accrue de la technologie dans le métier de conseiller en orientation. On y tenait également compte des besoins des futurs conseillers, de leur degré d’exposition à la technologie et de leur expérience avec celle-ci, ainsi que des occasions pour l

  11. GESTION DES FLUX ÉNERGÉTIQUE DANS UN SYSTÈME PHOTOVOLTAÏQUE AVEC STOCKAGE CONNECTER AU RÉSEAU – Application à l'habitat

    OpenAIRE

    Riffonneau , Yann

    2009-01-01

    The work done during this thesis contributes to the intensive penetration of the photovoltaic electricity production into the electric grid. Photovoltaic energy holds an immense potential, in particular in the housing sector, but intermittent nature limits its large scale development. In this thesis, we propose to add a storage element to the grid connected photovoltaic system (housing application). First, we introduce the notion of energy management in these systems called « hybrids systems ...

  12. Ionization techniques in capillary electrophoresis-mass spectrometry: principles, design, and application.

    Science.gov (United States)

    Hommerson, Paul; Khan, Amjad M; de Jong, Gerhardus J; Somsen, Govert W

    2011-01-01

    A major step forward in the development and application of capillary electrophoresis (CE) was its coupling to ESI-MS, first reported in 1987. More than two decades later, ESI has remained the principal ionization technique in CE-MS, but a number of other ionization techniques have also been implemented. In this review the state-of-the-art in the employment of soft ionization techniques for CE-MS is presented. First the fundamentals and general challenges of hyphenating conventional CE and microchip electrophoresis with MS are outlined. After elaborating on the characteristics and role of ESI, emphasis is put on alternative ionization techniques including sonic spray ionization (SSI), thermospray ionization (TSI), atmospheric pressure chemical ionization (APCI), atmospheric pressure photoionization (APPI), matrix-assisted laser desorption ionization (MALDI) and continuous-flow fast atom bombardment (CF-FAB). The principle of each ionization technique is outlined and the experimental set-ups of the CE-MS couplings are described. The strengths and limitations of each ionization technique with respect to CE-MS are discussed and the applicability of the various systems is illustrated by a number of typical examples. Copyright © 2011 Wiley Periodicals, Inc.

  13. Pengaruh Perebusan, Penggaraman Dan Penjemuran Pada Udang Dan Cumi Terhadap Pembentukan 7 Ketokolesterol

    Directory of Open Access Journals (Sweden)

    Rudi Riyanto

    2007-12-01

    Full Text Available Penelitian pengaruh perebusan, penggaraman dan penjemuran pada udang dan cumi terhadap pembentukan 7‑ketokolesterol telah dilakukan. Dalam penelitian ini, udang dan cumi masing ­masing dibagi dalam dua kelompok. Pada kelompok pertama diberikan perlakuan perebusan dalam air, dan pada kelompok kedua diberikan perlakuan perebusan dalam air garam (3% air garam untuk udang dan 20% air garam untuk cumi. Setelah perebusan, dilakukan pengeringan di bawah matahari (udang dikupas dahulu sebelum dijemur. Pengambilan sampel dilakukan saat kondisi segar, setelah direbus dan setelah dijemur. Pengamatan dilakukan terhadap kandungan 7‑ketokolesterol, kolesterol, nilai TBA, dan kadar air. Hasil penelitian menunjukkan bahwa perebusan, penggaraman dan penjemuran berpengaruh terhadap pembentukan 7‑ketokolesterol sampai konsentrasi 20,82 ppm pada udang dan 15,05 ppm pada cumi sebagai konsentrasi tertinggi produk hasil oksidasi kolesterol yang terbentuk. Penelitian ini dapat dijadikan bukti bahwa pemanasan (perebusan dan penjemuran, serta penggaraman berpengaruh dalam proses oksidasi kolesterol pada udang dan cumi.

  14. Profil Sensori dan Nilai Gizi Beberapa Jenis Ikan Patin dan Hibrid Nasutus

    Directory of Open Access Journals (Sweden)

    Theresia Dwi Suryaningrum

    2010-11-01

    Full Text Available Penelitian mengenai profil sensori dan nilai gizi filet patin Siam (Pangasius hypopthalmus, Jambal (Pangasius djambal Bleeker, Pasupati, Nasutus serta hasil silangan Siam dan Nasutus (hibrid Nasutus telah dilakukan. Analisis sensori dilakukan dengan uji pembeda menyeluruh, uji pembeda atribut, uji kesukaan, dan uji rangking. Pengamatan lainnya dilakukan terhadap edible portion dan nilai gizi (proksimat dan profil asam amino. Hasil penelitian menunjukkan bahwa filet patin hibrid Nasutus lebih memiliki kesamaan warna dengan filet patin Nasutus daripada filet patin Siam. W arna daging filet patin hibrid Nasutus berbeda nyata dengan induknya yaitu patin Nasutus dan patin Siam. Panelis lebih menyukai warna filet patin hibrid Nasutus dibandingkan dengan patin Pasupati. Patin hibrid Nasutus mempunyai tekstur yang berbeda nyata dengan Nasutus dan Jambal yang kompak dan padat, tetapi mempunyai kesamaan dengan patin Siam dan Pasupati yang agak kompak dan agak padat. Berdasarkan intensitas warna, hasil uji pembeda atribut dan uji kesukaan, maka secara berturut-turut panelis menyukai filet patin Jambal, Nasutus, hibrid Nasutus, Pasupati, dan Siam. Hibrid Nasutus mempunyai edible portionpaling tinggi (49% dibandingkan dengan patin lainnya tetapi mempunyai kadar air, kadar lemak, dan kadar protein yang lebih rendah dan berbeda nyata dengan induknya (patin Siam dan Nasutus. Patin Siam mengandung asam amino esensial paling tinggi di antara berbagai jenis patin yang diteliti. Profil asam amino patin hibrid Nasutus, Jambal, Pasupati, dan Nasutus hampir sama, kecuali pada patin Siam yang mengandung glisin, leusin, isoleusin, histidin, serin, treonin, dan prolin yang lebih tinggi dibandingkan dengan patin lainnya

  15. Les adjectifs à valeur intensive dans les groupes nominaux

    Directory of Open Access Journals (Sweden)

    Buvet Pierre-André

    2012-07-01

    Full Text Available Un dictionnaire électronique est élaboré dans la perspective du Traitement Automatique des Langues. Il s'agit d'une ressource qui est exploité par un ensemble d'outils informatiques pour donner lieu à une application dédiée au traitement de l'information textuelle. Le dictionnaire électronique présenté dans l'article concerne principalement des adjectifs prédicatifs à forme simple qui ont fait l’objet d’un recensement exhaustif et qui ont été décrits formellement. Sa macrostructure est constituée de plus de 20 000 emplois adjectivaux. Sa microstructure comporte des descripteurs normalisés de telle sorte que les informations métalinguistiques stipulées permettent d'effectuer des analyses sémantiques fines. Les adjectifs prédicatifs à forme complexe sont également incorporés au dictionnaire; ils sont décrits comme les adjectifs prédicatifs à forme simple dans la mesure où ils fonctionnent de la même façon. Dans un premier temps, nous discutons de la notion d'adjectif prédicatif en précisant préalablement les notions de prédicat et d'emploi prédicatif ainsi que celles de signification lexicale et de signification grammaticale. Nous présentons les marqueurs de l’intensité qui correspondent à des adjectifs monolexicaux et prédicatifs ou bien polylexicaux et prédicatifs. Nous discutons de ces adjectifs dans un premier temps selon qu’il s’agit de modifieurs libres, dans un deuxième temps de modifieurs liés et dans un troisième temps de constituants d’une détermination figée. Nous précisons dans les trois cas de figure quelles sont les conditions d’occurrences des adjectifs prédicatifs dans les groupes nominaux en nous appuyant sur les descriptions des adjectifs et des déterminants du français qui proviennent de deux bases de données exhaustives.

  16. Modelling solar radiation interception in row plantation. 3. Application to a traditional vineyard; Modélisation de l’interception des rayonnements solaires dans une culture en rangs. 3. Application à une vigne traditionnelle

    Energy Technology Data Exchange (ETDEWEB)

    Sinoquet, H. [Institut National de la Recherche Agronomique, Pointe a Pitre (France); Valancogne, C.; Lescure, A.; Bonhomme, R.

    1992-07-01

    A previously described model of solar radiation interception was applied to a spatially discontinuous canopy: that of a traditional vineyard in which the classical terms of the radiative balance and the spatial distribution of the radiation transmitted to the soil were measured. Comparison of measured and simulated data gave satisfactory agreement for reflected radiation (fig 4), but major discrepancies appeared for mean transmitted radiation (fig 5). The use of small stationary sensors for measuring the transmitted radiation explains the latter observation, since most of the time they measured radiation received on the ground in the sunflecks or in the shaded area rather than mean radiation. This was verified by comparing the measured and simulated spatial distribution of transmitted radiation (figs 7, 8). Finally, the influence of the woody parts which were not taken into consideration in the model was clearly identified : it significantly reduced the transmission of incident radiation (fig 9), and to a greater degrees the closer the sensor was to the vegetation row. (author) [French] Un modèle d’interception du rayonnement solaire décrit précédemment est appliqué à un couvert spatialement discontinu : une vigne traditionnelle sur laquelle ont été mesurés les termes classiques du bilan radiatif et la distribution spatiale du rayonnement transmis au sol. La comparaison des mesures au modèle révèle un ajustement satisfaisant pour le rayonnement réfléchi (fig 4), mais assez médiocre pour le rayonnement transmis moyen (fig 5). Ceci est expliqué par l’utilisation de capteurs ponctuels qui, en raison de leur taille, mesurent plus souvent le rayonnement reçu au sol dans les taches de soleil ou les zones d’ombre qu’un rayonnement moyen. Ceci est vérifié en comparant les distributions mesurées et calculées du rayonnement transmis au sol (figs 7 et 8). Enfin, l’influence des parties ligneuses, non prise en compte dans le modèle, est

  17. MENGENALI GEJALA TINITUS DAN PENATALAKSANAANNYA

    Directory of Open Access Journals (Sweden)

    Dewi Purwita Agustini

    2016-05-01

    Full Text Available Telinga berdenging atau dikenal dalam bahasa medis sebagai tinitus, banyak dikeluhkan sebagai suatu bising atau bunyi yang muncul di kepala tanpa adanya rangsangan dari luar. Adapun keluhan yang dialami ini seperti bunyi mendengung, mendesis, menderu, atau berbagai variasi bunyi yang lain. Tinitus bukanlah penyakit atau sindroma, tapi hanya merupakan gejala yang mungkin berasal dari satu atau sejumlah kelainan. Sebetulnya suara yang terdengar oleh telinga tersebut belum tentu bersifat kelainan atau patologis. Jika orang sehat yang terbukti telinganya normal, berada dalam ruang kedap (anehoic chamber, maka ia akan dapat mendengar berbagai macam suara yang berasal dari berbagai organ tubuhnya sendiri yang memang bekerja setiap saat, contohnya: pernapasan, kontraksi jantung, dan aliran darah. Kenyataannya, dalam kehidupan sehari-hari, suasana yang memungkinkan suara fisiologis atau normal tersebut terdengar oleh seseorang sangat jarang tercipta dan bahkan dalam kamar yang sunyi di malam hari sekalipun. Hal ini dikarenakan, bunyi masking dari lingkungan dengan berintensitas bunyi sekitar 25 – 30 dB. Tinitus baru menjadi gejala jika suara organ tubuh intensitasnya melebihi bunyi masking lingkungan tadi. Tinitus kerap diderita terutama orang pada kelompok usia pertengahan dan usia tua. Menurut data statistic dari pusat kesehatan di Amerika, sekitar 32% orang dewasa pernah mengalami tinitus pada suatu saat tertentu dalam hidupnya, dan 6 % nya sangat menganggu dan cukup sulit disembuhkan. Di Inggris, 17% populasi juga memiliki masalah tinitus. Sayangnya di Indonesia belum ada data statistic yang memadai, namun berdasarkan pengalaman empiris, penderita tinitus cukup banyak dan sering ditemui di tempat praktek, klinik, maupun rumah sakit. Meski tinitus bukanlah keadaan yang membahayakan, munculnya gejala ini pada hampir kebanyakan orang sangat mengganggu dan sering mempengaruhi kualitas hidup dan pekerjaannya. Kata Kunci: Tinitus, berdenging, telinga

  18. Le CRDI dans les Philippines

    International Development Research Centre (IDRC) Digital Library (Canada)

    Le CRDI appuie la recherche dans les. Philippines depuis 1972. Le travail qu'y ont accompli des universités et des instituts de recherche vigoureux et la participation active de la société civile ont entraîné d'importantes améliorations dans les domaines de l'agriculture, du suivi de la pauvreté et de la gestion des forêts.

  19. XML specifications DanRIS

    DEFF Research Database (Denmark)

    2009-01-01

    XML specifications for DanRIS (Danish Registration- og InformationsSystem), where the the aim is: Improved exchange of data Improved data processing Ensuring future access to all gathered data from the year 1999 until now......XML specifications for DanRIS (Danish Registration- og InformationsSystem), where the the aim is: Improved exchange of data Improved data processing Ensuring future access to all gathered data from the year 1999 until now...

  20. Ketergantungan Online Game Dan Penanganannya

    OpenAIRE

    Syahran, Ridwan

    2015-01-01

    Penelitian ini dimaksudkan untuk mengetahui perilaku yang ditimbulkan dari kecanduan bermaian online game pada siswa SMP Negeri 1 Palu yang meliputi faktor-faktor penyebab kecanduan, keadaan psikologis yang ditimbulkan dari kecanduan bermain online game dan dampak-dampak yang ditimbulkan dari kecanduan bermain online game.Pendekatan penelitian ini adalah penelitian kualitatif dengan jenis penelitian studi kasus dengan berdasarkan responden dan informan sebagai bahan sumber data. Dalam proses ...

  1. ENERGI DAN DAMPAKNYA TERHADAP LINGKUNGAN

    Directory of Open Access Journals (Sweden)

    I Made Astra

    2010-11-01

    Full Text Available Energi dapat berubah dari satu bentuk ke bentuk yang  lainnya, perubahannya sering mempengaruhi lingkungan dan udara yang kita hirup dengan berbagai cara. Energy kimia dalam bahan bakar fosil diubah menjadi energy panas, mekanik, atau listrik melalui pembakaran dan  ini sebagai penghasil polutan terbesar. Dan dengan demikian pembangkit listrik, kendaraan bermotor, dan kompor adalah penyebab utama terjadinya polusi udara.  Polutan yang dikeluarkan biasanya dikelompokan menjadi  hidrokarbon (HC, nitrogen oksida (NOx, dan  karbon monoksida (CO. Polutan yang dihasilkan pada pembakaran fosil merupakan faktor terbesar terjadinya asap, hujan asam,  pemanasan global dan perubahan iklim.   The conversion of energy from one form to another often affects the environment and the air we breath in many ways. Pollutants are emitted as the chemical energy in fossil fuels is converten to thermal, mechanical, or electrical energy via combustion, and thus power plants, motor vehicles, and even stoves take the blame for air pollution, and  the pollutants released by the vehicles are usually grouped as hydrocarbons (HC, nitrogen oxides (NOx, and carbon monoxide (CO. Pollutans emitted during the combustion of fossil fuels are responsible for smog, acid rain, and global warming and climate change.

  2. Isolasi dan Karakterisasi Ralstonia syzygii

    Directory of Open Access Journals (Sweden)

    Yanuar Danaatmadja

    2009-07-01

    Full Text Available Ralstonia syzygii is one of important pathogens of cloves. This study was aimed at obtaining pure culture of R. syzygi from diseased plant tissue samples. The acterium was isolated from infected clove plantations in Ungaran, Central Java. It had the ability to make clove seedlings show symptoms and then die 41 days after inoculation. The reisolated bacterium also showed its ability to kill clove seedlings after 17 days. The bacterium is gram negative, able to ultilize glucose, sucrose, maltose, mannitol, sorbitol, dulcitol, and glycerol, able to hydrolyze starch, grow well at 27oC, able to catalyze and release water and oxygen from hydrogen peroxyde (H2O2 and aerobically.   Ralstonia syzygii merupakan salah satu patogen penting pada tanaman cengkeh. Penelitian ini dilakukan untuk mendapakan isolat murni R syzygii dari jaringan tanaman terinfeksi. Bakteri diisolasi dari pertanaman cengkeh sakit yang berasal dari daerah Ungaran, Jawa Tengah. Bakteri menunjukkan kemampuan untuk menyebabkan bibit tanaman cangkeh sakit dan kemudian mati 41 hsi. Bakteri hasil reisolasi juga menunjukkan kemampuannya menyebabkan sakit dan kematian pada bibit tanaman cengkeh setelah 17 hsi. Bakteri yang diperoleh bersifat gram negatif, mampu memanfaatkan glukosa, sukrosa, maltosa, manitol, sorbitol, dulsitol, dan gliserol, mampu menghidrolisis pati, tumbuh baik pada suhu 27o C, mampu mengkatalisis dan melepaskan air dan oksigen dari hydrogen peroxide (H2O2 dan bersifat aerob.

  3. PRINSIP-PRINSIP DASAR EKONOMI ISLAM DAN PENGARUH TERHADAP PENETAPAN STANDAR AKUNTANSI

    Directory of Open Access Journals (Sweden)

    Koenta Adji Koerniawan

    2012-02-01

    Full Text Available Ekonomi islam merupakan suatu hal yang harus diimplementasikan dalam kehidupan bisnis. Tidak ada keraguan sebagai mayoritas pemeluk Islam untuk melaksanakan konsep-konsep yang didasarkan pada Al-Qur’an dan Al-Hadist. Dalam pandangan Islam, hukum berasal dari Tuhan (Allah dan manusia hanya bisa mendaftar dan memperluasnya untuk situasi yang berbeda. In the west, laws are passed to accommodate existing situations while, in the Islamic view, existing situations must be transformed to conform to Divine Law. Di barat, hukum dilewatkan untuk mengakomodasi situasi yang ada sementara, dalam pandangan Islam, situasi yang ada harus berubah menjadi sesuai dengan Hukum Ilahi. Singkatnya, tanpa aplikasi pengaturan Islami'ah Syariat Islam Standar Akuntansi tidak mungkin. Elements which should be considered include: Islamic economy elements the most important of which is social justice through application of prohibition of riba, zakat, and Islamic ethics. Elemen yang harus dipertimbangkan mencakup: elemen-elemen ekonomi Islam yang paling penting yang adalah keadilan sosial melalui penerapan larangan riba, zakat, dan etika Islam. Other factors such as Environmental and International elements which influence Muslims community and adoption of these elements are possible based on Ijtihad through application of "Time" and "Place". Faktor-faktor lain seperti dan Internasional elemen Lingkungan yang mempengaruhi masyarakat Muslim dan adopsi dari unsur-unsur yang mungkin didasarkan pada ijtihad melalui penerapan "Waktu" dan "Tempat".

  4. OPTIMASI TATA GUNA LAHAN DAN PENERAPAN REKAYASA TEKNIK DALAM ANALISA BANJIR DI DAERAH ALIRAN SUNGAI: STUDI KASUS DAERAH ALIRAN SUNGAI CILIWUNG HULU DI BENDUNG KATULAMPA (The Optimization of Land Use and the Application of Engineering Treatment in Flood

    Directory of Open Access Journals (Sweden)

    Yohana Lilis Handayani

    2005-07-01

    Full Text Available ABSTRAK Peningkatan aliran puncak dan volume runoff dari flood hydrograph dapat disebabkan oleh konversi penggunaan lahan. Fenomena ini terjadi di cekungan hulu sungai Ciliwung sebagai daerah konservasi. DAS ini memiliki peran penting dalam memelihara ketersediaan air di cekungan Ciliwung dan untuk pengendalian banjir di daerah hilir. Berdasarkan data yang dicatat dari 1993 sampai dengan 1996, 14,6% kejadian banjir di daerah hilir disebabkan oleh banjir kiriman. Evaluasi konversi penggunaan lahan di daerah hulu Ciliwung dilakukan dengan membandingkan penggunaan lahan tahun 1989 dan 1998. Optimasi tata guna lahan dilakukan dengan optimasi linier untuk meminimasi nilai koefisien composite runoff. Pendekatan teknis dan penerapan rekayasa teknik digunakan untuk simulasi penurunan aliran puncak dan volume runoff dari flood hydrograph. Perlakuan ini meliputi terracing dan normalisasi kolam detensi (detention pond. Simulasi dilakukan untuk periode banjir 10 tahunan. Hasil analisis menunjukkan bahwa dalam periode 10 tahun (1989-1998 penggunaan lahan dikonversi secara signifikan. Konversi ini menyebabkan peningkatan aliran puncak dan volume runoff masing-masing 18,97% dan 18,87%.   ABSTRACT The risk of peak flow and runoff volume of a flood hydrograph may be caused by land use conversion. This phenomenon had happened in upstream of Ciliwung basin. As a conversation area, this catchment has an important role in maintaining the water availability of Ciliwung basin and for flood control in downstream area. Based on the collected flood data recorded from 1993 to 1996, 14.6% of flood events in downstream of Ciliwung basin were caused by delivery flood from upstream area. Evaluation of land use conversion in upstream of Ciliwung basin was carried out by comparing land use in 1989 and in 1998. Land use optimization was done using linear optimization to minimize the value of composite runoff coefficient. Technical approach of engineering treatment was used to

  5. Derivatization reagents in liquid chromatography/electrospray ionization tandem mass spectrometry.

    Science.gov (United States)

    Santa, Tomofumi

    2011-01-01

    Liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) is one of the most prominent analytical techniques owing to its inherent selectivity and sensitivity. In LC/ESI-MS/MS, chemical derivatization is often used to enhance the detection sensitivity. Derivatization improves the chromatographic separation, and enhances the mass spectrometric ionization efficiency and MS/MS detectability. In this review, an overview of the derivatization reagents which have been applied to LC/ESI-MS/MS is presented, focusing on the applications to low molecular weight compounds. 2010 John Wiley & Sons, Ltd.

  6. Blocage de Coulomb dans une boite quantique laterale contenant un faible nombre d'electrons

    Science.gov (United States)

    Gould, Charles

    Dans ce travail on utilise une nouvelle geometrie pour augmenter le controle sur le nombre d'electrons contenus dans une boite quantique laterale, et ainsi atteindre un regime de petit nombre d'electrons. Ces echantillons permettent une etude du blocage de Coulomb quand les electrons sont injectes a partir d'un gaz electronique a deux dimensions (2DEG). Les mesures a faible champ magnetique demontrent la grande flexibilite des echantillons et montrent que l'on peut faire varier le nombre d'electrons dans une boite quantique a partir de plus de 40 electrons jusqu'a un seul electron, ce qui est assez courant dans les boites quantiques verticales, mais ce qui n'avait jamais ete reussi dans une boite quantique laterale. Nos resultats montrent egalement que dans les boites quantiques laterales il est possible de determiner le spin du niveau qui participe au transport a l'aide du phenomene de blocage de spin. De plus, dans certaines circonstances il est meme possible de determiner le spin total de la boite quantique, ce qui peut avoir des applications pratiques dans des domaines tels l'informatique quantique. Les mesures dans le regime de renversement de spin a un champ magnetique plus eleve montrent l'importance des correlations electrons---electrons dans ces boites quantiques, qui menent a des depolarisations et a des structures de spins qui ont un effet sur le transport. En particulier, ces correlations menent a l'existence de niveaux excites de basse energie qui causent une dependance anormale de l'amplitude des pics de blocage de Coulomb en fonction de la temperature. Nos experiences demontrent egalement la possibilite d'utiliser ces boites quantiques comme sondes pour etudier les proprietes du bord d'un 2DEG. Une voie de recherche a etre exploree.

  7. ALGORITMA RC4 DALAM PROTEKSI TRANSMISI DAN HASIL QUERY UNTUK ORDBMS POSTGRESQL

    Directory of Open Access Journals (Sweden)

    Yuri Ariyanto

    2009-01-01

    Full Text Available In this research will be worked through about how cryptography RC4's algorithm implementation in protection to query result and of query, security by encryption and descryption up to both is in network. Implementation of this research which is build software in client that function access databases that is placed by the side of server. Software that building to have facility for encryption and descryption query result and of query that is sent from client goes to server and. transmission query result and of query can secure its security. Well guaranted transmission security him of query result and of query can be told to succeed if success software can encryption query result and of query which transmission so that in the event of scanning to both, scanning will not understand data content. Conclusion of this research that is woke up software succeed encryption query and result of query which transmission between application of client and of server databases. Abstract in Bahasa Indonesia: Pada penelitian ini dibahas mengenai bagaimana mengimplementasikan algoritma kriptografi RC4 dalam proteksi terhadap query dan hasil query, pengamanan dilakukan dengan cara melakukan enkripsi dan dekripsi selama keduanya berada di dalam jaringan. Pengimplementasian dari penelitian ini yaitu membangun sebuah software yang akan diletakkan di sisi client yang berfungsi mengakses database yang diletakkan di sisi server. Software yang dibangun memiliki fasilitas untuk mengenkripsi dan mendektipsi query dan hasil query yang dikirimkan dari client ke server dan juga sebaliknya. Dengan demikian tramsmisi query dan hasil query dapat terjamin keamanannya.Terjaminnya keamanan transmisi query dan hasil query dapat dikatakan berhasil jika software berhasil mengenkripsi query dan hasil query yang ditransmisikan sehingga apabila terjadi penyadapan terhadap keduanya, penyadap tidak akan mengerti isi data tersebut. Kesimpulan dari penelitian ini yaitu software yang dibangun

  8. Penskalaan Butir Format Respons Pilihan dan Respons Bebas Berdasarkan Model Rasch dan Partial Credit

    OpenAIRE

    Eko Hariadi

    2007-01-01

    Penelitian melihat pengaruh jumlah parameter butir, kategori respons bebas (RB), pengaruh sampel terhadap akurasi estimasi parameter kemampuan untuk menghasilkan estimasi yang stabil dan pengaruh pembobotan butir RP dan butir RB terhadap kesalahan baku. Penelitian dalam dua tahap, simulasi menggunakan 30 kondisi dengan replikasi 50 dengan variabel panjang tes, jumlah kategori, dan jumlah parameter butir, dan analisis deskriptif, dilanjutkan penerapan penskalaan gabungan butir tipe res...

  9. Metode Sederhana dan Efektif untuk Penghitungan dan Visualisasi Tiga Dimensi (3D) Biofilm Vibriio Cholera

    OpenAIRE

    Kurniawan, Andi; Fadjar, Mohamad; Sukoso, Sukoso; Prihanto, Asep Awaludin

    2015-01-01

    Mikroorganisme yang mampu menghasilkan biofim menimbulkan masalah yang serius dalam bidang kesehatan dan pangan. Penelitian biofim bagi sebagian peneliti sangat identik dengan kerumitan proses penghitungan dan visualisasi penutupan permukaan substrat penempelan bakteri. Penelitian ini ditujukan untuk mengetahui efiiensi metode alternatif untuk menghitung dan memvisualisasikan biofimVibrio cholera. Pada penelitian ini beberapa faktor lingkungan seperti pH, suhu, dan kondisi kultur diujicobakan...

  10. PROTOTIPE VIDEO EDITOR DENGAN MENGGUNAKAN DIRECT X DAN DIRECT SHOW

    Directory of Open Access Journals (Sweden)

    Djoni Haryadi Setiabudi

    2004-01-01

    Full Text Available Technology development had given people the chance to capture their memorable moments in video format. A high quality digital video is a result of a good editing process. Which in turn, arise the new need of an editor application. In accordance to the problem, here the process of making a simple application for video editing needs. The application development use the programming techniques often applied in multimedia applications, especially video. First part of the application will begin with the video file compression and decompression, then we'll step into the editing part of the digital video file. Furthermore, the application also equipped with the facilities needed for the editing processes. The application made with Microsoft Visual C++ with DirectX technology, particularly DirectShow. The application provides basic facilities that will help the editing process of a digital video file. The application will produce an AVI format file after the editing process is finished. Through the testing process of this application shows the ability of this application to do the 'cut' and 'insert' of video files in AVI, MPEG, MPG and DAT formats. The 'cut' and 'insert' process only can be done in static order. Further, the aplication also provide the effects facility for transition process in each clip. Lastly, the process of saving the new edited video file in AVI format from the application. Abstract in Bahasa Indonesia : Perkembangan teknologi memberi kesempatan masyarakat untuk mengabadikan saat - saat yang penting menggunakan video. Pembentukan video digital yang baik membutuhkan proses editing yang baik pula. Untuk melakukan proses editing video digital dibutuhkan program editor. Berdasarkan permasalahan diatas maka pada penelitian ini dibuat prototipe editor sederhana untuk video digital. Pembuatan aplikasi memakai teknik pemrograman di bidang multimedia, khususnya video. Perencanaan dalam pembuatan aplikasi tersebut dimulai dengan pembentukan

  11. Strategi Komunikasi Program Internet Sehat Dan Aman Kementerian Komunikasi Dan Informatika Republik Indonesia (Studi Kasus Evaluasi Program Incakap Tahun 2015

    Directory of Open Access Journals (Sweden)

    Sucianty Dyah Astuti

    2016-07-01

    Full Text Available Internet has become a lifestyle in community along with the development of internet technology in the life and social relationship. The high number of internet users in Indonesia gave rise to a variety of impacts on society, both positive and negative. Relates with these impacts, to create an understanding in the community against the use of the internet the Government through the Ministry of communications and Informatics of the Republic of Indonesia create program, that is Internet healthy and safe in order to socialize the use of the internet for healthy and safe through the ethics of the Internet learning healthy by involving all components of society.The research focused on the evaluation of healthy and safe internet programme conducted by the Ministry of communications and Informatics of the Republic of Indonesia in 2015. The objective of the research is to perceive the communication strategy and the achievement of the objectives of the healthy and safe internet program by KemKominfo. This research used the qualitative method with descriptive case study research. The data obtained through interviews and literature studies, while informants in this study was KemKominfo staff on to the various Directorate General Application Infomatika sub direktotar empowerment of informatics as many as three people. Through the whole concatenation of process research obtained results that indicate that: (1 the achievement of healthy and safe Internet Programme until 2015 has achieved the target but not 100%. (2 in the implementation of the program there are some obstacles faced by KemKominfo, specifically: (i the limitation of APBN, (ii affordability limitations due to the geographical of indonesia as an archipelago state. (3\tthe evaluation needs to be done about the use of online media in the communication strategy of healthy and secure internet program. There were some changes since the beginning of the implementation of the Insan program in the year

  12. Localization of alpha emitters by damage production in a thin film. Application to the study of alpha emitter diffusion in irradiated samples; Localisation des emetteurs alpha par creation de dommages dans un film mince. Application a l'etude de la diffusion des emetteurs alpha dans des echantillons irradies

    Energy Technology Data Exchange (ETDEWEB)

    Houdaille, B; Perrot, M [Commissariat a l' Energie Atomique, 91 - Saclay (France). Centre d' Etudes Nucleaires

    1968-07-01

    The process of recording {alpha} particles on cellulose nitrate films, called alpha-graphy, is applied to the study of the diffusion of {alpha}-emitting elements in irradiated alloys. The existence of diffusion is shown by attacking the film with concentrated caustic soda after exposition. The insensitivity of the recorder to {beta} {gamma} radiation emitted by the sample after passing in the reactor makes it possible to operate with long exposure times and to detect small diffusions. The concentration-penetration curves are drawn up after carrying out a densitometric analysis of the alpha-graphies. - As the cellulose nitrate is affected only by {alpha} particles of energies of between 0.5 and 4 MeV, it was first necessary to determine the yield of the recorder for {alpha} particles emitted by a thick source, i.e. whose energy varies between 0 and E{sub 0}, E{sub 0} being the energy of the alpha emitter. - The concentration C of the {alpha}-emitter, as a function of the optical density D of the alpha-graphy, and of the exposure time t is given by a simple relationship: C = D/at where a is an experimental constant determined by calibration. It depends on the nature of the cellulose nitrate, of the {alpha}-emitting element and of the alloy studied. (authors) [French] Le procede d'enregistrement des particules alpha sur film de nitrate de cellulose, ou alphagraphie, est applique a l'etude de la diffusion d'elements emetteurs alpha dans des alliages irradies. La diffusion est mise en evidence par une attaque du film de nitrate, apres exposition, dans de la soude concentree. L'insensibilite de l'enregistreur au rayonnement {beta} {gamma}, emis par l'echantillon apres son sejour en pile, permet d'operer sur de longs temps de pose et de detecter des diffusions faibles. Les courbes concentration - penetration sont etablies par exploitation densitometrique des alphagraphies. - Comme le nitrate de cellulose n'est impressionne que par des particules alpha dont l'energie est

  13. MIKROENKAPSULASI Lactobacillus sp. DENGAN TEKNIK EMULSI DAN APLIKASINYA PADA DODOL SIRSAK [Microencapsulation of Lactobacillus sp. using Emulsion Technique and Its Application in Soursop Sweet Cakes

    Directory of Open Access Journals (Sweden)

    Anis Usfah Prastu Jati

    2015-12-01

    Full Text Available Two probiotic strains Lactobacillus acidophilus 2B4 and L. rhamnosus R23 were microencapsulated by an emulsion technique using sodium alginate and vegetable oil. The present study aimed to enhance probiotic survival on their application in the production of soursop sweet cakes (dodol sirsak and their stability during storage at room temperature. The probiotic biomasses were mixed with 3% sodium alginate and then added dropwise into a mixture of soybean oil and Tween 80. The microencapsulation technique applied resulted in excellent survival (95-96% for both Lactobacillus sp. strains. Encapsulation significantly improved the survival of probiotics (P<0.05 during exposure to heat process (60, 65, and 70°C for 20 min, low pH (pH 2 and bile salt (0.5%. Encapsulation did not alter the ability of both probiotics in inhibiting the growth of Escherichia coli ATCC 25922. The viability of encapsulated strains in soursop sweet cakes were improved to the adequate number, i.e. 6 Log CFU g-1 up to 3 and 2 weeks storage, as compared to that of controls survivors, i.e. 4.3 and 2.5 Log CFU g-1, for L. acidophilus 2B4 and L. rhamnosus R23, respectively, during a week of storage.

  14. Study of the anodic process in the electrolysis of molten chlorides. Application to the chlorine electrode; Contribution a l'etude du processus anodique dans l'electrolyse des chlorures fondus. Application a l'electrode de chlore

    Energy Technology Data Exchange (ETDEWEB)

    Fondanaiche, J C [Commissariat a l' Energie Atomique, Fontenay-aux-Roses (France). Centre d' Etudes Nucleaires

    1967-05-01

    The oxidation reaction of Cl{sup -} ions on a carbon electrode occurs with a very low over-voltage in molten LiCl-KCl, NaCl-KCl, CaCl{sub 2} and AgCl electrolytes and therefore the properties of the electrode 'polarized' anodically with a current density I are, as a first approximation, identical to those which it possesses at a chlorine pressure P (produced by the addition of external chlorine). This property of the Cl{sup -} ion oxidation reaction has enabled us to propose an electrochemical method for the study of the absorption equilibrium of the chlorine between a solid and a liquid phase. We can in effect replace this addition of outside chlorine at a pressure P by an electrolysis at a current density I. We have developed a mechanism which accounts for the reaction kinetic of the discharge of Cl{sup -} ions. It has been checked with the help of intensity-potential curves and potential-time curves which characterize the carbon depolarization in an open circuit. Two methods have been used for measuring the amount of chlorine adsorbed on the carbon. It has been possible to determine the nature of the bonds linking the adsorbed chlorine to the carbon, and the electrode-electrolyte surface exchange by varying the temperature and the nature of the electrode and of the electrolyte. Certain anomalies and in particular certain transient phenomena have been explained by the influence of the oxygen present in the molten salt in the form of O{sup 2-} ions and, on the electrode surface, in the form of chemisorption complexes. (author) [French] La reaction d'oxydation des ions Cl{sup -} sur une electrode de carbone s'effectue avec une surtension tres faible dans les electrolytes fondus LiCl-KCl, NaCl-KCl, CaCl{sub 2} et AgCl et par consequent les proprietes de l'electrode ''polarisee'' anodiquement avec une densite de courant I sont, en premiere approximation, identiques a celles qu'elle possede sous une pression de chlore P (creee par un apport exterieur de chlore). Cette

  15. Modifikasi Limbah Tulang Sapi Bali dan Pemanfaatannya untuk Adsorpsi Methylene Blue (MODIFICATION OF BALI COW BONE WASTE AND ITS APPLICATION TO ADSORPTION OF METHYLENE BLUE

    Directory of Open Access Journals (Sweden)

    I Nengah Simpen

    2017-01-01

    Full Text Available The research of modification, characterization, and application of nano-porous adsorbent base onBali cow bone waste to methylene blue (MB adsorption has been carried out. The modification was carriedout through extraction of hydroxyapatite (HA from cow bone, then its activated by 0.4 M NaOH solutionand coating to form active sites of Fe and Fe-Al oxides. The adsorbent was applied to know quantitativelyadsorption capacity coated-HA (CHA to MB as wastewaters simulation. Compound of CHA wascharacterized amount of active sites by base-acid titration, Bronsted-Lewis acid sites by FTIR spectroscopy,specific surface area by MB method and pore size by surface area analyzer gasorption nitrogen. While,amount of coated-Fe and Al by LIBS. Amount of MB adsorbed was analyzed by UV-Vis spectrophotometer.The results showed that coating of Fe and Fe-Al oxides increased amount of active sites, sites distributionof new Lewis acid site, everage nano pore size with pore volume is microporous (less than 2 nm, and Fe andFe-Al oxides was into HA crystal structure. The amount of active sites was the higest of T1-Fe-Al2O3 andall pores diameter less than 58.182 nm.While, the specific surface area increased T3-Fe2O3>T3-Fe-Al2O3>T2-Fe2O3 respectively. In the adsorption isotherm, coating on HA significantly increased ability of adsorbentand through Freundlich model (R2 > 0.77 with the higest adsorption capacity on T3-Fe2O3 (3.2019 mg/gthen T2-Fe-Al2O3 (2.7921 mg/g. Results of this research indicate that Fe and Fe-Al oxides HA-modifiedincreased adsorption ability.

  16. Study of the magnetic characteristics of ferrites with a view to their application in a proton synchrotron; Etudes des caracteristiques magnetiques des ferrites en vue de leur application dans un synchrotron a protons

    Energy Technology Data Exchange (ETDEWEB)

    Nguyen, K C [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1966-10-01

    In this report magnetic properties of some Ni Zn ferrites available in France are investigated for the purpose of their use in accelerating cavities of proton synchrotron. An attempt is made to measure permeability and quality factor of ferrite versus various physical parameters such as frequency F, the induction B, the magnetic bias field Hp and the temperature, the investigation ranges being: F {<=} 40 Mc/s; B {<=} 10{sup -2} Tesla; Hp {<=} 5000 AT/m; T {<=} 100 C. The measurements were carried out with the one hand, conventional impedance bridge (Q-meter, RX-meter) and on the other hand, with resonating method using an inductive ferrite loaded cavity in parallel with an external capacity. The latter method is of particular interest for the measurements in function of induction and magnetic bias field. (author) [French] Ce travail consiste a etudier les proprietes magnetiques d'un certain nombre de ferrites de Ni Zn disponibles sur le marche francais en vue de leur utilisation dans les cavites acceleratrices d'un synchrotron a protons. On se propose de mesurer la permeabilite et le facteur de qualite du ferrite en fonction de divers parametres physiques tels que la frequence F, l'induction B, le champ magnetique de polarisation Hp et la temperature T, avec: F {<=} 40 Mc/s; B {<=} 10{sup -2} Tesla; Hp {<=} 5000 AT/m; T {<=} 100 C. On effectue les mesures d'une part a l'aide des ponts d'impedance classiques (Q-metre, RX-metre) et d'autre part par la methode du resonateur qui consiste a mettre en parallele une cavite inductive chargee de ferrite et une capacite exterieure. Cette derniere methode est particulierement interessante pour les mesures en fonction de l'induction et du champ magnetique polarisant. (auteur)

  17. Enseignement Basé sur les Compétences : Manuel d'Application dans le Domaine des Sciences Agronomiques a L'Université d'Abomey-Calavi

    NARCIS (Netherlands)

    Koutinhouin, B.; Hupkes, M.; Gooijer, de G.; Aho, N.; Windmeijer, P.N.

    2011-01-01

    Le présent manuel est produit dans le cadre du Projet d’Appui au Renforcement des Programmes de Formation et de Recherche en Agriculture à la Faculté des Sciences Agronomiques et à l’Ecole Polytechnique d’Abomey-Calavi, financé par le Gouvernement du Royaume des Pays-Bas (Projet NPT/BEN/146). Il est

  18. METHOD 332.0: DETERMINATION OF PERCHLORATE IN DRINKING WATER BY ION CHROMATOGRAPHY WITH SUPPRESSED CONDUCTIVITY AND ELECTROSPRAY IONIZATION MASS SPECTROMETRY

    Science.gov (United States)

    This method is applicable to the identification and quantitation of perchlorate in raw and finished drinking waters. The approach used is ion chromatography with suppressed conductivity and electrospray ionization mass spectrometry (IC-ESI/MS)

  19. Purwarupa Sistem Integrasi Quadcopter dan Mobile Robot

    OpenAIRE

    Dharmawan, Andi; Lusiarta Putera, Christian Antonia

    2012-01-01

    AbstrakQuadcopter, juga dikenal sebagai quadrotor, adalah helikopter dengan empat motor yang dilengkapi dengan  empat buah propeller pada masing-masing motornya yang digunakan untuk terbang dan bermanuver. Pada quadcopter terdapat 3 variabel sudut yang menjadi element utama dalam pengendaliannya yaitu roll, pitch, dan yaw yang diperoleh dari penggabungan sensor accelerometer, gyroscope dan magnetometer dengan metode Direction Cosine Matrix. Pada sistem integrasi mobile robot dan quadcopter, d...

  20. Review Dendrimer : Definisi, Sintesis, Aplikasi Dan Prospektif

    OpenAIRE

    Rahmi, Dwinna

    2013-01-01

    Dendrimer merupakan makrostruktur monodisperse dengan banyak cabang yang homogen dan degree of branching (DB) 100%. Dua cara sintesis dendrimer yaitu convergent dan divergent dilakukan. Convergent dilakukan dengan reaksi kovalen antara dua dan lebih monomer. Divergent dimulai dengan pembentukan inti dilanjutkan dengan pembentukan cabang yang merupakan group fungsional yang aktif. Sejauh ini dendrimer sudah banyak diterapkan pada bidang farmasi yaitu drug delivery dan non farmasi pada proses i...

  1. Rancang Bangun Aplikasi Enkripsi dan Dekripsi Email Dengan Menggunakan Algoritma Advanced Encryption Standard Dan Knapsack

    Directory of Open Access Journals (Sweden)

    Timothy John Pattiasina

    2014-07-01

    Full Text Available Advanced Encryption Standard (AES dan Knapsack adalah dua algoritma enkripsi simetris dan asimetris yang paling sering digunakan. Penelitian ini menganalisa kedua algoritma AES dan algoritma Knapsack. Prototipe aplikasi enkripsi email ini dirancang dengan menggabungkan karateristik algoritma AES dan Knapsack untuk memecahkan masalah keamanan email. Algoritma AES digunakan untuk mengenkripsi dan deskripsi email berupa teks atau file, sedangkan Algoritma Knapsack di gunakan untuk mengenkripsi kunci AES. Enkripsi hybrid yang diterapkan pada aplikasi bertujuan untuk menambah keamanan informasi dalam sebuah jaringan.

  2. Turn-on fluorogenic and chromogenic detection of Fe(III) and its application in living cell imaging

    International Nuclear Information System (INIS)

    Sivaraman, Gandhi; Sathiyaraja, Vijayaraj; Chellappa, Duraisamy

    2014-01-01

    Two rhodamine-based sensors RDI-1, RDI-2 was designed and synthesized by incorporation of the rhodamine 6G fluorophore and 2-formyl imidazole as the recognizing unit via the imine linkages. RDI-1, RDI-2 exhibits very high selectivity and an excellent sensitivity towards Fe(III) ions in aqueous buffer solution on compared with other probes. The color change from colorless to pink and turn-on fluorescence after binding with iron (III) was observed. Based on jobs plot and ESI-MS studies, the 1:1 binding mode was proposed. Live cell imaging experiments with each probe showed that these probes widely applicable to detect Fe 3+ in living cells. -- Highlights: • Two rhodamine based probes was synthesized and used to recognize iron (III). • The chemosensors can be applied to detect iron(III) ions by color and turn-on fluorescent changes. • The very low detection limit was reported. • The applicability of these probes for live cell fluorescence imaging was studied

  3. Turn-on fluorogenic and chromogenic detection of Fe(III) and its application in living cell imaging

    Energy Technology Data Exchange (ETDEWEB)

    Sivaraman, Gandhi; Sathiyaraja, Vijayaraj; Chellappa, Duraisamy, E-mail: dcmku123@gmail.com

    2014-01-15

    Two rhodamine-based sensors RDI-1, RDI-2 was designed and synthesized by incorporation of the rhodamine 6G fluorophore and 2-formyl imidazole as the recognizing unit via the imine linkages. RDI-1, RDI-2 exhibits very high selectivity and an excellent sensitivity towards Fe(III) ions in aqueous buffer solution on compared with other probes. The color change from colorless to pink and turn-on fluorescence after binding with iron (III) was observed. Based on jobs plot and ESI-MS studies, the 1:1 binding mode was proposed. Live cell imaging experiments with each probe showed that these probes widely applicable to detect Fe{sup 3+} in living cells. -- Highlights: • Two rhodamine based probes was synthesized and used to recognize iron (III). • The chemosensors can be applied to detect iron(III) ions by color and turn-on fluorescent changes. • The very low detection limit was reported. • The applicability of these probes for live cell fluorescence imaging was studied.

  4. PENERAPAN PULSED ELECTRIC FIELD PADA PASTEURISASI SARI BUAH APEL VARIETAS ANA: KAJIAN KARAKTERISTIK NILAI GIZI, SIFAT FISIK, SIFAT KIMIAWI DAN MIKROBIA TOTAL Application of Pulsed Electric Field in Pasteurization of Apple Juice of Ana Cultivar : Study on

    Directory of Open Access Journals (Sweden)

    La Choviya Hawa

    2012-05-01

    Full Text Available Apple juice, extracted from apple of ana cultivar , was pasteurized using a pulsed electric field (PEF method. The aimof this research was to analyze the changes on nutritional, physical and chemical properties and total microbes from apple juice after pasteurization. The research was conducted from July until Oktober 2009 located in Malang. The PEF treatment was carried out using treatment time variation for 10, 20, 30, 40, 50 and 60 seconds. Several parameters of vitamin A and C, water content, density, pH, total soluable solid and total microbes were observed. The results showed that PEF treatment did not significantly change nutritional, physical and chemical properties and total microbes after pasteurization with PEF in compared with no treatment pasteurization. The highest degradation was found in treatment time for 60 seconds, i.e. 93.53 %. ABSTRAK Sari buah apel, yang diekstrak dari apel varietas ana, dipasteurisasi dengan metode pulsed electric field (PEF. Tujuanpenelitian ini adalah untuk mengetahui perubahan karakteristik nilai gizi, sifat fisik, kimiawi dan total mikrobia sari buah apel sesudah dipasteurisasi. Penelitian dilaksanakan bulan Juli sampai dengan Oktober 2009 di Malang. Penelitian ini menggunakan variasi waktu pengolahan 10, 20, 30, 40, 50 dan 60 detik. Parameter pengamatan yaitu vitamin A dan C, kadar air, berat jenis, pH, total padatan terlarut dan total mikrobia. Hasil penelitian menunjukkan bahwa nilai gizi, sifat fisik dan kimiawi dari sari apel  tidak mengalami perubahan signifikan dibandingkan sari apel tanpa perlakuan PEF. Penurunan total mikrobia terbesar pada waktu perlakuan 60 detik dengan efektivitas pembunuhan sebesar 93,53%.

  5. KORELASI ANTARA ISLAM DAN EKONOMI

    Directory of Open Access Journals (Sweden)

    Akmal Zainal Abidin

    2015-03-01

    Full Text Available CORELATION BETWEEN ISLAM AND ECONOMY. This paper aims to identifies about the correlation between economic and Islam. Islam is the perfect religion that governs all things in life, including the economy. This is evident with the concept of  well-being which is described in the al-Quran and Sunnah. Basically the goal of every human life is to prosper, although humans make sense of  well- being with a different perspective. Most understand economics assume that welfare is the welfare of  earthly material. But to make sense of well-being with the term al-Falah, is meaning holistic wellbeing and balance between material and spiritual dimensions. al-Quran and Sunnah have taught that the human being will be achieved if  living in balance between material and spiritual. This is because human life does not just stop in the life of this world, but there is still a second life that will be faced by humanity in the hereafter, and well-being will be achieved with the truth is that people can balance the needs of the world and the hereafter, and that is what is taught in Islamic economics. Keywords: Islam, Economy, Prosperity. Tulisan ini bertujuan untuk menjelasakn tentang korelasi antara ekonomi  dan  Islam.  Islam  adalah  agama  yang  sempurna  yang mengatur segala hal dalam kehidupan ini, termasuk juga ekonomi. Hal ini terbukti dengan konsep kesejahteraan yang dipaparkan dalam al-Quran dan Sunnah. Pada dasarnya tujuan hidup setiap manusia adalah untuk mencapai kesejahteraan, meskipun manusia memaknai kesejahteraan dengan perspektif  yang berbeda-beda. Sebagian besar paham ekonomi menganggap bahwa kesejahteraan adalah kesejahteraan material duniawi. Namun Islam memaknai kesejahteraan dengan istilah  Falah  yang  berarti  kesejahteraan  holistik  dan  seimbang antara dimensi material dan spiritual. Al-Quran dan Sunnah telah mengajarkan bahwa kesejahteraan akan tercapai jika manusia menjalani hidup secara seimbang antara material dan

  6. Karakteristik Dan Spektrum Manajemen Pendidikan Islam

    OpenAIRE

    Jannah, Siti Raudhatul

    2013-01-01

    Artikel ini mendiskusikan mengenai manajemen pendidikan Islam, karakteristik, dan spektrumnya. Karakteristik manajemen pendidikan Islam harus didasarkan pada al-Qur'an dan Hadits serta pemikiran rasional yang telah diuji validitasnya. Spektrum manajemen pendidikan Islam meliputi lingkup manajemen personalia pendidikan Islam, manajemen peserta didik pendidikan Islam, maanjemen kurikulum pendidikan Islam, manajemen keuangan pendidikan Islam, manajemen sarana dan prasarana pendidikan Islam, mana...

  7. PRODUKSI NANOFIBER DAN APLIKASINYA DALAM PENGOLAHAN AIR

    OpenAIRE

    Krisnandika, Vania Elita

    2017-01-01

    Abstrak Kebutuhan air meningkat seiring meningkatnya jumlah penduduk dan taraf kehidupan masyarakat. Pembangunan yang dilakukan secara terus-menerus dan sangat cepat di Indonesia mengakibatkan penurunan kualitas air permukaan. Teknologi membran merupakan salah satu teknologi pengolahan air yang menghasilkan produk dengan kualitas tinggi. Membran berstruktur nano, khususnya nanofiber, saat ini menjadi perhatian karena menjawab kebutuhan teknologi filtrasi yang efektif dan hemat biaya. Pr...

  8. DETEKSI DAN MANAJEMEN REFEEDING SYNDROME

    Directory of Open Access Journals (Sweden)

    Darmadi Darmadi

    2012-09-01

    Full Text Available AbstrakRefeeding syndrome (RFS dideskripsikan sebagai perubahan biokimiawi, manifestasi klinis dan komplikasi sebagai konsekuensi pemberian nutrisi pada pasien kurang gizi. Refeeding syndrome ini menyebabkan dampak buruk dan kematian. Sindroma ini lebih sering terjadi pada kelompok risiko. Refeeding syndrome merupakan suatu sindroma yang sering tak terdiagnosis oleh karena itu perlu peningkatan pengetahuan dan kesadaran dari tenaga medis untuk mengurangi morbiditas dan mortalitas dari RFS. Karena alasan tersebut ditulis tinjauan pustaka ini yang akan membahas mengenai patofisiologi, faktor risiko, manifestasi klinis, dan manajemennya.Kata kunci : refeeding syndrome, kurang gizi, hipofosfatemia, dukungan nutrisiAbstractRefeeding syndrome (RFS describel as biochemical changes, clinical manifestations, and complications that can occur as a consequence of feeding a malnourished individual. RFS can result in serious harm and death. RFS more commonly occurs in at-risk populations. Increased awareness amongst healthcare professionals is likely to reduce morbidity and mortality. This review examines the pathophysiology, risk factors, clinical manifestations, and management of RFS.Key word : refeeding syndrome, malnourished, hypophosphatemia, nutritional support

  9. Islam, Media, dan Politik : Sebuah Perdebatan dan Kontempelasi Nilai Berdemokrasi

    Directory of Open Access Journals (Sweden)

    Idil Akbar

    2016-10-01

    Full Text Available Infact, press or media is one of pilar democracy. Media in democracy is a public sphere to communi-cation and makes relation, and a same time as public arena to gain information. But, media also could not release from streotypes and tendency that usually bring of interest, either the owner or ideology. It is meaning media can not released from perspective distorsion, values bias and take a side. Media also effective to become propaganda instrument for a political interest and an ideology. It is seen like how media in US, for example, stereotype of Islam in discourses contradiction and glob-al interest opposition. Then, Islam dominantly identified as doctrine teaches radicalism, fundamen-talism and terorism. Thus, it is often be justification for US to operate the military mission in the name of democracy. Tak dipungkiri pers atau media menjadi salah satu pilar bagi demokrasi. Media dalam demokrasi adalah sebagai ruang bagi publik berkomunikasi dan berinteraksi, sekaligus sarana publik mem-peroleh informasi tentang banyak hal. Namun, media juga tak bisa dilepaskan dari stereotip dan kecenderungan-kecenderungan, yang biasanya membawa kepentingan, baik pemilik maupun ide-ologi. Media karenanya tak lepas dari distorsi perspektif, bias nilai dan berpihak. Media juga efektif menjadi alat propaganda bagi sebuah kepentingan politik dan ideologi, seperti bagaimana media di negara Amerika, misalnya, menstereotipkan Islam dalam analisis pertentangan wacana dan kepent-ingan global. Sehingga, dominan Islam diidentikkan dengan sematan sebagai ajaran yang mengajarkan radikalisme, fundamentalisme dan terorisme. Karenanya pula seringkali menjadi alasan pembenar bagi Amerika untuk menjalankan misi militer atas nama demokrasi.

  10. PROFIL DAN KARAKTER SOSIAL EKONOMI PETANI TANAMAN PANGAN DIBOJONEGORO

    Directory of Open Access Journals (Sweden)

    Kuntoro Boga Andri

    2014-10-01

    Full Text Available ABSTRAKPetani Bojonegoro saat ini didorong untuk meningkatkan kesejahteraan mereka dengan cara optimalisasi pertanian, revitalisasi agribisnis, diversifikasi pertanian dan fasilitasi dari pemerintah daerah. Penelitian  ini bertujuan untuk mengetahui profil petani di Kabupaten Bojonegoro yang berisi tentang kondisi petani, kepemilikan lahan, pendapatan dan potensi yang dimiliki, serta menganalisis faktor-faktor penentu yang mempengaruhi perilaku petani dan kondisi sosial ekonomi mereka. Penelitian dilaksanakan dengan memahami dan mengelola data sekunder maupun data primer untuk kemudian dianalisis deskriptif dan finansial untuk mengetahui profil petani dalam usaha bidang petanian, sehingga mampu memberikan solusi dalam upaya meningkatkan pendapatan dan kesejahteraan petani. Hasil analisa usahatani menggambarkan sebagian besar komoditas tanaman pangan yang diusahakan oleh petani di Kabupaten Bojonegoro sudah memberikan tingkat keuntungan yang sangat memuaskan. Meski demikian masih diperlukan optimalisasi penerapan teknologi dan input pertanian agar  potensi  unggulan dapat dimaksimalkan dengan intervensi  berbagai  program meliputi  keseluruhan  proses  mulai  dari  on  farm/ produksi/ hulu  sampai  off  farm/industri/ hilir dan permodalan usahatani.ABSTRACTFarmers in Bojonegoro are currently supported to improve their welfare by means of optimization of agriculture, revitalize agribusiness, agricultural diversification and facilitation of the local government. This study aims to determine the profile of farmers in Bojonegoro which contains the conditions of farmers, land ownership , revenue and potential, and to analyze the determinants that influence the behavior of farmers and their socio-economic conditions. The experiment was conducted with the understanding and managing secondary data and primary data for the analysis to determine the financial and descriptive profile of farmers in the business of agricultural fields

  11. Musisi Sekuler dan Gerejawi

    Directory of Open Access Journals (Sweden)

    Benny Cristovel

    2007-12-01

    Full Text Available Menjadi seorang musisi tidak sekedar bermain musik atau menyanyi saja. Ada jenjang-jenjang yang akan dilewatidalam dunia musik, yang pada akhirnya setiap musisi dihadapkan kepada tanggung jawab dalam dunia tersebut. Di jaman ini, jika jenjang seorang musisi sudah tahap profesional, maka musik dan bisnis merupakan hal yang tidak terpisahkan. Jadi tidak heran jika ada banyak orang yang memimpikan untuk berkarier dalam bidang musik, bahkan telah men1adicita-cita sejak kecil.Jadi penting bagi musisi gerejawi benar-benar "mengkotakkan dirinya" terhadap persepsi yang dianut oleh musisi sekuler, bukan mencampurkannya. Hal ini sangat esensial, karena musisi gerejawi bukan melayani manusia melainkan oleh anugerah Tuhan dipercayakan pekerjaan ini. Dengan demikian pelayanan sebagai musisi gerejawi tidak tercemar oleh persepsi dari dunia musik sekuler. Selain itu musisi gerejawi dapat merefleksikan Tuhan yang disembahnya kepada dunia sekuler, karena tujuan dari semua yang dilakukannya adalah untuk kemuliaan nama Tuhan.

  12. QUESTION ANSWERING SYSTEM DAN PENERAPANNYA PADA ALKITAB

    Directory of Open Access Journals (Sweden)

    Gunawan Gunawan

    2006-01-01

    Full Text Available Question answering system is a system that allows user to state his or her information need in the form of natural language question, and return short text excerpts or even phrases as an answer. The availability of a wide and various information source and improvements in the techniques of natural language processing, information extraction (wrapper, and information retrieval give a big effect on the development of question answering system, from just answering questions in a specific domain by consulting to structured information source such as database, and like in this research, answering any questions based on information stored in an unstructured text collection. A general architecture of question answering system based on text consists of six processing stages, i.e. question analysis, document collection preprocessing, candidate document selection, candidate document analysis, answer extraction, and response generation. Application of question answering system like AnswerBus, Mulder, and Webclopedia that are developed with its own characteristics has similar processing steps as in the general architecture. Answers returned by a question answering system need to be evaluated for performance measure. This research completed with a simple question answering system application using english Bible in World English Bible (WEB version as the source of information to answer some questions. Because specific domain is selected: Bible, questions that can be posed by user could ask about information in the Bible itself only. Question is also limited to three types of answers that can be supported by the application: person (who, location (where, and date (when. Abstract in Bahasa Indonesia : Question answering system (QA system adalah sistem yang mengijinkan user menyatakan kebutuhan informasinya dalam bentuk natural language question (pertanyaan dalam bahasa alami, dan mengembalikan kutipan teks singkat atau bahkan frase sebagai jawaban. Ketersediaan

  13. Argumen Eksistensi Tuhan Dalam Metafisika Ibn Rusyd Dan St. Thomas Aquinas

    Directory of Open Access Journals (Sweden)

    Wardani Wardani

    2015-06-01

    Full Text Available Abstract : To establish an argumentation for the existence of God is properly the most crucial as well as complicated effort in the life of religion and faith of human being. There are various approaches and methods have been applicated to reach it by theologians, thinkers, and scientists, including philosophers with their demonstrative-philosophical method. Some arguments which were initiated by Aristotle are ones of the most popular and have been adopted and improved as well by many thinkers and philosophers after him, some arguments which proposed by Ibn Rusyd and St. Thomas Aquinas with some modifications and improvisations are the best examples of it. In the case of elaboration and analysis toward those arguments for the existence of God, this article attempts to compare between metaphysical thought of Ibn Rushd (well-known in the West as Averroës and St. Thomas Aquinas. There is no doubt that both are Aristotelian in their philosophy. Therefore, to seek the similarities and differences, and to analyze the influence of Aristotle on their modes of thought, especially in argumentation for the existence of God, are an urgent point in the way to find more stronger and relevant arguments.Keywords: argument of creation (dalīl al-ikhtirā`, teleological argument (dalīl al-‘ināyah, unmoved mover, prime cause, influence, parallelism.Abstrak : Menggagas argumentasi tentang eksistensi Tuhan sejatinya merupakan upaya yang paling krusial sekaligus pelik dalam kehidupan beragama dan kepercayaan umat manusia. Berbagai pendekatan dan metode telah ditempuh untuk meraihnya oleh para teolog, pemikir, dan ilmuwan, termasuk para filsuf dengan pendekatan dan metode demonstratif-filosofisnya. Argumen-argumen yang diprakarsai oleh Aristoteles adalah diantara yang paling populer dan telah diadopsi serta dikembangkan oleh para pemikir dan filsuf setelahnya, tak terkecuali argumen-argumen yang Ibn Rusyd dan St. Thomas Aquinas kemukakan dengan segenap modifikasi

  14. PENGELOLAAN ZAKAT OLEH NEGARA DAN SWASTA Studi Efektifitas dan Efisiensi Pengelolaan Zakat Oleh BAZ Dan LAZ Kota Madiun

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    Atik Abidah

    2010-12-01

    Full Text Available Abstraks: Keberadaan lembaga zakat di Indonesia yang diakui oleh perundang-undangan ada dua, yaitu Badan Amil Zakat (BAZ dan Lembaga Amil Zakat (LAZ. BAZ adalah lembaga zakat yang dikelola oleh pemerintah, sedangkan LAZ adalah lembaga yang dikelola oleh masyarakat. Artikel ini merupakan merupakan hasil penelitian lapangan dengan menggunakan pendekatan kualitatif. Data digali langsung dari BAZ Kota Madiun dan LAZ dalam hal ini ada 2 lembaga, yaitu Lembaga Manajemen Infaq (LMI dan Baitul Maal Hidayatullah (BMH. Hasil penelitian BAZ lebih efektif dibanding LAZ, karena BAZ di bawah naungan Pemerintah Kota Madiun dan didukung dengan kebijakan dalam menjalankan progam kerjanya. Sedangkan pada LAZ (LMI dan BMH karena sifatnya mandiri, maka segala sesuatunya akan efektif jika mereka bekerja keras, dan itulah yang selama ini dilakukan oleh LMI dan BMH, sehingga sampai saat ini mereka masih eksis.

  15. INTERAKSI DAN HARMONI UMAT BERAGAMA

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    Joko Tri Haryanto

    2012-05-01

    Masyarakat Singkawang adalah masyarakat yang terdiri atas berbagai kelompok suku bangsa dan agama. Secara historis, masyarakat Singkawang mampu mem­pertahankan harmoni antar agama. Model interaksi sosial yang bersifat asosiatif tampaknya potensial untuk mendukung harmoni di dalam masyarakat. Ber­dasarkan paradigma fungsional-struktural, masyarakat diasumsikan sebagai sistem organik yang memiliki huungan antar bagiannya untuk mempertahankan masyarakat. Interaksi sosial di dalam masyarakat Singkawang dikembangkan melalui interaksi di dalam lingkup keluarga, lingkungan sekitar, aktifitas ekonomi, para pimpinan agama, dan hubungan di dalam lingkup budaya dan tradisi. Meskipun demikian, hubungan antar unsur masyarakat masih kosmopolitan, yang di dalamnya anggota masyarakat kurang aktif dalam mengembangkan harmoni masyarakat.

  16. The study by means of a photomultiplier of the scintillations produced by {alpha} particles striking a zinc sulphide screen; Etude, au photomultiplicateur, des scintillations produites par les particules {alpha} dans un ecran de sulfure de zinc. Application a la numeration precise des particules {alpha}

    Energy Technology Data Exchange (ETDEWEB)

    Anthony, J P [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1955-06-15

    The object of the study is the accurate counting of {alpha} particles by p-m. detection of their scintillations upon impact with a zinc sulphide screen. The main advantage of the method is the extreme simplicity of the electronics used: the possibility of obtaining a utilizable pulse from the p-m. (EMI5311) without any amplification, and in linear response, is demonstrated. The scintillation produced by an impact on Zn-S has also been studied experimentally. The decrease of light intensity in relation to time may be interpreted by the exponential relation: I = I{sub 0} exp (-t / {tau}) whereby {tau} = (39 {+-} 0,1) 10{sup -6} s. The relation between scintillation intensity and remaining trajectory after travel through a given air-space has also been determined. Possible suitable applications of this method of {alpha} counting are those where good stability and low background are necessary. Results stated bear on air contamination studies, isotopic composition variation measurement of uranium, bismuth content measurement in alloys by irradiation of specimens in a thermal neutron flux and {alpha} count on the Po formed. (author) [French] Ce travail est consacre a l'etude de la numeration precise des particules {alpha} par detection au photomultiplicateur des scintillations produites par ces particules dans un ecran de sulfure de zinc. Le principal avantage de cette methode reside dans l'extreme simplicite de l'appareillage electronique; il est en effet montre qu'il est possible, tout en convoyant une reponse lineaire, d'obtenir du photomultiplicateur (EMI5311) un signal electrique utilisable sans aucune amplification. La scintillation produite par l'impact des particules {alpha} sur un ecran de Zn-S est etudiee experimentalement. La decroissance de l'intensite lumineuse en fonction du temps est interpretable par la relation exponentielle I = I{sub 0} exp (-t / {tau}) avec {tau} = (39 {+-} 0,1) 10{sup -6} s. La relation entre l'intensite de la scintillation et le

  17. ETIKA BISNIS AL-GHAZALI DAN ADAM SMITH DALAM PERSPEKTIF ILMU BISNIS DAN EKONOMI

    Directory of Open Access Journals (Sweden)

    AM. M. Hafidz MS.

    2013-05-01

    Full Text Available Penelitian ini adalah untuk mengeksplorasi: (1 pembangunan etika bisnis yang telah dirumuskan oleh al-Ghazali dan Adam Smith, (2 persamaan dan perbedaan antara dua etika bisnis pria, dan (3 relevansi bisnis mereka etika bisnis modern dunia dan ekonomi. Bisnis etika dibangun oleh al-Ghazali dan Smith di dataran praksis tidak jauh berbeda. Etika bisnis konstruksi dibangun oleh al-Ghazali didasarkan pada prinsip-prinsip seperti orientasi itikad baik tentang dunia dan akhirat, kejujuran, kepentingan pribadi dan social keseimbangan, dan perilaku / perbuatan yang tepat. Di sisi lain, etika bisnis konstruksi dibangun oleh Smith, berdasarkan keadilan, altruisme, keadilan dan liberal (kebebasan ekonomi. Baik etika bisnis yang diperkenalkan oleh kedua sangat relevan untuk menjadi digunakan sebagai bahan pokok acuan dalam etika bisnis modern.

  18. Pengembangan Sistem Otomatisasi AC dan Lampu Menggunakan Fuzzy dan Raspberry Pi

    Directory of Open Access Journals (Sweden)

    Rudy Ariyanto

    2017-11-01

    Full Text Available Otomatisasi AC dan lampu dilakukan untuk menghemat energi yang digunakan pada kehidupan sehari-hari. Dalam pengembangan otomatisasi AC dan lampu perlu menerapkan sebuah perangkat yang memiliki fungsi maksimal dengan harga yang minimal. Raspberry Pi merupakan perangkat atau modul dengan harga rendah yang mampu melakukan komunikasi wireless tanpa bantuan modul lain. Dalam pengembangan otomatisasi AC dan lampu juga diperlukan sebuah metode yang mampu melakukan kontrol terhadap nyala AC dan lampu. Penerapan metode fuzzy dapat dilakukan untuk menghimpun informasi keadaan ruang yang didapat dari sensor untuk menentukan nyala AC dan lampu secara otomatis. Oleh sebab itu pada penelitian ini mengusulkan pengembangan otomatisasi AC dan lampu menggunakan Raspberry Pi dan Fuzzy. Otomatisasi AC dan lampu menggunakan Raspberry Pi yang menerapkan metode Fuzzy dapat menghemat energi hingga 59,87% dalam hal lama waktu nyala AC dan 57,47% untuk lumenasi lampu

  19. Sistem Informasi Penjualan dan Pemesanan Layanan Berbasis Web dan SMS Gateway di Petshop "PetZone"

    Directory of Open Access Journals (Sweden)

    Siska Fadhilah Wati

    2013-09-01

    Full Text Available Dewasa ini teknologi informasi sangat membantu dalam dunia bisnis. Kemudahan yang ditawarkan akan menjaring lebih banyak konsumen. Namun, perusahan tingkat menengah seperti PetZone saat ini masih jarang yang menawarkan kemudahan berbelanja atau pemesanan layanan secara online. Oleh karena itu diperlukan sebuah sistem berbasis web di perusahaan PetZone yang dapat memudahkan pemilik dan karyawan dalam apenjualan, pelayanan, dan pemasaran, serta memudahkan pelanggan dalam jual-beli barang dan jasa. Atas dasar masalah tersebut dibangun Sistem Informasi Penjualan dan Pemesanan Layanan Berbasis Web dan SMS Gateway untuk menunjang proses bisnis yang ada. Sistem informasi dibangun menggunakan bahasa pemrograman PHP framework Codeigniter, javascript untuk tampilan yang dinamis, dan database MySQL. Proses pembuatan dan pengembangan Sistem Informasi Penjualan ini menggunakan metode air terjun. Metode air terjun meliputi kebutuhan pengguna, analisis, rancangan, implementasi dan pengujian. Pemodelan Sistem Informasi yang dibangun menggunakan metode berorientasi objek UML (Unified Modeling Language yang terdiri dari Use case  diagram, Class diagram dan Sequence diagram. Hasil pengujian Sistem Informasi Penjualan dan Pemesanan Layanan Berbasis Web dan SMS Gateway menunjukkan bahwa semua fitur yang terdapat baik dalam sistem informasi maupun SMS gateway dapat bekerja dengan baikdengan ratusan sample data, dan server SMS gateway dapat memproses lebih dari satu SMS secara bersamaan. Dalam perkembangan ke depannya nanti, Sistem Informasi Penjualan dan Pemesanan Layanan Berbasis Web dan SMS Gateway masih dapat dikembangkan lagi dengan menambah fitur-fitur pada SMS gateway sehingga lebih memudahkan konsumen.

  20. Efikasi Kendiri: Perbandingan Antara Islam dan Barat

    Directory of Open Access Journals (Sweden)

    Noornajihan, J.

    2014-12-01

    Full Text Available Terminologi efikasi kendiri (EK merupakan terminologi yang diperkenalkan dalam ilmu psikologi sekitar tahun 70-an. Namun, istilah ini masih kurang difahami oleh kebanyakan individu terutama mereka yang bukan berlatar belakangkan bidang psikologi. Oleh itu, satu keperluan hasil penulisan ini diketengahkan, memandangkan konsep ini penting dalam diri setiap individu bagi memacu kecemerlangan diri. Justeru, kertas kerja ini akan mengupas serba ringkas mengenai konsep EK dari perspektif Islam dan Barat, dengan melihat kepada beberapa titik persamaan dan perbezaan antara kedua-dua pandangan. Islam dan Barat bersetuju bahawa individu yang memiliki EK yang tinggi merupakan individu yang berfikiran positif, berani mengambil risiko dan tidak mudah berputus. Namun pandangan Islam terhadap konsep ini lebih luas, kerana Islam mengaitkan konsep ini dengan konsep tauhid uluhiyyah dan konsep manusia sebagai ahsan al-taqwim. Oleh demikian, EK dari perspektif Islam lebih bersifat kekal dan umum, di samping individu yang berefikasi tinggi menurut Islam ialah individu yang memiliki sifat sabar, syukur, redha dan redha.

  1. PERANCANGAN DAN PENGEMBANGAN PROTOTYPE SISTEM PARKIR

    Directory of Open Access Journals (Sweden)

    Indah Ayu Septriyaningrum

    2016-10-01

    Abstrak  Sistem parkir manual pada pelayanan parkir mall memerlukan pengelolaan dan pengembangan sistem yang lebih rumit dan jauh dari kata efisien. Informasi yang didapatkan pengelola parkir terkait kondisi parkir di lapangan setiap harinya masih kurang. Tujuan dari penelitian ini adalah merancang dan mengembangkan prototype sistem parkir. Metode pengembangan dan perancangan sistem pada penelitian ini adalah metode Waterfall. Hasil yang didapatkan adalah sistem ini dapat mendeteksi keberadaan mobil pada slot parkir yang tersedia dengan bantuan Intel Galileo Board Gen 2 sebagai kontroler, sensor LDR (Light Dependent Resistor dan sensor ultrasonik (PING sebagai alat bantu pendeteksi keberadaan mobil. Sistem dapat menampilkan aktifitas parkir pada aplikasi web seperti kondisi lahan parkir kosong, lahan terisi, waktu masuk, waktu keluar, lama parkir dan kapasitas parkir yang tersedia serta grafik pemakaian lahan parkir. Dapat disimpulkan bahwa perancangan dan pengembangan sistem berhasil diimplementasikan. Kata Kunci : Sistem parkir, waterfall, Intel Galileo Board Gen 2,sensor LDR (Light Dependent Resistor, sensor ultrasonik

  2. PENGEMBANGAN MOBILE ADVERTISING SEBAGAI SARANA PROMOSI TOKO ROTI DAN KUE MENGGUNAKAN LOCATION BASED SERVICE

    Directory of Open Access Journals (Sweden)

    Ika Arfiani

    2016-07-01

    Full Text Available Pertumbuhan pengguna layanan mobile data dan mobile internet di Indonesia meningkat pesat dibandingkan voice dan sms. Sehingga kehidupan manusia bagai tak terpisah antara jarak, tempat, dan waktu. Dengan mudahnya manusia dapat melakukan komunikasi dan mengakses informasi tak peduli dimanapun dia tempatnya. Apalagi dengan beragamnya alat komunikasi yang kini beredar ditengah masyarakat, salah satunya adalah smartphone android. Permasalahan yang umum dihadapi adalah bagaimana membangun suatu aplikasi pada platform Android untuk pencarian lokasi toko roti dan kue beserta alamatnya. Hal tersebut telah terjawab dengan adanya sistem operasi android yang open source, Dengan adanya aplikasi ini maka pengguna yang mempunyai tingkat kesibukan atau mobilitas yang tinggi tidak perlu lagi mencari lokasi toko roti dengan mencari ataupun bertanya dimana lokasi toko roti yang terdekat, karena Aplikasi ini telah menyediakan fitur pencarian secara lengkap, sehingga pengguna dapat mencari lokasi toko roti yang terdekat kapanpun dan dimanapun hanya dengan ponsel Android yang dimilikinya. Kelebihan aplikasi ini dapat digunakan untuk membantu mencari lokasi toko roti dan kue berdasarkan jenis tokonya serta lokasi yang terdekat dari posisi kita berada. Aplikasi ini akan menampilkan secara detail informasi dari toko yang ada berupa nama, alamat, nomor telepon, gambar / foto dan tampilan peta yang bersumber dari Google Maps.Hasil pengujian sistem menunjukkan bahwa aplikasi dapat memberikan informasi lokasi toko kepada pengguna, melakukan panggilan telepon ke toko yang dituju, melakukan share promosi, serta menampilkan map sekaligus rute terpendek menuju lokasi merchant yang ingin dituju. Rute terpendek yang didapat telah mampu menemukan lokasi tujuan dengan jarak yang relative pendek dan tergambar dalam google map. Kata Kunci : Android, Mobile Application, Rute Terpendek, Location Based Service,

  3. Identifikasi dan Tingkat Penerapan Inovasi Teknologi Padi Sawah di Kabupaten Parigi Moutong Sulawesi Tengah

    Directory of Open Access Journals (Sweden)

    Syafruddin Syafruddin

    2016-07-01

    Full Text Available Pencapaian tingkat swasembada dan ketahanan pangan khususnya beras tidak terlepas dari beberapa dukungan seperti sumberdaya alam dan penerapan inovasi teknologi. Kabupaten Parigi Moutong merupakan salah satu wilayah penghasil beras yang cukup besar di Sulawesi Tengah yang diharapkan dapat menjadi sumber pertumbuhan baru produksi beras Nasional di Indonesia. Pemerintah Daerah menetapkan wilayah ini, sebagai daerah penyangga beras terbesar di Sulawesi Tengah. Tujuan dari Penelitian ini adalah untuk : 1. Mengidentifikasi berbagai permasalahan dan tingkat penerapan inovasi teknologi pertanian di Kabupaten Parigi Moutong dan 2. Menetapkan arahan dan alternatif teknologi yang potensial untuk pengembangan lahan di Kabupaten Parigi Moutong. Penelitian ini dilaksanakan sebanyak dua tahap yaitu tahap 1 Desk study dan 2. Penelitian Lapangan. Desk study dilakukan dengan cara penelusuran pustaka dan diskusi dengan stake holders lainnya. Untuk Penelitian lapangan dilaksanakan dengan menggunakan metode survey dengan melakukan pengamatan kondisi sosial ekonomi dan budaya serta pengamatan tingkat penerapan inovasi teknologi melalui pendekatan Partisifatif Rural Aprasial atau Pengenalan Desa Secara Partisifatif (PRA. Pelaksanaan penelitian dilakukan selama 2 bulan yaitu dari bulan Juni hingga bulan Juli 2014. Hasil penelitian menunjukkan bahwa terdapat potensi perluasan areal persawahan dan peningkatan luas tanam karena didukung oleh iklim dan irigasi yang cukup baik. Tingkat penerapan teknologi masih cukup rendah terutama penggunaan varietas unggul, benih unggul dan bermutu serta pemupukan. The achievement level of self-sufficiency and food security, particularly in rice production should be supported by natural resources and the application of technology innovation.  Parigi Moutong Regency is one of the largest rice producer areas in Central Sulawesi, which is expected to be a new growth source area of national rice production in Indonesia. Local government

  4. Application d’une approche inspirée des colonies de fourmis pour la recommandation des chemins d’apprentissage dans un cours en ligne : modèle et expérience

    Directory of Open Access Journals (Sweden)

    Aziz Dahbi

    2014-01-01

    Full Text Available Dans cet article, nous présentons la mise en œuvre, l’expérimentation et l’évaluation d’une approche pour la recommandation des chemins d’apprentissage dans un cours en ligne. Le processus de recommandation est inspiré de l’intelligence en essaim et plus particulièrement de l’optimisation par colonies de fourmis (OCF (ant colony optimization [ACO]. Dans ce contexte, nous avons considéré une différenciation des chemins d’apprentissage en fonction de l’activité explorée pour l’apprentissage d’un cours. Dans l’objectif de recommander des chemins d’apprentissage considérés optimaux et d’évaluer ainsi leur impact sur l’apprentissage d’un cours en ligne, l’approche proposée est basée à la fois sur la recommandation de chemins pertinents par l’enseignant et sur les résultats stockés au fur et à mesure par les apprenants sur les chemins empruntés. Notre approche a été validée expérimentalement et les résultats obtenus ont montré l’émergence d’un chemin d’apprentissage favorisant la réussite d’un nombre d’apprenants relativement considérable.

  5. Efektivitas Weblog dan Facebook Terintegrasi untuk Pembelajaran Virtual

    OpenAIRE

    Hartono

    2014-01-01

    Abstrak: Saat ini, banyak mahasiswa menghabiskan waktu mereka di internet. Mereka melakukan kegiatan seperti membuat blog, mengunduh, mengunggah, chatting, dan berinteraksi melalui facebook. Mahasiswa sekarang ini hidup dengan teknologi. Penelitian menunjukkan bahwa weblog dan facebook berpotensi mendukung belajar dan mengajar. Guru dan pendidik menggunakan kegiatan tersebut untuk meningkatkan kualitas belajar. Penelitian ini bertujuan untuk mengetahui efektivitas weblog dan facebook ketika d...

  6. POPULATION ET SANTÉ DANS LES PAYS EN DÉVELOPPEMENT

    International Development Research Centre (IDRC) Digital Library (Canada)

    aux applications en harmonie avec les stratégies et les pratiques élaborées. ...... ainsi que de recrutement et de formation du personnel de terrain, notamment des ..... des stratégies en matière de services ou des politiques, ce qui nécessite la ..... La vérification des données est aussi entreprise dans le but de détecter les ...

  7. Application of indoxacarb for managing shoot and fruit borer of eggplant (Solanum melongena L.) and its decontamination.

    Science.gov (United States)

    Saimandir, Jayakrishnan; Gopal, Madhuban

    2009-03-01

    Indoxacarb was applied at 75 and 150 g a.i. ha(-1) for two years to an eggplant (Solanum melongena L.) crop grown in the field plots in order to evaluate its efficacy for management of the lepidopteron pest, shoot and fruit borer. The residues of the insecticide were quantified by high-pressure liquid chromatography (HPLC). The mean initial deposits of indoxacarb on eggplant fruits were found to be 2.60-2.634 mg kg(-1) and 3.64-3.68 mg kg(-1) from the two rates of applications, respectively. They declined with time and reached to non-detectable (indoxacarb was found to be by washing with a mixture of alkali and potassium permanganate (KMnO(4)) thereby resulting in the removal of 67.5% and 59.2 % residues for 5 and 10 microg g(-1) spiking doses, respectively. Major products formed on reaction of indoxacarb with alkali were identified by electron spray ionization chromatography/mass spectrometry (ESI/MS). The per cent reduction on the weight and number basis of treated eggplant plots were compared to those observed in control plots to demonstrate the effectiveness of indoxacarb treatment on shoot and fruit borer population.

  8. Pro-Kontra Hukuman Mati (Presepsi Tokoh Agama Islam dan Praktisi Hukum di Kota Palembang

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    Qodariyah Barkah

    2016-03-01

    Full Text Available Penelitian ini merupakan hasil penelitian yang membahas tentang pro-kontra hukuman mati, dengan memfokuskan kajian kepada presepsi tokoh agama agama Islam dan praktisi hukum di kota Palembang. Penelitian ini menyimpulkan bahwa Hukuman mati dalam persfektif hukum pidana di Indoneia adalah tertuang dalam Kitab Undang-undang Hukum Pidana (KUHP dan perundang-undangan lainnya yang memuat tentang hukuman mati, antara lain didalam Pasal 10 dan Pasal 11 KUHP. Hukuman pidana mati penerapannya di Indonesia menurut perspektif Tokoh Agama Islam dan praktisi hukum di kota Palembang masih terjadi pro dan kontra. Baik dikalangan praktisi hukum sendiri terjadi pro dan kontra, apakah hukuman pidana mati masih diperlukan penerapannya begitu juga dengan kalangan Tokoh Agama Islam. This article discusses the pros and cons of the death penalty, with a focus on the study of the perception of Islam and religious leaders, legal practitioners in the city of Palembang. This study concluded that the death penalty in criminal law perspective at Indoneia is contained in the Code of Criminal Law (Penal Code and other legislation that contains about the death penalty, among others in Article 10 and Article 11 of the Criminal Code. Penalty death penalty application in Indonesia from the perspective of Islamic religious leaders and legal practitioners in the city of Palembang is still going on pros and cons. Both among legal practitioners itself there are pros and cons, whether the punishment of the death penalty is still necessary application as well as the Islamic Religious Leaders.

  9. Meningkatkan Kemandirian Belajar dan Hasil Belajar Siswa melalui Pengembangan Modul Administrasi Kepegawaian Berbasis Strategi Pembelajaran Inkuiri Terbimbing

    Directory of Open Access Journals (Sweden)

    Kharisma Swandhana

    2016-11-01

    Full Text Available Abstract: This research and development aimed to produce a module of Employee Administration based on Guided Inquiry Learning Strategy for the twelfth grade students of Office Administration program, to determine the feasibility of the module developed through validation, and to know whether there is an improvement towards independent learning and students’ ourcomes before and after using the module This research and development used 4D model. It consisted of 4 stages of development: define, design, develop, and disseminate. It was obtained the average sore of post-test 91.76 in the experimental class, and the results of material and module validation reached 90.66% and 88.30%.  The result of questionnaire distribution of independent learning using the module showed 90%. Thus, from the results of this research showed that the Employee Administration module was applicable and able to improve independent learning and students’ outcomes. It was suggested to use this module as a supporting alternative for learning Employee Administration, specifically on material of discharging employees and pension. ABSTRAK: Penelitian dan pengembangan ini bertujuan untuk menghasilkan bahan ajar berupa Modul Administrasi Kepegawaian Berbasis Strategi Pembelajaran Inkuiri Terbimbing untuk siswa SMK kelas XII Program Keahlian Administrasi Perkantoran., mengetahui kelayakan modul yang telah dikembangkan melalui hasil validasi, dan mengetahui apakah terjadi peningkatan kemandirian belajar dan hasil belajar siswa sebelum dan sesudah menggunakan modul. Penelitian dan pengembangan ini dilakukan dengan menggunakan 4D model. Model ini terdiri dari 4 tahap pengembangan, yaitu define, design, develop, dan disseminate. Diperoleh hasil rata rata nilai post test 91,76 pada kelas eksperimen, hasil validasi oleh ahli materi dan ahli modul mencapai hasil 90,66% dan 88,30%, hasil penyebaran angket kemandirian belajar siswa dengan menggunakan modul juga mencapai persentase 90

  10. APLIKASI ANIMASI INTERAKTIF PENCAMPURAN TIGA WARNA PRIMER DAN PENGENALAN BENTUK GEOMETRI PADA PAUD AL-MUSLIMUN

    Directory of Open Access Journals (Sweden)

    Mayya Nurbayanti Shobary

    2016-03-01

    Full Text Available Abstract - The development of Interactive animation application mixing three colors and introduction of geometric shapes for early childhood, aims to increase learning tool for parents and teachers to attract the attention of children to learn about colors and shapes using interactive animation application. Application built using the concept of PAUD Al-Muslimun in educating early childhood in knowing the result of mixing three primary colors and geometric shapes. The development of application take an example of how theachers in educating early childhood that began with the introduction of color and shapes, and practice how to mix the primary three colors, by showing interisting picture related to colors and shapes are introduced. Data collection methods used for this study is the direct observation of the teaching and learning activities from the perspective of teachers, children and parents to get an idea of the optimal design of an application built on. The development of Interactive animation application mixing three primary colors and introduction of geometric shapes for early childhood for early childhood through the five steps, analyzing, designing, implemeting, testing, and revision errors or shortfall. In this application there are learning processes knowing the primary color and introduction of geometric shapes with support interactive buttons, interesting picture and audio to enhance the absorption of early childhood to the contents of the material, learning and display concerned and to help parents or teachers role in educating children once more creative . Keywords: Applications, Animation, Interactive, Early Childhood Abstrak - Pembangunan aplikasi animasi interaktif pencampuran tiga warna primer dan pengenalan bentuk geometri untuk anak usia dini, bertujuan untuk menambah sarana pembelajaran untuk orang tua dan guru dalam menarik perhatian anak untuk belajar mengenal warna dan bentuk dengan menggunakan aplikasi animasi interaktif

  11. Lõuka tuuliku restaureerimine / Dan Lukas

    Index Scriptorium Estoniae

    Lukas, Dan

    2005-01-01

    Hiiumaal Pühalepa vallas Vahtrepa külas Lõuka talu maadel asuva pukktuuliku ajaloost, restaureerimise käigust. Teostus: Dan Lukas. Muinsuskaitseline järelevalve: Tõnu Sepp, tema kommentaar. Ill.:pukktuuliku lõiked ja korruste plaanid, 7 värv. fotot

  12. Internal Control: Peran Dan Perkembangannya

    OpenAIRE

    Murtin, Alek

    2000-01-01

    Perhatian terhadap pentingnya internal control dalam organisasi berjalan dari waktu ke waktu untuk meningkatkan fungsi internal control yang disesuaikan dengan perkembangan lingkungan organisasi, dimulai dengan adanya internal check, kemudian internal control system, internal control structure dan terakhir adalah internal control-integrated framework. Internal control system sempat berkembang beberapa tahun di Indonesia yang selanjutnya digantikan oleh internal control structure yang digunaka...

  13. Asuransi Takaful: Prospek Dan Tantangannya

    OpenAIRE

    Sobirin, Achmad; Muhtar, Muchsin

    1994-01-01

    Dewasa ini perhatian terhadap nilai-nilai syariah Islam terhadap muamalah khususnya di bidang ekonomi menjadi besar. Lembaga perekonomian yang terjalin dengan pranata keagamaan makin menggejala dimana-mana dan kini sedang tumbuh mencari bentuk untuk dapat diterima di tengah-tengah masyarakat.

  14. KETENTUAN TENTANG STANDAR PELAYANAN MINIMAL BIDANG KELUARGA BERENCANA DAN KELUARGA SEJAHTERA BERDASARKAN ASAS PERIKEMANUSIAAN DAN HAK ASASI MANUSIA

    Directory of Open Access Journals (Sweden)

    . Riyanti

    2017-01-01

    Hasil penelitian, ketentuan tentang standar pelayanan minimal bidang keluarga berencana, keluarga sejahtera dan asas perikemanusiaan dengan hak asasi manusia sangat berhubungan keterbatasan lingkup pelayanan dan standar pelaksanaan Komunikasi Informasi dan Edukasi yang tidak jelasberdampak pada tidak dipenuhinya hak asasi manusia untuk mendapatkan kesetaraan dan kebebasan dalam pelayanan keluarga berencana dan keluarga sejahtera.

  15. Geochemical modeling of water-gas-rock interactions. Application to mineral diagenesis in geologic reservoirs; Modelisation geochimique des interactions eau-gaz-roche. Application a la diagenese minerale dans les reservoirs geologiques

    Energy Technology Data Exchange (ETDEWEB)

    Bildstein, O

    1998-03-13

    The Ph.D. report describes a conceptual and numerical model for simulating gas-water-rock interaction during mineral diagenesis of sediments. The main specific features of this model are the following: applicable to open systems, half-implicit resolution numerical method, feedback on the texture evolution (grain model), existence of a gas phase, oxido-reduction phenomena. (author) 217 refs.

  16. KINERJA DAN EFISIENSI BANK PEMERINTAH (BUMN DAN BUSN YANG GO PUBLIK DI INDONESIA

    Directory of Open Access Journals (Sweden)

    Sugeng Haryanto

    2012-06-01

    Full Text Available Penelitian ini menganalisis kinerja dan tingkat efisiensi bank-bank BUMN dan BUSN yang go Publik di Bursa Efek Indonesia.  Sample penelitian ini mengambil  tiga bank BUMN Bank BNI 46, Bank Mandiri dan Bank BRI  dan tiga bank BUSN (Bank BCA, Bank Niaga dan Bank Panin dengan periode analisis tahun 2005-2011. Varibael yang digunakan meliputi ROA, ROE, LAR. LDR, NPL dan BOPO. Tujuan dari penelitian ini adalah melihat dan menganalisis perbedaan kinerja antara Bank BUMN dan BUSN yang go public di Bursa Efek Indonesia tahun 2005-2011.  Pendekatan pengukuran kinerja yang digunakan adalah Return on Asset (ROA, Return on Equity (ROE dan Loan to Deposit Ratio (LDR, Loan to Asset Ratio (LAR,  dan efisiensi bank. Hasil dari penelitian menunjukkan bahwa 1 Bank-bank nasional, baik itu bank BUMN maupun BUSN menunjukkan kinerja yang semakin baik, 2 tidak terdapat perbedaan yang signifikan antara kinerja bank BUMN dan BUSN untuk variabel ROA, ROE, LAR, LDR, dan BOPO sedangkan variabel NPL yang merupakan indikator risiko kredit menunjukkan adanya perbedaan yang signifikan antara Bank BUMN dan BUSN

  17. Kontrak Baku Franchise Ditinjau dari Ketentuan Unidroit dan KUH Perdata

    Directory of Open Access Journals (Sweden)

    Susiana Susiana

    2015-04-01

    Full Text Available ABSTRAK: Kontrak baku merupakan kontrak yang telah dipersiapkan oleh salah satu pihak, dimana pihak lain tidak memiliki andil dalam merumuskan isi kontrak. Kontak franchise sebagai salah satu jenis kontrak yang berkembang dalam praktek kontrak bisnis internasional dewasa ini, umumnya telah dibuat dalam bentuk baku. Dalam perdagangan internasional, khusus mengenai kontrak bisnis internasional berlaku ketentuan yang diatur dalam Unidroit. Di Indonesia, pembuatan kontrak diatur dalam KUH Perdata. Tulisan ini bertujuan untuk mengkaji dan menjelaskan prinsip-prinsip kontrak dalam Unidroit dan KUH Perdata serta melakukan analisis apakah kontrak franchise yang dibuat dalam bentuk kontrak baku tersebut bertentangan dengan prinsip-prinsip kontrak yang diatur dalam Unidroit dan KUHPerdata. Dari hasil kajian kepustakaan dapat dijelaskan bahwa prinsip-prinsip kontrak yang diatur dalam Unidroit Principle (UP antara lain: prinsip kebebasan berkontrak, itikad baik dan transaksi jujur, Prinsip kesepakatan melalui penawaran dan penerimaan, Prinsip perlindungan pihak lemah dari syarat-syarat baku, Prinsip contra proferentem dalam penafsiran kontrak baku.  Franchise Standardized Contract Viewed from the Rules of Unidroit and the Civil Code ABSTRACT: Standard contract is a contract which has been prepared by one of the parties, in which the other party has not participated in making the contract. Contract francise as one the the types of contracts that developed in the practice of today’s international business contracts, generally have been made in raw form. In international trade, especially regarding international business contracts applicable provisions laid down in Unidroit. In Indonesia, the manufacturing contract stipulated in the Civil Code. The result show that the contract principles set out in Unidroit Principle (UP, among other: the principle of freedom of contract, good faith and transaction honest (fair dealing. Principles of the agreement through

  18. KENDALI OPTIMAL DARI SISTEM INVENTORI DENGAN PENINGKATAN DAN PENURUNAN BARANG

    Directory of Open Access Journals (Sweden)

    P Affandi

    2016-03-01

    Full Text Available Terdapat banyak permasalahan yang melibatkan teori sistem dan teori kontrol serta aplikasinya. Contohnya, beberapa referensi teori  yang mengaplikasikan teori kontrol ke dalam masalah inventori. Masalah klasik dalam masalah inventori adalah bagaimana mengatur perubahan permintaan konsumen pada sebuah produk barang jadi. Selain mengalami penurunan yang disebabkan kerusakan dan kemerosotan, ternyata inventori juga bisa mengalami peningkatan. Biasanya, inventori yang mengalami peningkatan terjadi pada inventori yang melakukan proses produksi yang berlangsung secara terus menerus; Sedangkan permintaan sedikit juga terjadi pada inventori makhluk hidup yang mengalami perkembangbiakan. Selanjutnya, hal ini mengakibatkan terjadinya peningkatan jumlah inventori. Dapat disimpulkan bahwa secara teori, sistem Inventori dapat mengalami peningkatan dan penurunan. Masalah ini dapat dimodelkan dan diselesaikan dengan menggunakan teknik kontrol optimal, sehingga akan diperoleh nilai optimal tingkat inventori dan rata-rata produksi optimal.There are many problems involving the theory of systems, control theory and its application. For example, some reference theories apply control theory to the inventory problems. The classical problem in the inventory problem was how to manage changes in consumer demand in a finished product. Besides it declines caused by damage and deterioration, evidently inventory can also increase. Typically, inventories that increased were inventories have production process continues over time; While little demand also occurred in inventories of living beings who have breeding. evidently, this led to an increasing in the amount of inventory. It can be concluded that, in theory, inventory system can be increased and decreased. This problem can be modeled and solved using optimal control techniques, so it will be obtained an optimum value of inventory levels and the average optimal production.

  19. PEMBINAAN DAN PENGEMBANGAN USAHA KECIL

    Directory of Open Access Journals (Sweden)

    Sentot Harman Glendoh

    2001-01-01

    Full Text Available Small business as an economic activity of society on a small scale, has a central role in the economy of Indonesia. Although the economic crisis has created a great disturbance in the live of large and middle-size business, apparently small business continues to function well in the lower levels of the economy. The main role of small business is: 1 use excess labor; 2 as a producer of goods and services at reachable prices for the lower economic levels of society; 3 as a potential producer of foreign exchange because of the success of this type of industry in producing non-oil commodities for export. Remembering that the role of small business is large and has great influence on the lower economic levels of society, it is quite necessary to pay attention to the development of this sector. Abstract in Bahasa Indonesia : Usaha kecil sebagai kegiatan ekonomi rakyat berskala kecil memiliki peran sentral dalam perekonomian Indonesia. Walaupun krisis ekonomi telah memporakporandakan kehidupan bidang usaha besar dan menengah, ternyata usaha kecil tetap tegar dan berjalan marak dikawasan kehidupan ekonomi tingkat bawah. Peran pokok usaha kecil ini adalah: (1 sebagai penyerap tenaga kerja, (2 sebagai penghasil barang dan jasa pada tingkat harga yang terjangkau bagi kebutuhan rakyat banyak yang berpenghasilan rendah, (3 sebagai penghasil devisa negara yang potensial kerena keberhasilannya dalam meproduksi komoditi ekspor non migas. Mengingat peran usaha kecil tersebut sangat besar andilnya bagi negara dan masyarakat kecil dilapisan bawah, maka pembinaan dan pengembangannya sangat perlu diperhatikan. Kata kunci: pembinaan, pengembangan, usaha kecil.

  20. THE INFLUENCE OF INTERACTIVE MULTIMEDIA AUDIO TELLING MACHINE (IMATE USE AND STUDENTS’ SELF REGU-LATED LEARNING LEVEL ON ENGLISH LANGUAGE GREET-INGS APPLICATION SKILLS (PENGARUH PENGGUNAAN INTERACTIVE MULTIMEDIA AU-DIO TELLING MACHINE (iMATE DAN TINGKAT SELF REGU-LATED LEARNING SISWA TERHADAP KEMAMPUAN MENERAP-KAN GREETINGS BAHASA INGGRIS

    Directory of Open Access Journals (Sweden)

    Muhammad Ridwan Sutisna

    2018-02-01

    Full Text Available Abstract. New trends of technology and also the higher needs of English proficiency have encouraged the quality improvent of English instructions. The aim of this research is to deter-mine the effect of Interactive Multimedia Audio Telling Machine (iMATE and self regulated learning level in English language greetings application skill of vocational school students. iMATE is an Interactive instructional media used in this research. While student’s self regulated learning is divided into high and low level. This research used experimental design. This re-search was held at SMK Pasundan 3 Bandung. Findings of this research were; (1 Generally students achieved better result when using iMATE. (2 There was an interaction between use of instructional media and students’ self regulated learning level. (3 Students with high self regu-lated learning achieved much better when using iMATE. (4 Students with low self regulated learning had a better result when not using iMATE. This Findings lead to the conclusion that students’ self regulated learning level may affect the succes of instructional media use, especially in teaching English language skills. Abstrak. Perkembangan teknologi dan kebutuhan akan kemampuan Bahasa Inggris yang lebih tinggi mendorong kualitas pembelajaran Bahasa Inggris juga mengalami perkem-bangan. Tujuan penelitian ini adalah untuk mengetahui pengaruh dari penggunaan Interactive Multimedia Audio Telling Machine (iMATE dan tingkat self regulated learning terhadap ke-mampuan menerapkan greetings Bahasa Inggris siswa SMK. iMATE adalah multimedia inter-aktif pembelajaran yang digunakan dalam penelitian ini. Siswa sebagai subjek penelitian dibagi kedalam dua kelompok yaitu yang memiliki tingkat self regulated learning yang tinggi dan ren-dah. Penelitian yang dilaksanakan di SMK Pasundan 3 Bandung ini menggunakan desain ek-sperimen. Temuan dari penelitian ini adalah (1 Secara umum siswa memperoleh hasil yang lebih baik dengan

  1. AGROFORESTRI UNTUK ADAPTASI DAN MITIGASI PERUBAHAN IKLIM

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    Tigor Butarbutar

    2017-01-01

    Full Text Available Hilangnya tutupan lahan hutan karena konversi hutan untuk pemukiman, perkebunan, pertanian dan kebutuhan untuk pembangunan di sektor lain, telah menyebabkan perubahan pola cuaca/iklim di berbagai tempat. Perubahan iklim dapat diantisipasi dengan mitigasi dan adaptasi. Mitigasi berarti usahausaha pencegahan yang perlu dilakukan, sedangkan adaptasi merupakan kegiatan-kegiatan penyesuaian yang perlu dilakukan untuk dapat hidup dan bertahan dan meningkatkan ketahanan, kelenturan dan mengarahkemigrasikarenakondisiiklimyangberbeda.Agroforestridapatmemitigasidanmengadaptasi perubahaniklim dengan alasan-alasansebagaiberikut: aPencampuranjenis pohonpenghasilkayu,buah dan lain-lain, karena campuran jenis lebih baik dari tanaman murni; b Pencampuran jenis yang didasarkan pada sifat toleransi ( dan , sehingga akan memanfaatkan seluruh cahaya untuk fotosintesis; c Pencampuran perbedaan umur; d Pencampuran berdasarkan perbedaan waktu pemanenan; e Penggabungan nilai ekonomi, sosial dan budaya sehingga perubahan vegetasi dapat berjalan seiring dengan perubahan sosial dan budaya secara berangsur yang dapat disesuaikan dengan perubahan iklim; dan f Dapat digunakan sebagai model untuk memfasilitasi perubahan kelompok vegetasi menjadi kelompok yang baru (adaptasi, seperti teori perubahan vegetasi melalui perladangan berpindah-pindahyangteratur.

  2. Fenton's reagent as a remediation process in water treatment: application to the degradation of polycyclic aromatic hydrocarbons in waters and sewage sludges; La reaction de fenton comme procede de rehabilitation dans le traitement des eaux: application a la degradation des hydrocarbures aromatiques polycycliques dans les eaux et les boues residuaires

    Energy Technology Data Exchange (ETDEWEB)

    Flotron, V

    2004-05-15

    This study is related to the application of Fenton's reagent to remedy matrices contaminated by polycyclic aromatic hydrocarbons (PAHs). In aqueous solution, the choice of the reagent implementation is important, in order to generate enough radicals to oxidize pollutants. Degradation of the organic compounds is possible, but a large difference in reactivity is observed between 'alternant' and 'non-alternant' PAHs (with a five carbon atoms cycle). Besides, if a few specific precautions are omitted, the PAHs can sorb onto the flask inside surface, and therefore not undergo oxidation. The results on sewage sludges show that under certain conditions (high reagent concentrations), the pollutants can be oxidised although they are adsorbed. Moreover, it appears that the matrix itself plays an important role, as the iron oxides seem to be able to decompose hydrogen peroxide, and thus initiate Fenton reaction. Its application to contaminated soils and sediments is also possible. (author)

  3. Fenton's reagent as a remediation process in water treatment: application to the degradation of polycyclic aromatic hydrocarbons in waters and sewage sludges; La reaction de fenton comme procede de rehabilitation dans le traitement des eaux: application a la degradation des hydrocarbures aromatiques polycycliques dans les eaux et les boues residuaires

    Energy Technology Data Exchange (ETDEWEB)

    Flotron, V.

    2004-05-15

    This study is related to the application of Fenton's reagent to remedy matrices contaminated by polycyclic aromatic hydrocarbons (PAHs). In aqueous solution, the choice of the reagent implementation is important, in order to generate enough radicals to oxidize pollutants. Degradation of the organic compounds is possible, but a large difference in reactivity is observed between 'alternant' and 'non-alternant' PAHs (with a five carbon atoms cycle). Besides, if a few specific precautions are omitted, the PAHs can sorb onto the flask inside surface, and therefore not undergo oxidation. The results on sewage sludges show that under certain conditions (high reagent concentrations), the pollutants can be oxidised although they are adsorbed. Moreover, it appears that the matrix itself plays an important role, as the iron oxides seem to be able to decompose hydrogen peroxide, and thus initiate Fenton reaction. Its application to contaminated soils and sediments is also possible. (author)

  4. INDUSTRIALISASI DAN TANTANGANNYA PADA SEKTOR PENDIDIKAN

    Directory of Open Access Journals (Sweden)

    Arif Unwanullah

    2015-10-01

    Full Text Available Abstrak: Industrialisasi dan Tantangannya pada Sektor Pendidikan. Sumbangan pendidikan dalam perubahan dan pembangunan masa lalu telah bergeser dengan kemajuan teknoekonomi dan komunikasi. Perubahan yang terjadi telah menggeser tatanan kehidupan dan pandangan masyarakat. Materialisme, kapitalisme, efisiensi, dan efektivitas telah menjadi tujuan dan semangat hidup. Pergeseran pandangan masyarakat telah mengubah pula pandangan keberhasilan dan mutu pendidikan, di mana pendidikan diukur dari keberhasilan dalam keterserapan lulusan dalam dunia kerja, oleh karenanya pendidikan dianalisis dari karakteristik sebagai investasi (capital-investment. Pergeseran makna dan tanggung jawab pendidikan mendorong dunia pendidikan melakukan pembaruan dengan alternatif: membangun pembaruan penalaran warganya menuju pemerdekaan dan pendewasaan, pendidikan dilaksanakan secara komprehensif dan bekerjasama dengan semua pihak secara kemitraan, dan membangun visi pendidikan secara komprehensif dan simultan dengan semua pihak. Kata kunci: perubahan sosial, materialistik, modernisasi dan kapitalis Abstract: Industrialization and its education Sector challenges. Contribution of education has shifted with the progress of technology, economy, and communication. The changes have shifted the society's views. Materialism, capitalism, efficiency, and effectiveness have become of interest and enthusiasm for life. The shift has changed society's view, i.e. the view of success and quality of education, in which education is measured from a rate of the absorption of graduates into labor market, therefore education is analyzed from the characteristics of an investment (capital-investment. A shift in meaning and responsibility of education encourages the education sector to create reformation through these following alternatives: creating new thoughts towards liberation and maturation, implementing education comprehensively and cooperating with all parties in partnership, and creating

  5. Desain dan Uji Kinerja Fungsional Sistem Penggerak dan Kendali ROVERGARD

    Directory of Open Access Journals (Sweden)

    Moh Fikri Pomalingo

    2017-04-01

    Full Text Available Abstract The high population rate has an impact on increasing of land function change from agricultural land become housing and commercial building. As a result, it is difficult to get land for planting in the urban area. Therefore, this research is aimed to design equipment that can be used for planting in the narrow land using vertical gardening. This paper will report about design and functional testing of drive and control system on ROVERGARD. Drive system is based on water pump with additional gear train and chainsprocket mechanism. Control system use was on open loop type based on timer. The performance test of drive system was focused on electrical energy consumption and rotational speed of the system that was measured by multifunctional mini ammeter and tachometer. The control system was tested during 4 days, to evaluate their performances between set point and actual timing while filling water tank and rotate the system at maximal load condition. Electrical power consumption was 208 W at average rotational speed 2703 rpm. Increasing load caused an increase of energy consumption but made the drive rotation decline. The position control performance had on position error around 50 cm. Consequently, setting time on timer must be adjusted. Abstrak Laju pertumbuhan penduduk yang tinggi, mengakibatkan tingginya alih fungsi lahan pertanian menjadi bangunan perumahan dan komersial. Masalah ini mengakibatkan sulitnya mencari lahan pertanian di daerah padat penduduk khususnya perkotaan. Oleh karena itu perlu dirancang sebuah alat yang dapat digunakan untuk bercocok tanam di lahan sempit. Tujuan dari penelitian ini adalah mendesain dan menguji sistem penggerak dan kendali pada ROVERGARD. Sistem penggerak berasal dari pompa air yang dimodifikasi. Sedangkan sistem kendali menggunakan tipe open loop berbasis waktu dimana timer sebagai komponen utamanya. Pengujian kinerja penggerak difokuskan pada konsumsi listrik dan rpm yang diukur menggunakan

  6. APPLICATION OF THE HACCP METHOD IN THE SWINE ABATTOIR BY SCALDING-SKINNING ECOLOGICAL PROCESSING / APPLICATION DE LA METHODE HACCP DANS L’ABATTOIR PORCIN PAR LE PROCESSUS ECOLOGIQUE D’ÉCHAUDAGE-DÉPEÇAGE

    Directory of Open Access Journals (Sweden)

    IULIAN SUCEVEANU

    2017-03-01

    Full Text Available In the food industry development, the food safety and the valorization of by-products represent important aspects. The present study consists in the application of the Hazard Analysis and Critical Control Point (HACCP method in pig slaughterhouses for scalding-skinning technology in order to ensure the conformity of meat quality and the by-products management and recycling. In order to optimize the scalding-skinning process of swine, all the classical technological steps of the technological processes were analyzed separately and globally, with the adaptation of the HACCP method for the new technology. The result of this study shows that the implementation of the new technology that combines existing technologies has many advantages from both an economic and a technological point of view. At the same time the new technology ensures food safety by taking account of the application of the food safety system, respectively, HACCP method.

  7. RESIKO PENULARAN INFEKSI DI RUANG AUTOPSI DAN PENERAPAN KEWASPADAAN UNIVERSAL

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    Citra Manela

    2015-12-01

    Full Text Available AbstrakPeningkatan resiko penularan infeksi di ruang autopsi semakin meningkat. Hal ini terjadi karena peningkatan jumlah kasus korban meninggal yang terinfeksi penyakit terutama di negara berkembang. Beberapa studi menyatakan terjadinya peningkatan prevalensi HIV, hepatitis B, C, D dan G, tuberkulosis, penyakit Prion, Hantavirus, campak, infeksi bakteri atau HTCV pada pekerja di ruang autopsi. Penerapan kewaspadaan universal, termasuk standar OSHA, pemilihan disinfektan dan pengolahan limbah medis sangat penting diperhatikan untuk mencegah resiko terjadinya penularan infeksi. Tujuan penulisan tinjauan pustaka ini adalah mengetahui risiko penularan infeksi pada pekerja di ruang autopsi dan penerapan kewaspadaan universal. Penulisan ini berdasarkan studi kepustakaan yang terkait dengan dua topik ini. Penerapan kewaspadaan universal sangat diperlukan dalam pencegahan penularan penyakit infeksi pada pekerja di ruang autopsi yaitu meliputi penggunaan alat pelindung diri yang tepat, perilaku, tindakan mencegah infeksi, disinfeksi dan penanganan sampah medis yang sesuai aturan.AbstractThe risk of infection transmissions in autopsy room is increasing. This happens because the increase of the number of cases died affected by infectious disease, especially in developing countries. Several studies found an increase on the prevalence of HIV , Hepatitis B , C , D and G, Tuberculosis , Prion Disease , Hantavirus , Measles , Bacterial Infection or HTCV on workers in autopsy room .The application of universal precaution , including OSHA standards , the selection of disinfectant, medical waste management is very important to prevent the risk of the infection transmission. The aim of this review was to explain the risks of infection transmissions on workers in autopsy room and the application of universal precaution. Literatures on these two topics were evaluated. Application of universal precautions are very necessary in the prevention of transmission of

  8. APPLICATION OF THE HACCP METHOD IN THE SWINE ABATTOIR BY SCALDING-SKINNING ECOLOGICAL PROCESSING / APPLICATION DE LA METHODE HACCP DANS L’ABATTOIR PORCIN PAR LE PROCESSUS ECOLOGIQUE D’ÉCHAUDAGE-DÉPEÇAGE

    OpenAIRE

    IULIAN SUCEVEANU; IRINA-CLAUDIA ALEXA; LUMINITA GROSU; OANA-IRINA PATRICIU; IRINA IFRIM; MIRELA SUCEVEANU

    2017-01-01

    In the food industry development, the food safety and the valorization of by-products represent important aspects. The present study consists in the application of the Hazard Analysis and Critical Control Point (HACCP) method in pig slaughterhouses for scalding-skinning technology in order to ensure the conformity of meat quality and the by-products management and recycling. In order to optimize the scalding-skinning process of swine, all the classical technological steps of the technological...

  9. KONTEKS DAN KONSTRUKSI SOSIAL MENGENAI KEMATIAN ELEKTIF ( EUTHANASIA ∗

    Directory of Open Access Journals (Sweden)

    Helly Prajitno Soetjipto

    2015-09-01

    konteks sosial dan konstruksi sosial kematian. Euthanasia didiskusikan di dalam suatu kerangka pikir yang mencoba memberi perhatian kepada hal-hal yang kontekstual dan interpretatif fenomena sosial suatu proses kematian dan kejadian kematian

  10. DIAGNOSIS DAN PENATALAKSANAAru LIMFOMA ORtsITA

    Directory of Open Access Journals (Sweden)

    Ardizal Rahman

    2014-12-01

    Full Text Available Limfoma orbita merujuk pada limfoma yang terjadi di konjungtiva, kelenjar lakrimal, palpebradan otot-otot ekstraokular. Limfoma primer non-Hodgkin (NHL dari orbita dapat ditemukanpada hanya 1o/o dari semua limforna non-Hodgkin. Anaiisis mutasi somatik pada regiovariabel (V dari immunoglobulin (ig dan segmen gen rantai berat (H telah menunjukkanperan dari stimulasi antigen kronik pada patogenesis limfoma /nucosa-associated lymphoidflssue (MALT. Patogen mikroba seperti Helicobacter pylaridan Chlamydia pneumonia dapaimendasari proses inflamasi dan pada akhirnya memicu akuisisi MALT juga memainkanperan penting dalam tranformasi maligna dan ekspansi klonal lanjutan limfoma. Penentuanstadium kanker sangat penting karena akan menentukan terapi apa yang akan diberikan dankemungkinan remisi dan prognosisnya. Berdasarkan sistem stadium Ann-Arbor, limfoma yangterbatas di orbita disebut sebagai stadium l, keterlibatan struktur sekitar (sinus paranasal,tonsil, dan hidung menjadikannya stadium ll. Stadium lll adalah penyakit nodal abdominaldibawah diafragma dan stadium lV merujuk pada keterlibatan yang tersebar dari satu ataulebih lokasi ekstranodal (hepar, sum-sum tulang atau sistem saraf pusat. Mayoritas pasiendatang dengan keluhan massa konjungtiva berwarna pink (91%, diikuti hiperemis konjungtiva(32%, propiosis (27%, massa palpebra atau orbita (19"fi, penurunan visus dan ptosis (6%,dan diplopia(2%. Bilateralitas terjadi pada 10% hingga 15% kasus dimana 80 % terjadisecarasimultan sedangkan 20% merupakan kondisi yang berurutan. Penilaian lanjut untuk stagingyang akurat dan perencanaan terapitermasuk anamnesis yang lengkap dan pemeriksaan fisik,pemeriksaan laboratorium rutin, elektroforesis protein sei-um, LDH serum, Fr-mikroglobulin,rontgen thoraks, CT scan thoraks, abdornen, dan pelvis, dan biopsisum-sum tulang. Diagnosapositif harus berdasarkan pada perneriksaan histologik dari sampeltumor yang memadai yangdiperoleh dengan biopsiorbita. Beberapa kriteria

  11. TRANSFORMASI ORGANISASIONAL DAN MSDM: HAMBATAN DAN IMPLIKASINYA PADA REKRUTMEN DAN SELEKSI

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    Licen Indahwati Darsono

    2002-01-01

    Full Text Available Rapid change of environment is an external force that causes the organization to transform. Fundamentally, the main purpose of the transformation is to change the organizational structure to be more flexible and competitive with fewer hierarchial levels, managers, and employees. The transformation needs to be radical, causing resistance from the organization's members. Their resistance can cause the transformation to fail, therefore organization must find ways to lessen this resistance. First, organization must learn about the diversity of its members' cultures and values. Second, organization must build its own organizational culture which can support the success of the transformation, by communicating it with the members of the organization. To support organizational culture building efforts, it needs changes in human resources practices, especially recruitment and selection. Abstract in Bahasa Indonesia : Perubahan yang cepat dalam lingkungan merupakan kekuatan eksternal yang mengakibatkan transformasi dalam sebuah organisasi. Pada dasarnya, tujuan utama dari transformasi tersebut adalah merubah struktur organisasi agar menjadi lebih fleksibel dan mampu bersaing, dengan tingkat structural yang sedikit, serta jumlah manajer dan karyawan yang lebih kecil. Transformasi tersebut harus menyeluruh, dan hal ini dapat menyebabkan resistensi dari para anggota organisasi yang memperhambat perubahan tersebut. Resistensi itu bisa menyebabkan perubahan tersebut batal, oleh karena itu organisasi harus mencari jalan untuk mengurangi hambatan-hambatan tersebut. Pertama, organisasi harus belajar keanekaragaman dari budaya dan nilai anggotanya. Kedua, organisasi harus mengembangkan budaya organisasi sendiri melalui komunikasi yang baik dengan anggotanya. Untuk mendukung usaha mengembangkan budaya organisasi, harus ada perubaban pada kebijakan sumber daya manusia, terutama dalam rekrutmen dan seleksi karyawan. Kata kunci: transformasi, resistensi, budaya

  12. Perbandingan Akurasi Pengukuran Suhu Dan Kelembaban Antara Sensor DHT11 Dan DHT22

    OpenAIRE

    Saptadi, Arief Hendra

    2014-01-01

    Suhu dan kelembaban merupakan dua objek pengukuran yang acapkali terdapat di dalam sistem akuisisi data. Terdapat banyak piranti sensor yang berfungsi untuk mengukur dua objek tersebut dan akurasi merupakan salah satu parameter yang dapat digunakan untuk memilihnya. DHT11 dan DHT22 adalah sensor seri DHT dari Aosong Electronics yang dapat melakukan pengukuran suhu dan kelembaban secara serempak dengan keluaran digital. Informasi tentang akurasi terdapat di dalam lembar data keduanya. Kendati ...

  13. Pertumbuhan dan Mutu Fisik Bibit Jabon (Anthocephalus Cadamba Miq.) di Polibag dan Politub

    OpenAIRE

    Junaedi, Ahmad

    2010-01-01

    Informasi pertumbuhan dan mutu fisik bibit jabon (Anthocephalus cadamba Miq.) di wadah bibit dengan volume yang berbeda diperlukan sebagai bagian yang akan diperhitungkan dalam pemilihan wadah bibit yang akan digunakan. Penelitian ini dilakukan untuk mengetahui pertumbuhan dan mutu fisik bibit jabon yang disapih pada wadah bibit polibag (volume 300 cm3) dan politub (volume 60 cm3). Tahapan penelitian meliputi : pembibitan serta pengamatan pertumbuhan dan penilaian mutu fisik bibit jabon yang ...

  14. Dampak belanja irigasi dan jaringan terhadap output PDRB sektor pertanian dan pertumbuhan ekonomi Kota Jambi

    OpenAIRE

    Aminah, Siti; Parmadi, Parmadi

    2018-01-01

    Penelitian ini bertujuan untuk menganalisis perkembangan Belanja irigasi dan jaringan serta perkembangan output GDP sektor pertanian Kota Jambi selama periode tahun 2005-2015 dan menganalisis pengaruh belanja irigasi dan jaringan terhadap  GDP Output sektor pertanian dan pertumbuhan ekonomi Kota Jambi. Hasil penelitian menunjukkan Selama periode penelitian tahun 2005-2015 dengan rata-rata pertumbuhan 61,98%, nilai rata-rata PDRB harga berlaku Kota Jambi sebesar 157.601,68 dalam juta rupi...

  15. Wacana Penjarahan Dan Kekerasan Simbolik Terhadap Petani

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    Agus Sudibyo

    2002-01-01

    Full Text Available Perlawanan kaum petani sudah lama terjadi dalam konteks sejarah hubungan antara si kaya dan si miskin dan antara kaum petani dan negara. Persoralannya selalu bahwa negara, aparat keamanan dan pemilik modal telah mengambil alih secara paksa surplus ekonomi dari petani. Mereka bekerja sama dalam aksi penyerobotan tanah petani, pendirian perkebunan-perkebunan dan dalam menghadapi gerakan protes petani. Negara bukan hanya menghadapi gerakan perlawanan petani dengan represi-represi fisik. Secara sistematis negara juga melakukan propaganda dengan menciptakan gambaran-gambaran yang unfavourable tentang petani pelaku penjarahan dalam berbagai representasi wacana. Dalam batas tertentu, media massa justru memperkuat kecenderungan ini dengan menonjolkan dimensi kekerasan, pemberontakan dan anarkisme dalam mewacanakan aksi-aksi penjarahan petani.

  16. Motivasi, Kebiasaan, dan Keamanan Penggunaan Internet

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    Zinggara Hidayat

    2017-01-01

    Full Text Available Abstract: This study investigates motivation, habits, and security of internet use by high schools and universities students in Jakarta, Bogor, Depok, Tangerang, and Bekasi. This descriptive and quantitative reasearch uses survey method. The findings of the study show that the strongest motivation is to show self existence, entertainment, and academic purposes. At some points, the habit of using the internet also makes the students face some risks such as verbal and nonverbal abuses, bullying, pornoghrapy, account hacking, and the risk of interaction with unknown parties. Abstrak: Penelitian ini menyelidiki motivasi, kebiasaan, dan keamanan penggunaan internet di antara siswa sekolah menengah atas dan universitas di Jakarta, Bogor, Depok, Tangerang, dan Bekasi. Penelitian deskriptif kuantitatif ini menggunakan metode survei. Hasil penelitian menunjukkan bahwa motivasi paling kuat adalah untuk memperlihatkan eksistensi diri, pencarian hiburan, dan penyelesaian tugas akademis. Kebiasaan penggunaan internet oleh pelajar dan mahasiswa menghadapi beberapa risiko, seperti kekerasan verbal dan nonverbal,

  17. SOSIAL MEDIA DAN PERUBAHAN INDEKS PRESTASI MAHASISWA

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    Risnah Risnah

    2015-12-01

    Tujuan dari penelitian ini adalah mengetahui jumlah mahasiswa semester II, IV, dan VI Jurusan Keperawatan yang menggunakan internet secara aktif dan karak-teristiknya, membandingkan hasil belajar mahasiswa semester II-III, IV-V, dan VI-VII Jurusan Keperawatan, dan mengetahui pengaruh sosial media (facebook dan twitter terhadap perubahan indeks prestasi mahasiswa, dengan jumlah res-ponden sebanyak 150 orang. Penelitian ini adalah deskriptif dengan desain pene-litian kausal. Pengumpulan data dengan menggunakan instrumen berupa kuesio-ner, dengan jumlah responden sebanyak 150 orang. Adapun hasil penelitian me-nunjukkan bahwa indeks prestasi mahasiswa dengan penggunaan sosial media umumnya responden menyatakan sosial media tidak mempengaruhi indeks prestasi. Dari hasil analisis uji statistik diperoleh terdapat pengaruh antara sosial media (facebook dan twitter dengan indeks prestasi. Dengan begitu, penggunaan sosial media harus digunakan sebagaimana mestinya, agar mahasiswa/i yang ak-tif pengunaan sosial media tidak mempengaruhi indeks prestasinya.

  18. Colloids: a review of current knowledge with a view to application to phenomena of transportation within PWR; Colloides: point de vue sur les connaissances actuelles en vue d`une application aux phenomenes de transport dans les REP

    Energy Technology Data Exchange (ETDEWEB)

    Guinard, L.

    1996-12-31

    In an attempt to minimise dosimetry within the primary circuit of PWR units, research is being carried out into understanding the phenomena of transportation and deposition of corrosion products. It is therefore desirable to known the form of these corrosion products and the laws governing this form. It is generally considered that they are in soluble or particulate form. A third starts with a general presentation of colloids and goes on to define points which are useful, both on a theoretical and experimental level, in terms of application to phenomena of transportation within PWRs. (author). 69 refs., 30 figs., 6 tabs., 3 appends.

  19. Persepsi Santri dan Kiai terhadap Pluralisme Agama di Pendidikan Ulama Tarjih Muhammadiyah (PUTM dan Aswaja Nusantara Yogyakarta

    Directory of Open Access Journals (Sweden)

    Zainal Arifin

    2017-05-01

    Abstrak: Perdebatan pluralisme agama masih mengemuka dalam konteks masyarakat majemuk di Nusantara. Bahkan, tidak jarang menimbulkan konflik dan perang pemikiran. Menarik melihat perspektif kiai dan santri Muhammadiyah dan NU terhadap isu pluralisme melalui praktik pendidikan di Ulama Tarjih Muhammadiyah (PUTM Yogyakarta dan Pondok Pesantren Aswaja Nusantara Yogyakarta yang dianggap representatif karena membawa muatan konsep, ide dan paradigma dari Muhammadiyah dan NU. Penelitian ini bersifat kualitatif,  data diperoleh dari wawancara dan studi kepustakaan dengan saling memberikan verifikasi, koreksi dan pelengkap. Hasil penelitian ini, PUTM dan Pesantren Aswaja Nusantara memiliki konsep yang sama dalam memegang teguh akidah, yakni sikap eksklusif dan menolak pluralisme secara teologis namun menerimanya secara sosiologis. Sehingga, paradigma dari dua lembaga tersebut merepresentasikan dari paradigma Muhammadiyah dan NU dalam merespon fenomena pluralisme agama dan budaya.

  20. VAKSIN DENGUE DAN PERKEMBANGANNYA SAAT INI DAN DI MASA MENDATANG

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    Triwibowo Ambar Garjito

    2012-09-01

    Full Text Available Dengue virus merupakan salah satu virus anggota dari famili Flaviviridae yang sejak tahun 1956 telah dikenal dapat menimbulkan demam dengue maupun demam berdarah dengue (DBD. Penyakit yang ditularkan oleh nyamuk Aedes aegypti ini diperkirakan telah menjangkiti pada selatar 50-100 juta manusia dengan 500.000 kasus di antaranya dalam manifestasi yang ganas yang dikenal sebagai dengue haemorrhagic fever dan dengue shock syndrome dan 25.000 di antaranya berakibat fatal (meninggal. Saat ini pengembangan vaksin merupakan salah satu solusi yang diharapkan dapat menekan penyebaran penyakit tersebut. E (envelope merupakan salah satu bagian dari protein struktural virus yang sangat penting dalam pengembangan vaksin, yaitu sebagai badan yang memproduksi antibodi netralisasi untuk protein. Non-struktural protein l juga telah diketahui sebagai salah satu komponen penting dalam pengembangan vaksin oleh karena kemampuannya untuk dapat diekspresi pada permukaan sel yang diinfeksi yang dapat menjadi target untuk immune cytolisis. Ada dua pendekatan yang digunakan dalam memproduksi suatu vaksin dengue, yaitu: a. Vaksin hidup yang telah dilemahkan (live attenuated vaccine: b. Vaksin hasil rekayasa (engineered vaccine. Penelitian terhadap vaksin DENV baik rekombinan maupun non-rekombinan yang didasarkan pada uji virus telah dilakukan secara terus-menerus baik pada monyet dan manusia. Sampai saat ini telah dikembangkan sejumlah kandidat vaksin DENV yang berdasar pada tetravalent virus dengue, yaitu a. vaksin konvensional, b. vaksin dengue rekombinan berdasar pada flavivirus, c. vaksin intertypic chimeric, d. vaksin chimerivac, e. vaksin dengue rekombinan menggunakan vector non-ftavivirus dan f. vector adenovirus. Namun demikian, sampai sekarang belum ada vaksin yang siap digunakan untuk menangkal infeksi ke empat serotype virus dengue, sehingga masih diharapkan untuk pengembangan virus lebih lanjut.   Kata kunci: Aedes aegypti, dengue virus, vaksin dengue.