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Sample records for extraction chromatographic resin

  1. Selenium extraction: development on extraction chromatographic resins compatible with Diffusive Gradient in Thin film (DGT)

    Science.gov (United States)

    Rad, S.; Dirks-Fandrei, C.; Happel, S. A.; Bombard, A.; Cary, L.

    2016-12-01

    Measurement of Selenium is of importance regarding public health as the ratio between beneficial daily intake and toxicity is rather low [1], [2]. Also from the radiological perspective, Se-79 as a long-lived fission nuclide (T1/2=2.8x105y) with high mobility in environment, is of concern regarding waste management and decommissioning [3], [4]. Due to the existence of different oxidation states Selenium has a complex speciation chemistry which makes extraction and separation schemes not straightforward. The aim of this research is to develop extraction methods for Selenium based on extraction chromatographic resins allowing for the extraction of Se(VI), as well as Se(IV), from water samples for later use on DGT (Diffusive Gradients in Thin films) devices. Extraction chromatographic resins have been tested and characterized for Se and other elements. For Se(VI) a commercially available Aliquat 336 based extraction chromatographic resin (TEVA resin[5]) was found to be most suitable, for Se(IV) a newly developed extraction chromatographic resin based on Piazselenol chemistry was found to be most effective, data on the selectivity of this resin will be presented. The extraction of Se(IV) and Se(VI) by these resins was tested on water sampled in Lille City, where a high Se spatial variability has been observed. Concentrations in groundwater can reach 30µg/L as a consequence; most Se-contaminated wells are no longer exploited by the water operators. One of the applications of this development is to be able to measure Se concentrations insitu in contaminated areas including very complex object such as hyporheic zone. [1] Cary L. et al. Applied Geochemistry 48 (2014) 70-82 [2] Chen C. et al. Biological Trace Element Research Vols. 71-72 (1999) 131-138 [3] http://www.irsn.fr/FR/Larecherche/publications-documentation/fiches-radionucleides/Documents/environnement/Selenium_Se79_v2.pdf last access 03/03/2016 [4] Uchida et al. WM2009 Conference, March 1-5, 2009, Phoenix, AZ [5

  2. Radiolytic stability of some recently developed ion exchange and extraction chromatographic resins containing diphosphonic acid groups

    Energy Technology Data Exchange (ETDEWEB)

    Chiarizia, R.; Horwitz, E.P.

    2000-01-01

    The effect of {sup 60}Co irradiation on the Diphonix{trademark}, Diphosil and Diphonix-CS chelating ion exchange resins, and on two Dipex{trademark} extraction chromatographic resins containing the P,P{prime}-di(2-ethylhexyl) methanediphosphonic acid (H{sub 2}DEH[MDP]) impregnated in the pores of a polymeric support (Dipex-1) and of silica (Dipex-2), respectively, has been investigated. The resins have been irradiated while in contact with HNO{sub 3} (Diphonix, Diphosil and Dipex resins) or NaOH (Diphonix-DS resin) up to an absorbed dose of about 200 Mrad. As a probe of the resin radiolytic degradation, metal uptake (both equilibrium and kinetics) and capacity measurements have been performed. Results show that the Diphonix-CS resin properties are practically unaffected by irradiation under the experimental conditions used in this work. The Diphonix, Diphosil, and especially the Dipex resins suffer substantial capacity losses, but their affinity for actinide ions is not seriously compromised. On the other hand, the kinetics of metal uptake by the silica based Diphosil and Dipex-2 resins becomes substantially slower indicating that, from a radiolytic degradation standpoint, polymeric materials perform better than silica as supports for H{sub 2}DEH[MDP] containing extraction chromatographic resins.

  3. An improved extraction chromatographic resin for the separation of uranium from acidic nitrate media

    Energy Technology Data Exchange (ETDEWEB)

    Dietz, M.L.; Horwitz, E.P.; Sajdak, L.R.; Chiarizia, R. [Chemistry Division, Argonne National Laboratory, 60439 Argonne, IL (United States)

    2001-07-06

    The preparation and characterization of a new extraction chromatographic resin exhibiting extraordinarily strong retention of hexavalent uranyl ion over a wide range of nitric acid concentrations and very high selectivity for U(VI) over Fe(III) and numerous other cations is described. This new material (designated U/TEVA-2) comprises a novel liquid stationary phase consisting of an equimolar mixture of diamyl amylphosphonate (DA[AP]) and Cyanex 923{sup registered} (a commercially available trialkyl-phosphine oxide, TRPO) sorbed on silanized silica or Amberchrom CG-71. Cyanex 923 is shown to be preferable to a related TRPO, Cyanex 925{sup registered}, due to its lower viscosity and higher selectivity for U(VI) over Fe(III). The retention of uranyl nitrate by the U/TEVA-2 resin, as measured by the k' values (number of free column values to peak maximum) is >5000 from approximately 0.1 to 8 M HNO{sub 3}. The ability of the new resin to strongly and selectively retain U(VI) from such a wide range of acid concentrations, along with its favorable physical properties, make it a good candidate for application in the separation and preconcentration of U(VI) from complex environmental, biological, and nuclear waste samples for subsequent determination.

  4. An improved extraction chromatographic resin for the separation of uranium from acidic nitrate media.

    Science.gov (United States)

    Dietz, M L; Horwitz, E P; Sajdak, L R; Chiarizia, R

    2001-07-01

    The preparation and characterization of a new extraction chromatographic resin exhibiting extraordinarily strong retention of hexavalent uranyl ion over a wide range of nitric acid concentrations and very high selectivity for U(VI) over Fe(III) and numerous other cations is described. This new material (designated U/TEVA-2) comprises a novel liquid stationary phase consisting of an equimolar mixture of diamyl amylphosphonate (DA[AP]) and Cyanex 923((R)) (a commercially available trialkyl-phosphine oxide, TRPO) sorbed on silanized silica or Amberchrom CG-71. Cyanex 923 is shown to be preferable to a related TRPO, Cyanex 925((R)), due to its lower viscosity and higher selectivity for U(VI) over Fe(III). The retention of uranyl nitrate by the U/TEVA-2 resin, as measured by the k' values (number of free column values to peak maximum) is >5000 from approximately 0.1 to 8 M HNO(3). The ability of the new resin to strongly and selectively retain U(VI) from such a wide range of acid concentrations, along with its favorable physical properties, make it a good candidate for application in the separation and preconcentration of U(VI) from complex environmental, biological, and nuclear waste samples for subsequent determination.

  5. Chromatographic zinc isotope separation by phenol formaldehyde benzo crown resin.

    Science.gov (United States)

    Ding, Xingcheng; Nomura, Masao; Suzuki, Tatsuya; Sugiyama, Yuichi; Kaneshiki, Toshitaka; Fujii, Yasuhiko

    2006-04-28

    New types of phenol formaldehyde resin having benzo crown as a functional group were synthesized and applied to zinc isotope chromatographic operation. Zinc adsorption and isotope separation capacities were dramatically improved by using phenol formaldehyde benzo-15-crown-5 resin. Zinc batch adsorption tests were performed by various dehydrated organic solvents. Separation coefficient, epsilon 8.1 x 10(-4) and height equivalent to a theoretical plate (HETP) 0.105 cm for the isotopic pair of 68Zn/64Zn in phenol formaldehyde benzo-15-crown-5 resin were obtained in the case of acetone as the solvent at 298+/-1K.

  6. Transesterification of propylene glycol methyl ether in chromatographic reactors using anion exchange resin as a catalyst.

    Science.gov (United States)

    Oh, Jungmin; Sreedhar, Balamurali; Donaldson, Megan E; Frank, Timothy C; Schultz, Alfred K; Bommarius, Andreas S; Kawajiri, Yoshiaki

    2016-09-30

    Reactive chromatography using an anion exchange resin is proposed for a transesterification reaction of propylene glycol methyl ether (DOWANOL™ PM) with ethyl acetate to produce propylene glycol methyl ether acetate (DOWANOL™ PMA). This reaction is studied in batch and chromatographic reactors catalyzed by an anion exchange resin. Several anion exchange resins are tested and compared based on the performance of resin as an adsorbent and a catalyst. A chromatographic column is packed with a selected catalyst, AMBERLITE™ IRA904, and both reaction and chromatographic elution are studied at different temperatures and feed concentrations. The resulting chromatograms are fitted to a mathematical model to obtain adsorption equilibrium and reaction kinetic parameters by the inverse method. Compared to esterification investigated in a previous study, transesterification has advantages such as a higher conversion at lower temperature and easy removal of the byproduct which may lead to higher productivity. Deactivation of anion exchange resins is observed and potential solutions are suggested.

  7. Extractables Screening of Polypropylene Resins used in Pharmaceutical Packaging for Safety Hazards.

    Science.gov (United States)

    Jenke, Dennis

    2017-05-15

    Pharmaceutical products are packaged in containers so that they can be manufactured, distributed and used. Because extractables from such containers are precursors of leachable impurities in the product, extractables represent potential hazards to user safety. Polypropylene resins are frequently used as materials of construction for packaging of liquid parenteral drug products. Thus extractables profiling of polypropylene resins may be an effective means of hazard identification associated with the resin's safe use. Twenty-one PP resins were extracted using aqueous and organic extraction solvents and the resulting extracts were screened for extractables using appropriate general chemistry, chromatographic and spectroscopic methodologies. The resulting extractables profiles were toxicologically reviewed by a defined process to identify potential hazards given a specified therapeutic application involving chronic use of a large volume aqueous parenteral drug product (LVP). The organic extractables profiles of individual PP resins were variable in terms of the individual extractable identified and their extracted levels, consistent with high variability in PP resin formulations and PP manufacturing. However, the profiles were similar in terms of the groups of extractable measured. Thus, for example, all the resins had extractables associated with antioxidants as all the resins contained antioxidants but the specific extractables for a given resin depended on the specific antioxidants present in that resin. Few of the targeted extractable elements were present in the extracts at measurable levels although most resins had measurable levels of extracted aluminum, silicon and alkali and alkaline earths. A worst case extractables profile (all the extractables measured in individual resins at their highest levels) was toxicologically reviewed considering an aqueous large volume parenteral (LVP) drug product. This review established certain extractables as potential hazards

  8. Extraction chromatographic separations of tantalum and tungsten from hafnium and complex matrix constituents

    Energy Technology Data Exchange (ETDEWEB)

    Snow, Mathew S.; Finck, Martha R.; Carney, Kevin P.; Morrison, Samuel S.

    2017-02-01

    Ta, Hf, and W analyses from complex matrices (including environmental samples) require high purification of these analytes from each other and major/trace matrix constituents, however, current state-of-the-art Ta/Hf/W separations rely on traditional anion exchange approaches that suffer from relatively similar distribution coefficient (Kd) values for these analytes. This work reports assessment of three commercially available extraction chromatographic resins (TEVA, TRU, and UTEVA) for Ta/Hf/W separations. Batch contact studies show differences in Ta/W,Hf Kd values of up to 106, representing an improvement of a factor of 100 and 300 in Ta/Hf and Ta/W Kd values (respectively) over AG1x4 resin. Variations in the Kd values as a function of HCl concentration for TRU resin show that this resin is well suited for Ta/Hf/W separations, with Ta/Hf, Ta/W, and W/Hf Kd value improvements of 10, 200, and 30 (respectively) over AG1x4 resin. Finally, analyses of digested soil samples (NIST 2710a) using TRU resin and tandem TEVA-TRU columns demonstrate the ability to achieve extremely high purification (>99%) of Ta and W from each other and Hf, as well as enabling very high purification of Ta and W from the major and trace elemental constituents present in soils, using a single chromatographic step.

  9. Extraction chromatographic separations of tantalum and tungsten from hafnium and complex matrix constituents.

    Science.gov (United States)

    Snow, Mathew S; Finck, Martha R; Carney, Kevin P; Morrison, Samuel S

    2017-02-10

    Tantalum (Ta), hafnium (Hf), and tungsten (W) analyses from complex matrices require high purification of these analytes from each other and major/trace matrix constituents, however, current state-of-the-art Ta/Hf/W separations rely on traditional anion exchange approaches that show relatively similar distribution coefficient (Kd) values for each element. This work reports an assessment of three commercially available extraction chromatographic resins (TEVA, TRU, and UTEVA) for Ta/Hf/W separations. Batch contact studies show differences in Ta/Hf and Ta/W Kd values of up to 10(6) and 10(4) (respectively), representing an improvement of a factor of 100 and 300 in Ta/Hf and Ta/W Kd values (respectively) over AG1×4 resin. Variations in the Kd values as a function of HCl concentration for TRU resin show that this resin is well suited for Ta/Hf/W separations, with Ta/Hf, Ta/W, and W/Hf Kd value improvements of 10, 200, and 30 (respectively) over AG1×4 resin. Analyses of digested soil samples (NIST 2710a) using TRU resin and tandem TEVA-TRU columns demonstrate the ability to achieve extremely high purification (>99%) of Ta and W from each other and Hf, as well as enabling very high purification of Ta and W from the major and trace elemental constituents present in soils using a single chromatographic step.

  10. Enrichment and separation of chlorogenic acid from the extract of Eupatorium adenophorum Spreng by macroporous resin.

    Science.gov (United States)

    Liu, Boyan; Dong, Beitao; Yuan, Xiaofan; Kuang, Qirong; Zhao, Qingsheng; Yang, Mei; Liu, Jie; Zhao, Bing

    2016-01-01

    A simple and efficient chromatographic method for separation of chlorogenic acid from Eupatorium adenophorum Spreng extract was developed. The adsorption properties of nine macroporous resins were evaluated. NKA-II resin showed much better adsorption/desorption properties. The adsorption of chlorogenic acid on NKA-II resin at 25°C was well fitted to Langmuir isotherm model and pseudo-second-order kinetic model. The dynamic adsorption and desorption experiments were carried out on columns packed with NKA-II resin to optimize the separation process. The content of chlorogenic acid in the product increased to 22.17%, with a recovery yield of 82.41%.

  11. Chromatographic analysis of water and wine samples for phenolic compounds released from food-contact epoxy resins.

    Science.gov (United States)

    Lambert, C; Larroque, M

    1997-02-01

    Food-contact epoxy resins can release phenolic compounds such as phenol, m-cresol, bisphenol F, bisphenol A, 4-tert-butylphenol, bisphenol F diglycidyl ether (BFDGE), and bisphenol A diglycidyl ether (BADGE) into foodstuffs. A validated high-performance liquid chromatographic method with fluorometric detection is described for the simultaneous analysis of these compounds in wine and mineral water. Sample preparation by solid-liquid extraction enables detection limits of 2.5 micrograms/L in wine and 0.25 microgram/L in mineral water to be achieved. Recovery rates are close to 100%, except for BFDGE and BADGE (around 60% in wine and 75% in mineral water).

  12. Ion chromatographic separation of inorganic ions using a combination of hydrophilic interaction chromatographic column and cation-exchange resin column.

    Science.gov (United States)

    Arai, Kaori; Mori, Masanobu; Hironaga, Takahiro; Itabashi, Hideyuki; Tanaka, Kazuhiko

    2012-04-01

    A combination of hydrophilic interaction chromatographic (HILIC) column and a weakly acidic cation-exchange resin (WCX) column was used for simultaneous separation of inorganic anions and cations by ion chromatography (IC). Firstly, the capability of HILIC column for the separation of analyte ions was evaluated under acidic eluent conditions. The columns used were SeQuant ZIC-HILIC (ZIC-HILIC) with a sulfobetaine-zwitterion stationary phase (ZIC-HILIC) and Acclaim HILIC-10 with a diol stationary phase (HILIC-10). When using tartaric acid as the eluent, the HILIC columns indicated strong retentions for anions, based on ion-pair interaction. Especially, HILIC-10 could strongly retain anions compared with ZIC-HILIC. The selectivity for analyte anions of HILIC-10 with 5 mmol/L tartaric acid eluent was in the order of I(-) > NO3(-) > Br(-) > Cl(-) > H2PO4(-). However, since HILIC-10 could not separate analyte cations, a WCX column (TSKgel Super IC-A/C) was connected after the HILIC column in series. The combination column system of HILIC and WCX columns could successfully separate ten ions (Na+, NH4+, K+, Mg2+, Ca2+, H2PO4(-), Cl(-), Br(-), NO3(-) and I(-)) with elution of 4 mmol/L tartaric acid plus 8 mmol/L 18-crown-6. The relative standard deviations (RSDs) of analyte ions by the system were in the ranges of 0.02% - 0.05% in retention times and 0.18% - 5.3% in peak areas through three-time successive injections. The limits of detection at signal-to-noise ratio of 3 were 0.24 - 0.30 micromol/L for the cations and 0.31 - 1.2 micromol/L for the anions. This system was applied for the simultaneous determination of the cations and the anions in a vegetable juice sample with satisfactory results.

  13. Ion chromatographic separation of inorganic ions using a combination of hydrophilic interaction chromatographic column and cation-exchange resin column

    Institute of Scientific and Technical Information of China (English)

    Kaori ARAI; Masanobu MORI; Takahiro HIRONAGA; Hideyuki ITABASHI; Kazuhiko TANAKA

    2012-01-01

    A combination of hydrophilic interaction chromatographic ( HILIC ) column and a weakly acidic cation-exchange resin (WCX) column was used for simultaneous separation of inorganic anions and cations by ion chromatography ( IC ).Firstly,the capability of HILIC column for the separation of analyte ions was evaluated under acidic eluent conditions.The columns used were SeQuant ZIC-HILIC (ZIC-HILIC) with a sulfobetainezwitterion stationary phase (ZIC-HILIC) and Acclaim HILIC-10 with a diol stationary phase (HILIC-10).When using tartaric acid as the eluent,the HILIC columns indicated strong retentions for anions,based on ion-pair interaction.Especially,HILIC-10 could strongly retain anions compared with ZIC-HILIC. The selectivity for analyte anions of HILIC-10 with 5 mmol/L tartaric acid eluent was in the order of I- > NO3- > Br- > Cl- >H2PO4-.However,since HILIC-10 could not separate analyte cations,a WCX column (TSKgel Super IC-A/C) was connected after the HILIC column in series.The combination column system of HILIC and WCX columns could successfully separate ten ions (Na+,NH4+,K+,Mg2+,Ca2+,H2PO4-,Cl-,Br-,NO3- and I-) with elution of 4 mmol/L tartaric acid plus 8 mmol/L 18-crown-6.The relative standard deviations (RSDs) of analyte ions by the system were in the ranges of 0.02% - 0.05% in retention times and 0.18% - 5.3% in peak areas through three-time successive injections.The limits of detection at signal-to-noise ratio of 3 were 0.24 - 0.30 μmol/L for the cations and 0.31 - 1.2 μmol/L for the anions.This system was applied for the simultaneous determination of the cations and the anions in a vegetable juice sample with satisfactory results.

  14. Extraction chromatographic separation of Sr, Pu and Am in environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Sidhu, Rajdeep

    2004-04-01

    An accurate determination of radionuclides from various sources in the environment is essential for assessment of the potential hazards and suitable countermeasures both in case of an authorised release, accidents and routine surveillance. Due to the short range of alpha and beta radiation, the accurate determination of pure alpha and beta emitters must always include radiochemical separations to separate the analytes from the matrix and from other interfering stable and radioactive nuclides. Hence, the procedures used for their determination are usually tedious and involve several preconcentration and separation steps. This work deals with the determination of {sup 90}Sr, {sup 241}Am, {sup 238}Pu, {sup 239,240}Pu and {sup 244}Cm, whic some of the most important artificial radionuclides. Due to either absence or low yield of gamma radiation, a secure determination of low concentrations of all these nuclides requires a dedicated chemistry. Selective extraction chromatographic resins (TRU- and Sr-Resin) have been utilised to develop new procedures for the analyses of Pu, Am and Cm isotopes in seawater and both these and {sup 90}Sr in soil, sediment, urine and low-level liquid radioactive effluents. The proposed method for the analyses of Pu and Am in seawater offers a quick and secure mode for the determination of these radionuclides in marine waters. Combined pre-concentration of actinides and strontium (oxalate or phosphate precipitation) followed by dual column separation on TRU- and Sr-Resin significantly reduces the through put time and costs compared to traditional ion exchange and precipitation methods. The greatest gain in productivity and environmental friendliness is achieved in Sr separations using Sr-Resin instead of precipitations involving fuming nitric acid and oxalate, hydroxide, chromate and carbonate precipitations. (author)

  15. Extraction, chromatographic and mass spectrometric methods for lipid analysis.

    Science.gov (United States)

    Pati, Sumitra; Nie, Ben; Arnold, Robert D; Cummings, Brian S

    2016-05-01

    Lipids make up a diverse subset of biomolecules that are responsible for mediating a variety of structural and functional properties as well as modulating cellular functions such as trafficking, regulation of membrane proteins and subcellular compartmentalization. In particular, phospholipids are the main constituents of biological membranes and play major roles in cellular processes like transmembrane signaling and structural dynamics. The chemical and structural variety of lipids makes analysis using a single experimental approach quite challenging. Research in the field relies on the use of multiple techniques to detect and quantify components of cellular lipidomes as well as determine structural features and cellular organization. Understanding these features can allow researchers to elucidate the biochemical mechanisms by which lipid-lipid and/or lipid-protein interactions take place within the conditions of study. Herein, we provide an overview of essential methods for the examination of lipids, including extraction methods, chromatographic techniques and approaches for mass spectrometric analysis.

  16. The kinetics of fossil resin extraction from a flotation concentrate

    Energy Technology Data Exchange (ETDEWEB)

    Li, L.; Yu, Q.; Miller, J.D. [Univ. of Utah, Salt Lake City, UT (United States)

    1995-11-01

    The kinetics of fossil resin extraction from a flotation concentrate by heptane were investigated as a function of process variables using monosize particles. Experimental results provide for a better understanding of the refining process and the basis for subsequent design and construction of a continuous resin refining circuit. Based on the effect of process variables (particle size, stirring speed, and temperature) the resin extraction rate appears to be controlled by surface solvation phenomena. The initial extraction rate was found to be inversely proportional to the initial particle size and a kinetic model is being developed to describe the experimental results.

  17. Extraction behaviour of Am(III) and Eu(III) from nitric acid medium in CMPO-HDEHP impregnated resins

    Energy Technology Data Exchange (ETDEWEB)

    Saipriya, K.; Kumar, T. [Bhabha Atomic Research Centre Facilities (India). Kalpakkam Reproscessing Plants; Kumaresan, R.; Nayak, P.K.; Venkatesan, K.A.; Antony, M.P. [Indira Gandhi Center for Atomic Research, Kalpakkam (India). Fuel Chemistry Div.

    2016-05-01

    Chromatographic resin containing extractants such as octyl(phenyl)-N,N-diisobutylcarbamoylmethylphosphine oxide (CMPO) or bis-(2-ethylhexyl)phosphoric acid (HDEHP) or mixture of extractants (CMPO + HDEHP) in an acrylic polymer matrix was prepared and studied for the extraction of Am(III) and Eu(III) over a range of nitric acid concentration. The effect of various parameters such as concentration of nitric acid in aqueous phase and the concentration of CMPO and HDEHP in the resin phase was studied. The distribution coefficient of Am(III) and Eu(III) in the impregnated resin increased with increased in the concentration of nitric acid for CMPO-impregnated resin, whereas a reverse trend was observed in HDEHP impregnated resin. In case of resin containing both the extractants, synergism was observed at low nitric acid concentration and antagonism at high nitric acid concentration. The mechanism of extraction was probed by slope analysis method at 0.01 and 2 M nitric acid concentrations. Citrate-buffered DTPA was used for the selective separation of Am(III), and a separation factor of 3-4 was obtained at pH 3.

  18. Ultrasonic extraction of resins from an historic textile.

    Science.gov (United States)

    Rezić, I; Krstić, D; Bokić, Lj

    2008-01-01

    Ultrasound assisted extraction was applied on the historical textile as the most appropriate sample preparation step for the identification of the resinous binder. Fragile silk banner from the 19th century was analyzed for the presence of different resins. After the ultrasonic extraction with ethyl acetate in the ultrasonic bath, resinous materials and unknown sample from the banner were separated by thin layer chromatography. The multiple developments in benzene-methanol (95:5) system as mobile phase and silica gel layer as stationary phase were applied, and afterwards the video densitometry determination of the components was performed by means of video camera HV-C20. The shellac resin was determined as an important part of the complex binder.

  19. Long term stability of cannabis resin and cannabis extracts

    DEFF Research Database (Denmark)

    Lindholst, Christian

    2010-01-01

      The aim of the present study was to investigate the stability of cannabinoids in cannabis resin slabs and cannabis extracts upon long-term storage. The levels of tetrahydrocannabinol (THC), cannabinol (CBN), cannabidiol (CBD) and cannabigerol (CBG) on both neutral and acidic form were measured...... stored in extracted form at room temperature the degradation rate of acidic THC increased significantly relative to resin material with concentration halve-lives of 35 and 91 days in daylight and darkness, respectively. Once cannabis material is extracted into organic solvents, care should be taken...

  20. Improved resins and novel materials and methods for solid phase extraction and high performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Freeze, Ronald [Iowa State Univ., Ames, IA (United States)

    1997-10-08

    Solid-phase extraction (SPE) has grown to be one of the most widely used methods for isolation and preconcentration of a vast range of compounds from aqueous solutions. By modifying polymeric SPE resins with chelating functional groups, the selective uptake of metals was accomplished. The resin, along with adsorbed metals, was vaporized in the ICP and detection of the metals was then possible using either mass or emission spectroscopy. Drug analyses in biological fluids have received heightened attention as drug testing is on the increase both in sports and in the work environment. By using a direct-injection technique, biological fluids can be injected directly into the liquid chromatographic system with no pretreatment. A new surfactant, a sulfonated form of Brij-30 (Brij-S) is shown to prevent the uptake of serum proteins on commercial HPLC columns by forming a thin coating on the silica C18 surface. Excellent separations of eight or more drugs with a wide range of retention times were obtained. The separations had sharper peaks and lower retention times than similar separations performed with the surfactant sodium dodecylsulfate (SDS). Quantitative recovery of a number of drugs with limits of detection near 1 ppm with a 5 μl injection volume were obtained. Finally, a method for solid-phase extraction in a syringe is introduced. The system greatly reduced the volume of solvent required to elute adsorbed analytes from the SPE bed while providing a semi-automated setup. SPE in a syringe consists of a very small bed of resin-loaded membrane packed into a GC or HPLC syringe. After extraction, elution was performed with just a few μl of solvent. This small elution volume allowed injection of the eluent directly from the syringe into the chromatographic system, eliminating the handling problems associated with such small volumes.

  1. Cu Purification Using an Extraction Resin for Determination of Isotope Ratios by Multicollector ICP-MS

    Directory of Open Access Journals (Sweden)

    Akio Makishima

    2014-06-01

    Full Text Available A new simple and quick method has been established for separation of Cu from solutions using an extraction chromatographic resin utilizing Aliquat® 336 (commercially available as TEVA™ resin and Cu(I. This method involves the use of a one milliliter column containing 0.33 mL TEVA™ resin on 0.67 mL Amberchrom® CG-71C acrylic resin. Copper was adsorbed on the column by forming Cu(I with 0.15% ascorbic acid in 0.05 mol·L−1 HBr, while other major elements except Zn showed no adsorption. After removal of the major elements (Na, Mg, Al, P, K, Ca, Cr, Mn, Fe, Co and Ni, Cu was recovered using 2 mol·L−1 HNO3. The recovery yield and total blank were 102% ± 2% and 0.25 ng, respectively. To evaluate the separation method, Cu isotope ratios were determined by a standard-sample-standard bracketing method using multicollector inductively coupled plasma-mass spectrometry (ICP-MS, with a repeatability of 0.04‰ and 0.25‰ (SD, for the standard solution and the solutions from low S (<0.1% S silicate standards, respectively.

  2. ADSORPTION OF GOLD ON TBP EXTRACTING RESIN FROM HCl SOLUTION

    Institute of Scientific and Technical Information of China (English)

    GaoHaoqi; CaoZhikai; 等

    1998-01-01

    Adsorption of gold on TBP extracting resin from HCl solution was researched.All the effects of factors,such as solution acidity,TBP content,temperature,etc.,on adsorption equilibrium were discussed and the equilibrium equation was formulated.The breakthough time of adsorption process with fixed bed was studied through experiment.

  3. Long term stability of cannabis resin and cannabis extracts

    DEFF Research Database (Denmark)

    Lindholst, Christian

    2010-01-01

      The aim of the present study was to investigate the stability of cannabinoids in cannabis resin slabs and cannabis extracts upon long-term storage. The levels of tetrahydrocannabinol (THC), cannabinol (CBN), cannabidiol (CBD) and cannabigerol (CBG) on both neutral and acidic form were measured...... at room temperature, 4 °C and - 20 °C for up to 4 years. Acidic THC degrades exponentially via decarboxylation with concentration halve-lives of approximately 330 and 462 days in daylight and darkness, respectively. The degradation of neutral THC seems to occur somewhat slower. When cannabinoids were...... stored in extracted form at room temperature the degradation rate of acidic THC increased significantly relative to resin material with concentration halve-lives of 35 and 91 days in daylight and darkness, respectively. Once cannabis material is extracted into organic solvents, care should be taken...

  4. A review of the extraction and chromatographic determination methods for the analysis of parabens.

    Science.gov (United States)

    Piao, Chunying; Chen, Ligang; Wang, Yu

    2014-10-15

    Parabens are a family of most widely used antimicrobial preservatives in food ingredients, cosmetic consumer products and pharmaceutical preparations. But several recent studies have cautioned that exposure to parabens may have more harmful consequences on animal and human health than what we realized previously, which made the analysis of parabens necessary. In this paper, we reviewed main sample preparation methods and chromatographic analysis methods proposed in formerly published works dealing with the analysis of parabens in different matrices. The sample preparation methods included ultrasonic assisted extraction, supercritical fluid extraction, pressurized liquid extraction, solid phase extraction, solid phase microextraction, liquid phase microextraction, dispersive liquid-liquid microextraction, stir bar sorptive extraction and matrix solid phase dispersion. The chromatographic analysis methods involved liquid chromatography, gas chromatography, and capillary electrophoresis. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. 45Ti extraction using hydroxamate resin

    DEFF Research Database (Denmark)

    Gagnon, K.; Severin, Gregory; Barnhart, T. E.

    2012-01-01

    As an attractive radionuclide for positron emission tomography, this study explores the extraction and reactivity of 45Ti produced via the 45Sc(p,n)45Ti reaction on a GE PETtrace. Using a small hydroxamate column, we have demonstrated an overall recovery of >50% of 45Ti in ~1 mL of 1M oxalic acid...

  6. Solid Phase Extraction: Applications to the Chromatographic Analysis of Vegetable Oils and Fats

    Energy Technology Data Exchange (ETDEWEB)

    Panagiotopoulout, P. M.; Tsimidou, M.

    2002-07-01

    Applications of solid-phase extraction for the isolation of certain lipid classes prior to chromatographic analysis are given. More information was found for sterols and related compounds, polar phenols and contaminants such as polycyclic aromatic hydrocarbons. Detailed analytical protocols are presented and discussed in many cases. (Author) 120 refs.

  7. SYNTHESES OF POLYSTYRENE RESINS CONTAINING POLYETHER OLIGOMERS AND THEIR EXTRACTION FOR GOLD (Ⅲ)

    Institute of Scientific and Technical Information of China (English)

    DONG Shihua; LIU Shi; XU Yuwu

    1994-01-01

    Three polystyrene resins containing polyether oligomers as extractants were synthesized and their extraction properties were studied. Gold (Ⅲ) ion could be extracted rapidly by the resins (T1/2<1min.)with high efficiency and capacity (for LS-B resin that were 99.8% and 95.8mg/gR respectively) from aqueous solution but most of the co-existing metal ions such as Pd (Ⅱ),Cu(Ⅱ), Zn (Ⅱ), Pb (Ⅱ) and Cd (Ⅱ) were remained. The extraction capacity and stripping percentage for gold (Ⅲ) remained unchanged in four extraction-stripping cycles. The resins also showed good column extraction-elution properties.

  8. Preprocessing and exploratory analysis of chromatographic profiles of plant extracts

    NARCIS (Netherlands)

    Hendriks, M.M.W.B.; Cruz-Juarez, L.; Bont, de D.; Hall, R.D.

    2005-01-01

    The characterization of herbal extracts to compare samples from different origin is important for robust production and quality control strategies. This characterization is now mainly performed by analysis of selected marker compounds. Metabolic fingerprinting of full metabolite profiles of plant ex

  9. Cloud point extraction of Δ9-tetrahydrocannabinol from cannabis resin.

    Science.gov (United States)

    Ameur, S; Haddou, B; Derriche, Z; Canselier, J P; Gourdon, C

    2013-04-01

    A cloud point extraction coupled with high performance liquid chromatography (HPLC/UV) method was developed for the determination of Δ(9)-tetrahydrocannabinol (THC) in micellar phase. The nonionic surfactant "Dowfax 20B102" was used to extract and pre-concentrate THC from cannabis resin, prior to its determination with a HPLC-UV system (diode array detector) with isocratic elution. The parameters and variables affecting the extraction were investigated. Under optimum conditions (1 wt.% Dowfax 20B102, 1 wt.% Na2SO4, T = 318 K, t = 30 min), this method yielded a quite satisfactory recovery rate (~81 %). The limit of detection was 0.04 μg mL(-1), and the relative standard deviation was less than 2 %. Compared with conventional solid-liquid extraction, this new method avoids the use of volatile organic solvents, therefore is environmentally safer.

  10. Separation of matrine and oxymatrine from Sophora flavescens extract through cation exchange resin coupled with macroporous absorption resin

    Directory of Open Access Journals (Sweden)

    Chen Haohao

    2016-06-01

    Full Text Available A simple method for separation of matrine and oxymatrine from Sophora flavescens was developed with cation exchange resin coupled with macroporous resin. Based on the adsorption characteristics of matrine and oxymatrine, 001×732 cation exchange resin was used to absorb target alkaloids for removing most of the foreign matter, while BS-65 macroporous resin was chosen to purify these alkaloids. The result showed that the equilibrium adsorption data of matrine and oxymatrine on 001×732 resin and BS-65 resin at 30°C was fitted to Langmuir isotherm and Freundlich isotherm, respectively. The contents of matrine and oxymatrine were increased from 0.73% and 2.2% in the crude extract of the root of Sophora flavescens to 67.2% and 66.8% in the final eluent products with the recoveries of 90.3% and 86.9%, respectively.

  11. On-line coupling of supercritical fluid extraction and chromatographic techniques.

    Science.gov (United States)

    Sánchez-Camargo, Andrea Del Pilar; Parada-Alfonso, Fabián; Ibáñez, Elena; Cifuentes, Alejandro

    2017-01-01

    This review summarizes and discusses recent advances and applications of on-line supercritical fluid extraction coupled to liquid chromatography, gas chromatography, and supercritical fluid chromatographic techniques. Supercritical fluids, due to their exceptional physical properties, provide unique opportunities not only during the extraction step but also in the separation process. Although supercritical fluid extraction is especially suitable for recovery of non-polar organic compounds, this technique can also be successfully applied to the extraction of polar analytes by the aid of modifiers. Supercritical fluid extraction process can be performed following "off-line" or "on-line" approaches and their main features are contrasted herein. Besides, the parameters affecting the supercritical fluid extraction process are explained and a "decision tree" is for the first time presented in this review work as a guide tool for method development. The general principles (instrumental and methodological) of the different on-line couplings of supercritical fluid extraction with chromatographic techniques are described. Advantages and shortcomings of supercritical fluid extraction as hyphenated technique are discussed. Besides, an update of the most recent applications (from 2005 up to now) of the mentioned couplings is also presented in this review.

  12. Aqueous extraction of anions from coal and fly ash followed by ion-chromatographic determination

    Directory of Open Access Journals (Sweden)

    Tasić Aleksandra M.

    2016-01-01

    Full Text Available Three different techniques were applied for the aqueous extraction of anions from coal and fly ash: rotary mixer- and ultrasonic-assisted extraction with different duration time, and microwave-assisted extraction at different temperatures. Validation showed that the ion-chromatographic method was suitable for the analysis of anions in coal and fly ash extracts. The variations in the amounts of anions using different extraction times during rotary-assisted extraction were minimal for all investigated anions. The efficiency of ultrasound-assisted extraction of anions from coal depended on the sonication time and was highest at 30 min. The ultrasound-assisted extraction was less efficient for the extraction of anions from fly ash than rotary-assisted extraction. Increase of temperature in the microwave-assisted extraction had a positive effect on the amounts of all anions extracted from coal and sulphate from fly ash, while the amounts of fluoride and chloride in fly ash extracts decreased. The microwave-assisted extraction of coal at 150°C was compared with standard ASTM methods, and results were in good agreement only for chloride. Changes in the pH value and conductivity during ultrasound-assisted extraction were measured in order to explain changes on the surface of coal particles in contact with water and different processes that occur under environmental conditions. [Projekat Ministarstva nauke Republike Srbije, br. 172030, br. 176006 i br. III43009

  13. Thin-layer Chromatographic (TLC) Separations and Bioassays of Plant Extracts to Identify Antimicrobial Compounds

    OpenAIRE

    Kagan, Isabelle A.; Flythe, Michael D.

    2014-01-01

    A common screen for plant antimicrobial compounds consists of separating plant extracts by paper or thin-layer chromatography (PC or TLC), exposing the chromatograms to microbial suspensions (e.g. fungi or bacteria in broth or agar), allowing time for the microbes to grow in a humid environment, and visualizing zones with no microbial growth. The effectiveness of this screening method, known as bioautography, depends on both the quality of the chromatographic separation and the care taken wit...

  14. Chemotaxonomic investigations on resins of the frankincense species Boswellia papyrifera, Boswellia serrata and Boswellia sacra, respectively, Boswellia carterii : a qualitative and quantitative approach by chromatographic and spectroscopic methodology

    OpenAIRE

    Paul, Michael

    2012-01-01

    Extracts from the resin exudates of the frankincense tree again returned into the focus of pharmacological research within the last 20 years. So far, several research groups reported on promising anti-inflammatory, anti-microbial and even anti-tumour effects (in vitro and in vivo). The Boswellic acids are regarded as one of the most potent active agents thereof. However, the resins still contain innumerable amounts of terpenoid compounds. Their interactions, when administered as an extract, a...

  15. Study on chromatographic fingerprint of sarcandra glabra (Thunb.) by microwave-assisted extraction coupled to HPLC/DAD

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    Microwave-assisted extraction(MAE)was used for extraction of effective components of sarcandra glabra(Thunb.),and then chromatographic fingerprint of sarcandra glabra(Thunb.)was studied by high performance liquid chromatography/diode array detector(HPLC/DAD).The conditions of MAE were optimized by an orthogonal experiment,and then the authentication and validation of the chromatographic fingerprint were conducted.Nine peaks were identified as common peaks in the fingerprint chromatograms,and isofraxidin was...

  16. In Vitro Color Change of Three Dental Veneering Resins in Tea, Coffee and Tamarind Extracts

    Directory of Open Access Journals (Sweden)

    S. Muttagi

    2011-09-01

    Full Text Available Objective: To study the in vitro color changes of three dental resin veneering materials when immersed in tea, coffee and tamarind extracts.Materials and Methods: The color changes of heat polymerized tooth colored acrylic resin (Stellondetrey, B, F14, DPI Dental products of India Ltd, Mumbai, auto polymerized tooth colored acrylic resin (DPI, B, QV5, DPI Dental products of India Ltd, Mumbai andlight polymerized resin composite (Herculite XRV, Enamel A2, part no. 22860, lot no. 910437, Kerr Corporation, West Collins Avenue, Orange, CA, USA when immersed in water extracts of tea (Tata Tea Ltd. Bangalore, India, coffee (Tata Coffee Ltd. Coorg, Indiaand tamarind were evaluated using computer vision systems. The color images were recorded in R (red, G (green and B (blue form and converted into H (hue, S (saturationand V (value.Results: Significant color change occurred for auto polymerized tooth colored acrylic resin in tamarind extract, for heat polymerized tooth colored acrylic resin in tea extract andfor light polymerized resin composite in coffee extract. Auto polymerized tooth colored acrylic resin samples showed an overall higher color change. However, for all the material samples coffee extract produced more color change.Conclusion: These results suggest that the color stability of the resins is influenced by the presence of secondary metabolites such as tartaric acid, tannins, caffeine, saponins and phenols in tamarind, tea and coffee extracts.

  17. Wound healing activity of ethanolic extract of Shorea robusta Gaertn. f. resin.

    Science.gov (United States)

    Wani, T A; Chandrashekara, H H; Kumar, D; Prasad, R; Gopal, A; Sardar, K K; Tandan, S K; Kumar, D

    2012-04-01

    The ethanolic extract of S. robusta resin (10 and 30 % w/w applied locally in excised and incised wounds) produced a dose-dependent acceleration in wound contraction and increased hydroxyproline content and tensile strength of wounds in rats. The results demonstrate wound healing activity of ethanolic extract of S. robusta resin.

  18. Variations in the contents of gingerols and chromatographic fingerprints of ginger root extracts prepared by different preparation methods.

    Science.gov (United States)

    Liu, Mei; Xia, Xinhua; Chou, Guixin; Liu, Dong; Zuberi, Aamir; Ye, Jianping; Liu, Zhijun

    2014-01-01

    In the present study, an HPLC-DAD method was optimized for the quantitative determination of 6-gingerol, 6-shogaol, 8-gingerol, and 10-gingerol in ginger extracts. A chromatographic fingerprinting method was also established to differentiate and evaluate the ginger extracts for bioactivity. Twenty-one extracts were prepared by methods differing in ginger type (fresh versus dried), solvent, and extraction methods. The ANOVA analysis showed the methods' influence on the mean extraction yields of gingerols increased in the order of: high pressure-high temperature (HP)>blender (BD)>low pressure (LP). The optimal solvent to extract gingerols was found to be 95% ethanol. The type of ginger used had significant effects on the content of gingerols, but its overall influence depended on the solvent used. In order to maximize the extraction efficiency of gingerols, a combination of dry ginger, 95% ethanol, and the HP extraction method should be employed. The chromatographic fingerprints were obtained to differentiate the unknown components from all ginger extracts. The similarity of the chromatographic fingerprints was used to evaluate the differences among all extracts. It can be concluded that the chromatographic fingerprints are able to ensure the stability of each extract and have some correlation with the observed bioactivity.

  19. Effect of ionol extraction temperature onto its gas chromatographic detection at transformer oil

    Directory of Open Access Journals (Sweden)

    Sergiy V. Zaitsev

    2015-03-01

    Full Text Available The gas chromatography used for detecting antioxidizing additive ionol at transformer oil presence helps to ensure reliable operation of oil-filled electrical equipment. Changes in the ionol preliminary extraction temperature do affect the reliability of measurement result. This study aim consisted in investigating the temperature effect on the value of extraction degree and distribution coefficients for ionol in the system “oil — ionol — ethanol” at extraction temperatures 15...75 °C. The experiment included optimization of gas chromatographic ionol in transformer oil detection conditions using method of ionol ethanol extraction and an estimated equation for a single extraction. Found is that the ionol extraction temperature increase in the range of 15...75 °C reduces the values of the ionol distribution coefficients and increases the value of ionol extraction degree and its concentration in the extract reducing the extraction duration, lowering the value of the detection threshold and the total duration of ionol in transformer oil detection. The recommended values for ionol extraction in the temperature range of 15...32 °C at a temperature of extraction 20 °C with precision temperature Δt ≤ ±1 °C, in the range of 32…40 °C, with a temperature of extraction 36 °C and Δt ≤ ±2 °C, in the range of 40...75 °C, with a temperature of extraction 65 °C and Δt ≤ ±5 °C.

  20. Quantitative high-performance liquid chromatographic determination of delta 4-3-ketosteroids in adrenocortical extracts.

    Science.gov (United States)

    Ballerini, R; Chinol, M; Ghelardoni, M

    1980-05-30

    A high-performance liquid chromatographic method is described for the determination of seven steroids in adrenocortical extracts showing a delta 4-3-ketonic conjugated system. The seven steroids (cortisol, cortisone, 11-dehydrocorticosterone, corticosterone, 11-deoxycortisol, aldosterone and 11-deoxycorticosterone) were separated with a chloroform-methanol gradient on a 5-micron silica column and with a water-acetonitrile gradient on a 10-micron RP-8 column. Effluents were monitored by UV absorption at 242 nm. Quantitative analysis was performed by comparing peak areas, which are proportional to the amounts of the individual substances (external standard method). The method is rapid, sensitive, easy to perform and reproducible.

  1. Chromatographic Separations Using Solid-Phase Extraction Cartridges: Separation of Wine Phenolics

    Science.gov (United States)

    Brenneman, Charles A.; Ebeler, Susan E.

    1999-12-01

    We describe a simple laboratory experiment that demonstrates the principles of chromatographic separation using solid-phase extraction columns and red wine. By adjusting pH and mobile phase composition, the wine is separated into three fractions of differing polarity. The content of each fraction can be monitored by UV-vis spectroscopy. When the experiment is combined with experiments involving HPLC or GC separations, students gain a greater appreciation for and understanding of the highly automated instrumental systems currently available. In addition, they learn about the chemistry of polyphenolic compounds, which are present in many foods and beverages and which are receiving much attention for their potentially beneficial health effects.

  2. Ion Exchange Extraction of Boron from Aqueous Fluids by Amberlite IRA 743 Resin

    Institute of Scientific and Technical Information of China (English)

    肖应凯; 廖步勇; 刘卫国; 肖云; SWIHART,GeorgeH.

    2003-01-01

    The ion exchange characteristics d Amherlite IRA 743 resin for extracting boron from aqueous fluids have been investigated in detail. The results show that AmherHte IRA 743 resin, a boron specific ion exchange resin, can quantitatively extract boron as the B (OH)4- spedes from weakly basle solution. Some exchangeable anions such as CI- and SO42- are present, resulting in an increase in pH value of the loeded solution within the nan, and the boron in natural aqueous fluids with low nH is also extracted by Amberlite IRA 743 resin. However, the voiume of loaded solution must be restricted. The maximum voiume of loaded solution giving quantitative extraction of boron decreases for sample soh.,tiom of lower pH value. Warm HCI solution is more effective than room temperature HCI solution for eluting boron from Amberllte IRA 743 resin.

  3. REMOVAL OF ACID-SOLUBLE LIGNIN FROM BIOMASS EXTRACTS USING AMBERLITE XAD-4 RESIN

    OpenAIRE

    Thomas James Schwartz; Martin Lawoko

    2010-01-01

    This paper describes a method for the removal of acid-soluble lignin from acid hydrolyzed hemicelluloses extracted from a mixture of northern hardwood chips, by using Amberlite XAD-4 resin, which was shown to remove 100% of furan derivatives and 90% of acid-soluble lignin. Subsequent fermentation of the resin treated hydrolyzates gave ethanol yields as high as 97% of theoretical and showed a marked increase in fermentation rate. Regeneration of resin performed with 75% acetone was 85% efficie...

  4. Chromatographic evaluation and antimicrobial activity of Neem (Azadirachta indica A. Juss., Meliaceae leaves hydroalcoholic extracts

    Directory of Open Access Journals (Sweden)

    Priscila D. Alves

    2009-06-01

    Full Text Available Neem (Azadirachta indica is an Indian tree well known for its several pharmacological activities, including antimicrobial activity. More than 300 composites have already been isolated and azadirachtin (AZA is its main active component. In the present work, Neem leaves hydroalcoholic extracts were prepared by percolation in 96% ethanol different concentrations (50%, 60%, 70%, 80% and 90% (v/v. The presence of AZA was tested by TLC by eluting the extracts and a standard solution of AZA through a chromatographic plate developed with anisaldehyde/sulfuric acid solution followed by heating. By HPLC, extracts elution took place on a C18 column, water:acetonitrile (60:40 as mobile phase, 1.0 mL/min flow rate and detection at λ217 nm. The extracts did not display AZA spots or peaks, however, they were tested against Gram-positive and Gram-negative bacteria, yeasts and a mold fungus. The extracts were tested in different increasing concentrations, in order to detect a dose-dependent relationship of the activity. Despite the absence of AZA, the 70% and 80% (v/v ethanol extracts showed activity against Staphylococcus aureus. However, this activity was not dose-dependent according to Tukey's test (q0,05;3;7.

  5. Microwave-Assisted Extraction Followed by Solid-Phase Extraction for the Chromatographic Analysis of Alkaloids in Stephania cepharantha.

    Science.gov (United States)

    Liu, Ying; Xie, Daotao; Kang, Yun; Wang, Yaqin; Yang, Ping; Guo, Jixian; Huang, Jianming

    2016-04-01

    A procedure involving microwave-assisted extraction (MAE) followed by solid-phase extraction (SPE) was established for the extraction and purification of three bisbenzylisoquinoline alkaloids from Stephania cepharantha, and a reversed-phase high-performance liquid chromatography (HPLC) method was developed for the quantification of the target alkaloids. Chromatographic separation was achieved on a Phenomenex Luna Phenyl-Hexyl column. Prior to the HPLC analysis, the alkaloids were rapidly extracted by an optimized MAE process using 0.01 mol/L hydrochloric acid as the solvent. The MAE extract was subsequently purified by SPE using a cation-exchange polymeric cartridge. The MAE-SPE procedure extracted the three alkaloids with satisfactory recoveries ranging from 100.44 to 102.12%. In comparison with the MAE, Soxhlet and ultrasonic-assisted extractions, the proposed MAE-SPE method showed satisfactory cleanup efficiency. Thus, the validated MAE-SPE-HPLC method is specific, accurate and applicable to the determination of alkaloids in S. cepharantha.

  6. Micellar liquid chromatographic determination of arbutin and hydroquinone in medicinal plant extracts and commercial cosmetic products.

    Science.gov (United States)

    Thogchai, W; Liawruangrath, B

    2013-06-01

    A simple micellar liquid chromatographic (MLC) procedure for simultaneous determination of arbutin and hydroquinone in medicinal plant extracts and commercial cosmetic products was proposed. This method was developed and validated. The chromatographic conditions were also optimized. All analyses were performed at room temperature in an isocratic mode, using a mixture of 1% (v/v) acetonitrile and 0.006 mol L⁻¹ Brij 35 (pH 6.0) as a mobile phase. The flow rate was set at 1.0 mL min⁻¹. The analytical column was a 150 × 3.9 mm Nova-Pak C-18 column. The effluent from the analytical column was monitored by UV detection at 280 nm. Under the optimum conditions, arbutin and hydroquinone could be determined within a concentration range of 2-50 μg mL⁻¹ of arbutin, and hydroquinone was obtained with the regression equations; y = 0.045x + 0.042 (r² = 0.9923) and y = 0.091x + 0.050 (r² = 0.9930) respectively. The limits of detection were found to be 0.51 μg mL⁻¹ and 0.37 μg mL⁻¹ for arbutin and hydroquinone respectively. The proposed MLC method was applied for the determination of arbutin and hydroquinone contents in medicinal plant extracts and commercial cosmetic products. This proposed MLC method is thus suitable for routine analysis of arbutin and hydroquinone in the pharmaceutical formulations, cosmetic products and raw medicinal plant extracts.

  7. A simple multi-scale Gaussian smoothing-based strategy for automatic chromatographic peak extraction.

    Science.gov (United States)

    Fu, Hai-Yan; Guo, Jun-Wei; Yu, Yong-Jie; Li, He-Dong; Cui, Hua-Peng; Liu, Ping-Ping; Wang, Bing; Wang, Sheng; Lu, Peng

    2016-06-24

    Peak detection is a critical step in chromatographic data analysis. In the present work, we developed a multi-scale Gaussian smoothing-based strategy for accurate peak extraction. The strategy consisted of three stages: background drift correction, peak detection, and peak filtration. Background drift correction was implemented using a moving window strategy. The new peak detection method is a variant of the system used by the well-known MassSpecWavelet, i.e., chromatographic peaks are found at local maximum values under various smoothing window scales. Therefore, peaks can be detected through the ridge lines of maximum values under these window scales, and signals that are monotonously increased/decreased around the peak position could be treated as part of the peak. Instrumental noise was estimated after peak elimination, and a peak filtration strategy was performed to remove peaks with signal-to-noise ratios smaller than 3. The performance of our method was evaluated using two complex datasets. These datasets include essential oil samples for quality control obtained from gas chromatography and tobacco plant samples for metabolic profiling analysis obtained from gas chromatography coupled with mass spectrometry. Results confirmed the reasonability of the developed method.

  8. Extraction chromatographic separation of Am(III) and Eu(III) by TPEN-immobilized gel

    Energy Technology Data Exchange (ETDEWEB)

    Takeshita, K. [Research Laboratory for Nuclear Reactors, Tokyo Institute of Technology, 2-12-1 Ookayama, Meguro-ku, Tokyo 157-8550 (Japan); Ogata, T.; Oaki, H.; Inaba, Y. [Solutions Research Organization, Tokyo Institute of Technology, 4259 Nagatsuta-cho, Midori-ku, Yokohama, Kanagawa 226-8503 (Japan); Mori, A. [Department of Chemical Science and Engineering, Kobe University, 1-1 Rokkodai-cho, Nada-ku, Kobe 657-8501 (Japan); Yaita, T. [Tokai Research and Development Center, Japan Atomic Energy Agency, 2-4 Shirakata-shirane, Tokai-mura, Naka-gun, Ibaragi 319-1195 (Japan); Koyama, S.I. [Oarai Research and Development Center, Japan Atomic Energy Agency. 4002 Narita, Oarai-cho, Ibaraki 311-1393 (Japan)

    2013-07-01

    A TPEN derivative with 4 vinyl groups, N,N,N',N' -tetrakis-(4-propenyloxy-2-pyridylmethyl)ethylenediamine (TPPEN) was synthesized for the separation of trivalent minor actinides (Am(III)) and lanthanides (Eu(III)). A co-polymer gel with TPPEN and N-isopropylacrylamide (NIPA) showed a high separation factor of Am(III) over Eu(III) (SF[Am/Eu]), which was evaluated to be 26 at pH=5. Thin film of NIPA-TPPEN gel (average thickness: 2-40 nm) was immobilized on the pore surface in porous silica particles (particle diameter : 50 μm, average pore diameter : 50 and 300 nm) and a chromatographic column (diameter: 6 mm, height: 11 mm) packed with the gel-coated particles was prepared. A small amount of weakly acidic solution (pH=4) containing Am(III) and Eu(III) was supplied in the column and the elution tests of Am(III) and Eu(III) were carried out. Eu(III) was recovered separately by a weakly acidic eluent (pH=4) at 313 K and Am(III) by a highly acidic eluent (pH=2) at 298 K. These results suggest that the contentious separation of minor actinides and lanthanides is attainable by a new extraction chromatographic process with two columns adjusted to 298 K and 313 K. (authors)

  9. Antimicrobial Activity and Chromatographic Analysis of Extracts from Tropaeolum pentaphyllum Lam. Tubers

    Directory of Open Access Journals (Sweden)

    Ritiel Corrêa da Cruz

    2016-04-01

    Full Text Available Background: Tropaeolum pentaphyllum Lam. tubers (Tropaeolaceae are known and used as a condiment and for the treatment of skin infections in Southern Brazil. However, its activity and composition has not yet been investigated. Thus, different extracts and the essential oil from the tubers were tested against a range of microorganisms. The most active extracts were submitted to chromatographic analysis. Methods: Hydroalcoholic extract (70%, fractions of it, and the essential oil from the tubers were tested against several bacteria, yeasts and molds, furnishing the corresponding inhibitory, bactericidal and fungicidal minimal concentration values. The most active extracts were submitted to GC-MS investigation. Results: The strongest effects against different strains of microorganisms, such as Gram-positive and negative bacteria, Candida spp. and dermatophytes were observed for the essential oil and the chloroform fraction, with minimal inhibitory concentrations (MICs well below 200 µg/mL. GC-MS analysis revealed that the major essential oil constituent is benzyl isothiocyanate (BITC, while the chloroform fraction is constituted of BITC, amides, sulfur, fatty acids and its esters, all compounds that may be related to the demonstrated activity. Conclusions: Overall, the results support the popular use of the plant for the treatment of skin infections, and revealed the main active compounds.

  10. The transverse strength of acrylic resin after Coleus amboinicus, Lour extract solution immersion

    Directory of Open Access Journals (Sweden)

    Devi Rianti

    2006-12-01

    Full Text Available A laboratoric experimental study was conducted on the transverse strength of acrylic resin after Coleus amboinicus, Lour extract solution immersion. The aim of this study is to know the difference of acrylic resin transverse strengths caused by immersion time variations in a concentrate solution. The study was carried out on unpolished acrylic resin plates with 65 × 10 × 2,5 mm dimension; solution with 15% Coleus amboinicus, Lour extract, and 30, 60, 90 days immersion times to measure the transverse strength and sterilized aquadest was used as control. Acrylic resin plates transverse strength was measured using Autograph AG-10 TE. The data was analyzed using One-Way Anova and LSD with 5% degree of significance. The result showed that longer immersion time will decrease the transverse strength of the acrylic resin plates. After 90 days immersion time, the transverse strength decrease is still above the recommended standard transverse strength.

  11. Solid-phase extraction and liquid chromatographic quantitation of quinfamide in biological samples.

    Science.gov (United States)

    Morales, J M; Jung, C H; Alarcón, A; Barreda, A

    2000-09-15

    This paper describes a high-performance liquid chromatographic method for the assay of quinfamide and its main metabolite, 1-(dichloroacetyl)-1,2,3,4,-tetrahydro-6-quinolinol, in plasma, urine and feces. It requires 1 ml of biological fluid, an extraction using Sep-Pack cartridges and acetonitrile for drug elution. Analysis was performed on a CN column (5 microm) using water-acetonitrile-methanol (40:50:10) as a mobile phase at 269 nm. Results showed that the assay was linear in the range between 0.08 and 2.0 microg/ml. The limit of quantitation was 0.08 microg/ml. Maximum assay coefficient of variation was 14%. Recovery obtained in plasma, urine and feces ranged from 82% to 98%.

  12. Chromatographic determination of cyanoglycosides prunasin and amygdalin in plant extracts using a porous graphitic carbon column.

    Science.gov (United States)

    Berenguer-Navarro, V; Giner-Galván, R M; Grané-Teruel, N; Arrazola-Paternina, G

    2002-11-20

    The determination of cyanogenic compounds in plants is often performed by HPLC. However, in this analysis, interferences due to compounds in the matrix, such as tannins and other pigments, are encountered, especially in roots and leaves. A new method is proposed for determining the cyanogenic glycosides amygdalin (D-mandelonitrile beta-D-gentiobioside) and prunasin (D-mandelonitrile beta-D-glucoside) in almond tree tissues, using poly(vinylpyrrolidone) or active carbon as scavengers for extracting cyanogenic compounds from roots or leaves, respectively. A new chromatographic approach for conducting the analysis is also discussed herein. The advantages of a Hypercarb column for the analysis of prunasin in roots are shown. The correlation coefficient with a reference method is high (>0.99), and statistical tests prove that the two methods are equivalent. In addition, the results provide evidence that prunasin is the only cyanoglycoside present in almond tree roots.

  13. Thin-layer chromatographic (TLC) separations and bioassays of plant extracts to identify antimicrobial compounds.

    Science.gov (United States)

    Kagan, Isabelle A; Flythe, Michael D

    2014-03-27

    A common screen for plant antimicrobial compounds consists of separating plant extracts by paper or thin-layer chromatography (PC or TLC), exposing the chromatograms to microbial suspensions (e.g. fungi or bacteria in broth or agar), allowing time for the microbes to grow in a humid environment, and visualizing zones with no microbial growth. The effectiveness of this screening method, known as bioautography, depends on both the quality of the chromatographic separation and the care taken with microbial culture conditions. This paper describes standard protocols for TLC and contact bioautography with a novel application to amino acid-fermenting bacteria. The extract is separated on flexible (aluminum-backed) silica TLC plates, and bands are visualized under ultraviolet (UV) light. Zones are cut out and incubated face down onto agar inoculated with the test microorganism. Inhibitory bands are visualized by staining the agar plates with tetrazolium red. The method is applied to the separation of red clover (Trifolium pratense cv. Kenland) phenolic compounds and their screening for activity against Clostridium sticklandii, a hyper ammonia-producing bacterium (HAB) that is native to the bovine rumen. The TLC methods apply to many types of plant extracts and other bacterial species (aerobic or anaerobic), as well as fungi, can be used as test organisms if culture conditions are modified to fit the growth requirements of the species.

  14. Extraction chromatographic methods in the sample preparation sequence for thermal ionization mass spectrometric analysis of plutonium isotopes.

    Science.gov (United States)

    Grate, Jay W; O'Hara, Matthew J; Farawila, Anne F; Douglas, Matthew; Haney, Morgan M; Petersen, Steven L; Maiti, Tapas C; Aardahl, Christopher L

    2011-12-01

    A sample preparation sequence for actinide isotopic analysis by thermal ionization mass spectrometry (TIMS) is described that includes column-based extraction chromatography as the first separation step, followed by anion-exchange column separations. The sequence is designed to include a wet ashing step after the extraction chromatography to prevent any leached extractant or oxalic acid eluent reagents from interfering with subsequent separations, source preparation, or TIMS ionization. TEVA resin and DGA resin materials, containing extractants that consist only of C, N, O, and H atoms, were investigated for isolation of plutonium. Radiotracer level studies confirmed expected high yields from column-based separation procedures. Femtogram-level studies were carried out with TIMS detection, using multiple monoisotopic spikes applied sequentially throughout the separation sequence. Pu recoveries were 87% and 86% for TEVA and DGA resin separations, respectively. The Pu recoveries from 400 μL anion-exchange column separation sequences were 89% and 93% for trial sequences incorporating TEVA and DGA resin. Thus, a prior extraction chromatography step in the sequence did not interfere with the subsequent anion-exchange separation when a simple wet ash step was carried out in between these column separations. The average measurement efficiency for Pu, encompassing the chemical separation recoveries and the TIMS ionization efficiency, was 2.73% ± 0.77% (2σ) for the DGA resin trials and 2.67% ± 0.54% for the TEVA resin trials, compared to 3.41% and 2.37% (average 2.89%) for two control trials. These compare with an average measurement efficiency of 2.78% ± 1.70%, n = 33 from process benchmark analyses using Pu spikes processed through a sequence of oxalate precipitation, wet ash, iron hydroxide precipitation, and anion-exchange column separations. We conclude that extraction chromatography can be a viable separation procedure as part of a multistep sequence for TIMS

  15. Adsorption of saponin compound in Carica papaya leaves extract using weakly basic ion exchanger resin

    Science.gov (United States)

    Abidin, Noraziani Zainal; Janam, Anathasia; Zubairi, Saiful Irwan

    2016-11-01

    Adsorption of saponin compound in papaya leaves juice extract using Amberlite® IRA-67 resin was not reported in previous studies. In this research, Amberlite® IRA-67 was used to determine the amount of saponin that can be adsorbed using different weights of dry resin (0.1 g and 0.5 g). Peleg model was used to determine the maximum yield of saponin (43.67 mg) and the exhaustive time (5.7 days) prior to a preliminary resin-saponin adsorption study. After adsorption process, there was no significant difference (p>0.05) in total saponin content (mg) for sample treated with 0.1 g (3.79 ± 0.55 mg) and sample treated with 0.5 g (3.43 ± 0.51 mg) dry weight resin. Long-term kinetic adsorption of resin-saponin method (>24 hours) should be conducted to obtain optimum freed saponin extract. Besides that, sample treated with 0.1 g dry weight resin had high free radical scavenging value of 50.33 ± 2.74% compared to sample treated with 0.5 g dry weight resin that had low free radical scavenging value of 24.54 ± 1.66% dry weights. Total saponin content (mg), total phenolic content (mg GAE) and free radical scavenging activity (%) was investigated to determine the interaction of those compounds with Amberlite® IRA-67. The RP-HPLC analysis using ursolic acid as standard at 203 nm showed no peak even though ursolic acid was one of the saponin components that was ubiquitous in plant kingdom. The absence of peak was due to weak solubility of ursolic acid in water and since it was only soluble in solvent with moderate polarity. The Pearson's correlation coefficient for total saponin content (mg) versus total phenolic content (mg GAE) and radical scavenging activity (%) were +0.959 and +0.807. Positive values showed that whenever there was an increase in saponin content (mg), the phenolic content (mg GAE) and radical scavenging activity (%) would also increase. However, as the resin-saponin adsorption was carried out, there was a significant decrease of radical scavenging activity

  16. VALIDATION OF AN EPA METHOD FOR THE ION CHROMATOGRAPHIC DETERMINATION OF PERCHLORATE IN FERTILIZERS USING A POLYVINYL ALCOHOL GEL RESIN.

    Science.gov (United States)

    This paper summarizes the key points of a joint study between the EPA and Metrohm-Peak, Inc., on the use of polyvinyl alcohol [PVA] columns for the ion chromatographic determination of percholorate in aqueous leachates or solutions of fertilizers. A series of fertilizer samples ...

  17. REMOVAL OF GLUCORAPHENIN FROM THE EXTRACT OF RADISH PIGMENT BY ANION EXCHANGE RESIN 201×7

    Institute of Scientific and Technical Information of China (English)

    ZhouXiaohua; ChenQi

    1998-01-01

    A method for removimg glucoraphenin from the extract of Radish pigment by anion exchange resin 201×7 was studied.The adsorption capacity of 201×7 resin for glucoraphenin was 72.8mg/ml resin,the equilibrium time 55 minutes,and the optinum pH5.5.All glucoraphenin that had been adsorbed on 201×7 resin was eluted by 1.5BV.hr-1, eluent in whinc concentration of NaOH was 0.05mol·L-1 at the flow rate of 1.5BV/h.Extracting solution of deglucoraphenin was enriched by vacuum and spray drying.A powder product of Radish pigment was obtained and E1cm1%=4.30.

  18. REMOVAL OF ACID-SOLUBLE LIGNIN FROM BIOMASS EXTRACTS USING AMBERLITE XAD-4 RESIN

    Directory of Open Access Journals (Sweden)

    Thomas James Schwartz

    2010-09-01

    Full Text Available This paper describes a method for the removal of acid-soluble lignin from acid hydrolyzed hemicelluloses extracted from a mixture of northern hardwood chips, by using Amberlite XAD-4 resin, which was shown to remove 100% of furan derivatives and 90% of acid-soluble lignin. Subsequent fermentation of the resin treated hydrolyzates gave ethanol yields as high as 97% of theoretical and showed a marked increase in fermentation rate. Regeneration of resin performed with 75% acetone was 85% efficient with respect to acid soluble lignin.

  19. HPLC method development for the online-coupling of chromatographic Perilla frutescens extract separation with xanthine oxidase enzymatic assay.

    Science.gov (United States)

    Kaufmann, Christine M; Grassmann, Johanna; Letzel, Thomas

    2016-05-30

    Enzyme-regulatory effects of compounds contained in complex mixtures can be unveiled by coupling a continuous-flow enzyme assay to a chromatographic separation. A temperature-elevated separation was developed and the performance was tested using Perilla frutescens plant extracts of various polarity (water, methanol, ethanol/water). Owning to the need of maintaining sufficient enzymatic activity, only low organic solvent concentrations can be added to the mobile phase. Hence, to broaden the spectrum of eluting compounds, two different organic solvents and various contents were tested. The chromatographic performance and elution was further improved by the application of a moderate temperature gradient to the column. By taking the effect of eluent composition as well as calculated logD values and molecular structure of known extract compounds into account, unknown features were tentatively assigned. The method used allowed the successful observation of an enzymatic inhibition caused by P. frutescens extract.

  20. Extraction of high quality DNA from seized Moroccan cannabis resin (Hashish.

    Directory of Open Access Journals (Sweden)

    Moulay Abdelaziz El Alaoui

    Full Text Available The extraction and purification of nucleic acids is the first step in most molecular biology analysis techniques. The objective of this work is to obtain highly purified nucleic acids derived from Cannabis sativa resin seizure in order to conduct a DNA typing method for the individualization of cannabis resin samples. To obtain highly purified nucleic acids from cannabis resin (Hashish free from contaminants that cause inhibition of PCR reaction, we have tested two protocols: the CTAB protocol of Wagner and a CTAB protocol described by Somma (2004 adapted for difficult matrix. We obtained high quality genomic DNA from 8 cannabis resin seizures using the adapted protocol. DNA extracted by the Wagner CTAB protocol failed to give polymerase chain reaction (PCR amplification of tetrahydrocannabinolic acid (THCA synthase coding gene. However, the extracted DNA by the second protocol permits amplification of THCA synthase coding gene using different sets of primers as assessed by PCR. We describe here for the first time the possibility of DNA extraction from (Hashish resin derived from Cannabis sativa. This allows the use of DNA molecular tests under special forensic circumstances.

  1. Aminoalkylated Merrifield Resins Reticulated by Tris-(2-chloroethyl Phosphate for Cadmium, Copper, and Iron (II Extraction

    Directory of Open Access Journals (Sweden)

    Mokhtar Dardouri

    2015-01-01

    Full Text Available We aimed to synthesize novel substituted polymers bearing functional groups to chelate heavy metals during depollution applications. Three polyamine functionalized Merrifield resins were prepared via ethylenediamine (EDA, diethylenetriamine (DETA, and triethylenetetramine (TETA modifications named, respectively, MR-EDA, MR-DETA, and MR-TETA. The aminoalkylated polymers were subsequently reticulated by tris-(2-chloroethyl phosphate (TCEP to obtain new polymeric resins called, respectively, MR-EDA-TCEP, MR-DETA-TCEP, and MR-TETA-TCEP. The obtained resins were characterized via attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR, elemental analysis (EA, and thermogravimetric (TGA, thermodynamic (DTA, and differential thermogravimetric (DTG analysis. The synthesized resins were then assayed to evaluate their efficiency to extract metallic ions such as Cd2+, Cu2+, and Fe2+ from aqueous solutions.

  2. Assessing similarity analysis of chromatographic fingerprints of Cyclopia subternata extracts as potential screening tool for in vitro glucose utilisation.

    Science.gov (United States)

    Schulze, Alexandra E; De Beer, Dalene; Mazibuko, Sithandiwe E; Muller, Christo J F; Roux, Candice; Willenburg, Elize L; Nyunaï, Nyemb; Louw, Johan; Manley, Marena; Joubert, Elizabeth

    2016-01-01

    Similarity analysis of the phenolic fingerprints of a large number of aqueous extracts of Cyclopia subternata, obtained by high-performance liquid chromatography (HPLC), was evaluated as a potential tool to screen extracts for relative bioactivity. The assessment was based on the (dis)similarity of their fingerprints to that of a reference active extract of C. subternata, proven to enhance glucose uptake in vitro and in vivo. In vitro testing of extracts, selected as being most similar (n = 5; r ≥ 0.962) and most dissimilar (n = 5; r ≤ 0.688) to the reference active extract, showed that no clear pattern in terms of relative glucose uptake efficacy in C2C12 myocytes emerged, irrespective of the dose. Some of the most dissimilar extracts had higher glucose-lowering activity than the reference active extract. Principal component analysis revealed the major compounds responsible for the most variation within the chromatographic fingerprints, as mangiferin, isomangiferin, iriflophenone-3-C-β-D-glucoside-4-O-β-D-glucoside, iriflophenone-3-C-β-D-glucoside, scolymoside, and phloretin-3',5'-di-C-β-D-glucoside. Quantitative analysis of the selected extracts showed that the most dissimilar extracts contained the highest mangiferin and isomangiferin levels, whilst the most similar extracts had the highest scolymoside content. These compounds demonstrated similar glucose uptake efficacy in C2C12 myocytes. It can be concluded that (dis)similarity of chromatographic fingerprints of extracts of unknown activity to that of a proven bioactive extract does not necessarily translate to lower or higher bioactivity.

  3. [Purification technology of procymidone residues in ginseng extracts by macroporous resins].

    Science.gov (United States)

    Cui, Li-Li; Zheng, Pei-He; Wang, Ying-Ping

    2014-07-01

    The macroporous resin separation technology has been mainly applied in the enrichment of saponins, flavonoids, alkaloids and other ingredients, and used in the removal of heavy metal impurities and pesticide residues in recent years. This paper focuses on the synthesis of the new-type macroporous adsorption resin LKS-11 according to the molecular structure characteristics of procymidone. Specifically, the selective absorptive property and other advantages of macroporous resin were utilized to analyze the procymidone removal efficiency in ginseng extracts from different sources. The type of macroporous resins, absorptive property and desorption conditions were observed respectively by static and dynamic adsorption methods to determined the optimum process conditions. According to the results, LKS-11 showed a good absorptive property to procymidone in ginseng extracts and provided a theoretical basis for studies on the removal of procymidone residues from ginseng extracts by using macroporous adsorption resin. Because of no secondary pollution on samples, low production and operation costs, high procymidone removal efficiency and high product recovery rate, this method is suitable to be applied in production.

  4. N-Acetyl cysteine restores viability and function of rat odontoblast-like cells impaired by polymethylmethacrylate dental resin extract.

    Science.gov (United States)

    Yamada, Masahiro; Kojima, Norinaga; Att, Wael; Hori, Norio; Suzuki, Takeo; Ogawa, Takahiro

    2009-01-01

    There is concern that dental-resin materials directly loaded on a prepared tooth adversely affect dental pulp tissue by releasing the resin chemicals through dentinal tubes. This study determined whether self-curing polymethyl methacrylate (PMMA)-based dental resin extract adversely affected the viability and function of odontoblast-like cells and whether the cytotoxicity of this resin, if any, could be eliminated by N-acetyl cysteine, an antioxidant amino acid derivative. Odontoblast-like cells isolated from rat maxillary incisor dental pulp tissue were exposed to a PMMA resin extract with or without N-acetyl cysteine for 1 h and then cultured in osteoblastic media. The percentage of viable cells 24 h after seeding was 20% in cells exposed to the resin extract without N-acetyl cysteine, whereas 45% of cells were viable after exposure to the N-acetyl cysteine-supplemented extract. The cells that had been exposed to the extract showed a strong tendency for apoptosis associated with the increased reactive oxygen species production and decreased intracellular glutathione level, which was improved by the addition of N-acetyl cysteine. N-Acetyl cysteine supplementation almost completely restored the significantly reduced alkaline phosphatase activity and matrix mineralization by the resin extract. These results conclusively demonstrated that exposure of odontoblast-like cells to the resin extract impaired the cell viability and function and, more intriguingly, N-acetyl cysteine supplementation to the extract significantly prevented these toxic effects.

  5. Fundulus heteroclitus gonadotropins.5: Small scale chromatographic fractionation of pituitary extracts into components with different steroidogenic activities using homologous bioassays

    Directory of Open Access Journals (Sweden)

    Petrino Teresa R

    2004-03-01

    Full Text Available Abstract Fractionation and characterization of gonadotropins (GtH from Fundulus heteroclitus pituitary extracts were carried out using a biocompatible liquid chromatographic procedure (Pharmacia FPLC system. Chromatographic fractions were monitored for gonadotropic activities (induction of oocyte maturation and steroid production using homologous follicle bioassays in vitro. Size-exclusion chromatography eluted gonadotropic activity in one major protein peak (Mr ~ 30,000. Anion-exchange and hydrophobic-interaction chromatography (HIC yielded two distinct peaks of 17beta-estradiol (E2- and 17alpha-hydroxy,20beta-dihydroprogesterone (DHP-promoting activity with associated oocyte maturation. Two-dimensional chromatography (chromatofocusing followed by HIC resolved pituitary extracts into two active fractions; both induced E2 synthesis, but one was relatively poor in eliciting DHP and testosterone production. Thus, using homologous bioassays, at least two quantitatively different gonadotropic (steroidogenic activities: an E2-promoting gonadotropin (GtH I-like and a DHP-promoting gonadotropin (GtH II-like, which has a lower isoelectric point but greater hydrophobicity than the former, can be distinguished from F. heteroclitus pituitaries by a variety of chromatographic procedures. This study complements previous biochemical and molecular data in F. heteroclitus and substantiates the duality of GtH function in a multiple-spawning teleost.

  6. Fundulus heteroclitus gonadotropins.5: Small scale chromatographic fractionation of pituitary extracts into components with different steroidogenic activities using homologous bioassays

    Science.gov (United States)

    Lin, Yu-Wai Peter; Petrino, Teresa R; Wallace, Robin A

    2004-01-01

    Fractionation and characterization of gonadotropins (GtH) from Fundulus heteroclitus pituitary extracts were carried out using a biocompatible liquid chromatographic procedure (Pharmacia FPLC system). Chromatographic fractions were monitored for gonadotropic activities (induction of oocyte maturation and steroid production) using homologous follicle bioassays in vitro. Size-exclusion chromatography eluted gonadotropic activity in one major protein peak (Mr ~ 30,000). Anion-exchange and hydrophobic-interaction chromatography (HIC) yielded two distinct peaks of 17beta-estradiol (E2)- and 17alpha-hydroxy,20beta-dihydroprogesterone (DHP)-promoting activity with associated oocyte maturation. Two-dimensional chromatography (chromatofocusing followed by HIC) resolved pituitary extracts into two active fractions; both induced E2 synthesis, but one was relatively poor in eliciting DHP and testosterone production. Thus, using homologous bioassays, at least two quantitatively different gonadotropic (steroidogenic) activities: an E2-promoting gonadotropin (GtH I-like) and a DHP-promoting gonadotropin (GtH II-like), which has a lower isoelectric point but greater hydrophobicity than the former, can be distinguished from F. heteroclitus pituitaries by a variety of chromatographic procedures. This study complements previous biochemical and molecular data in F. heteroclitus and substantiates the duality of GtH function in a multiple-spawning teleost. PMID:15040801

  7. Ionic-liquid-impregnated resin for the microwave-assisted solid-liquid extraction of triazine herbicides in honey.

    Science.gov (United States)

    Wu, Lijie; Song, Ying; Hu, Mingzhu; Yu, Cui; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming

    2015-09-01

    Microwave-assisted ionic-liquid-impregnated resin solid-liquid extraction was developed for the extraction of triazine herbicides, including cyanazine, metribuzin, desmetryn, secbumeton, terbumeton, terbuthylazine, dimethametryn, and dipropetryn in honey samples. The ionic-liquid-impregnated resin was prepared by immobilizing 1-hexyl-3-methylimidazolium hexafluorophosphate in the microspores of resin. The resin was used as the extraction adsorbent. The extraction and enrichment of analytes were performed in a single step. The extraction time can be shortened greatly with the help of microwave. The effects of experimental parameters including type of resin, type of ionic liquid, mass ratio of resin to ionic liquid, extraction time, amount of the impregnated resin, extraction temperature, salt concentration, and desorption conditions on the extraction efficiency, were investigated. A Box-Behnken design was applied to the selection of the experimental parameters. The recoveries were in the range of 80.1 to 103.4% and the relative standard deviations were lower than 6.8%. The present method was applied to the analysis of honey samples.

  8. Maximizing Chromatographic Information from Environmental Extracts by GCxGC-ToF-MS

    NARCIS (Netherlands)

    Skoczynska, E.M.; Korytar, P.; Boer, de J.

    2008-01-01

    Comprehensive two-dimensional gas chromatography (GCxGC) coupled with a time-of-flight (ToF) detector allows the separation of many constituents of previously unresolved complex mixtures (UCM) of contaminants in sediment samples. In addition to the powerful chromatographic resolution, automated mass

  9. Separation and purification of rebaudioside A from extract of Stevia Rebaudiana leaves by macroporous adsorption resins

    Directory of Open Access Journals (Sweden)

    Anvari Masoumeh

    2016-03-01

    Full Text Available The separation and purification of rebaudioside A from Stevia rebaudiana crude extracts (Steviosides by macroporous resin were optimized by Taguchi orthogonal array (OA experimental design methodology. This approach was applied to evaluate the influence of five factors (adsorption temperature, desorption time, elution solution ratio, adsorption volume and type of resin on the rebaudioside A yield. The percentage contribution of each factor was also determined. The results showed that elution solution ratio and adsorption volume made the greatest (59.6% and the lowest (1.3% contribution, respectively. The results showed that the Taguchi method is able to model the purification of rebaudioside A process well (R2 > 0.998 and can therefore be applied in future studies conducted in various fields. Adsorption temperature 35°C, desorption time 60min, elution solution ratio 3, adsorption volume 200ml and HPD-400 as resin were the best conditions determined by the Taguchi method.

  10. Chronic swelling from entrapment of acrylic resin in a surgical extraction site

    Directory of Open Access Journals (Sweden)

    Weiting Ho

    2010-01-01

    Full Text Available When acrylic resin is inadvertently embedded in oral tissue, it can result in a pronounced chronic inflammatory response. This report describes a case in which temporary crown and bridge resin was forced into a surgical extraction site after the two adjacent teeth were prepared for a bridge immediately following extraction of a maxillary premolar. The patient experienced swelling at the extraction site over a ten month period despite treatment with antibiotics and anti-inflammatory drugs. After detection and removal of the foreign body, the symptoms resolved. The episode contributed to periodontal bone loss around an adjacent tooth. While morbidity of this nature is rare, this case reinforces the need to investigate persistent signs of inflammation and account for dental materials that are lost during the course of treatment.

  11. Genetic toxicology of dental composite resin extracts in somatic cells in vivo.

    Science.gov (United States)

    Arossi, Guilherme Anziliero; Dihl, Rafael Rodrigues; Lehmann, Mauricio; Reguly, Maria Luiza; de Andrade, Heloísa Helena Rodrigues

    2010-07-01

    The aim of this study was to assess the potential genetic toxicity associated to nine aqueous extracts from dental composite resins (Charisma, Fill Magic, Fill Magic Flow, Durafill, TPH Spectrum, Concept, Natural Look, Filtek Z250 and Filtek P60) and one random extract. Homologous mitotic recombination, point and chromosomal mutation effects were determined in somatic proliferative cells of Drosophila melanogaster exposed to aqueous extracts of the clinically used composites. Reproducible increases in clone mutant spot frequencies induced by diluted extract of Fill Magic Flow were observed. These increments were exclusively associated to the induction of homologous recombination - a genetic phenomenon involved in the loss of heterozygosis. The other eight composite resins and the random extract had no statistically significant effect on total spot frequencies - suggesting that they are non-genotoxic in the somatic mutation and recombination test assay, which agrees with the applications they have in dentistry. These findings - supported by numerous studies showing a positive correlation between carcinogenicity in man and genotoxicity in the Drosophila wing spot test - point to the potential risks some composite resins pose to the health of patients and dentistry personnel.

  12. Effect of apricot tree resin hydroethanolic extract on skin wound healing in rats

    Directory of Open Access Journals (Sweden)

    Karim Javadabadi

    2017-03-01

    Full Text Available Background : Impairment of wound healing in chronic diseases is a therapeutic challenge. In terms of anti-inflammatory and regenerative effects of hydro-alcoholic extract of apricot gum tree this extract used on skin wound healing in rats. Materials and Methods: 28 Wistar male rats were divided into four groups: group I, normal without surgery, group II, control group without treatment, group III, a wound treatment with Vaseline, and group I˅, wound care therapy apricot tree resin extract. In the treated and placebo groups after anesthesia applied induction circular wound area of 280 square millimeters behind rats, but treated groups continued treatment for 21 days. Daily treatment was done with hydro-alcoholic extract of apricot tree gum. Wound size is measured every day by analyzing digital images for 21 days and then rats killed and samples were fixed in formalin. Slices were stained with hematoxylin and eosin. Tissue sections were studied qualitatively and quantitatively, to check regeneration of cells, the collagen fibers, angiogenesis, and distribution of inflammatory cells. Normal data analyzed using Tukey test and data with non-normal distribution were compared between groups by Mann-Whitney test. Results: Use of apricot tree resin, reduces the blood vessels from the second week onwards, reduction of inflammatory cells and increased collagen fibers and tissue epithelialization. Conclusion: Apricot tree resin extract can promote wound healing faster made substantial improvements.

  13. Extracting gold from pyrite roster cinder by ultra-fine-grinding and resin-in-pulp

    Institute of Scientific and Technical Information of China (English)

    危俊婷; 严规有; 郭炳昆; 高桂兰

    2003-01-01

    The ultra-fine-grinding and resin-in-pulp with pH value of 10 are used to extract gold from pyrite roster cinder. During leaching process, aluminium oxide ball is used as stirring medium, hydrogen peroxide as leaching agent and sodium hexametaphosphate as grinding agent. With AM-26 resin as absorber and sulfocarbamide as eluent, gold is recovered from cyanide pulp of pyrite roster cinder by resin-in-pulp. The effects of contact time, temperature and acidity etc. on the gold absorption are investigated by static methods and dynamic method respectively. The effects of flow rate of solution on dynamic adsorption and elution of gold are studied. The results show that AM-26 resin has good adsorbability in cyanide solution, and gold can be easily eluated from the loaded resin with 0. 1mol/L hydrochloric acid and lmol/L sulfocabamide. The adsorption rate and the elution of gold exceed 98%. When leaching time is 2 h, mass ratio of liquid to solid 4: 1, consumption of sodium cyanide 3 kg/t, concentration of hydrogen peroxide and sodium hexametaphosphate 0. 05% respectively, adsorption time 30 min, temperature 10-30 ℃, volume of resin 3 mL, ratio of eluent to resin (10-20): 1, velocity of eluent 1.5 mL/min, the leaching rate of gold reaches 85%. Compared with traditional leaching technology, it can reduce leaching time, avoid complex filter process, decrease sodium cyanide consumption and increase leaching rate of gold by 35%.

  14. Comparison of extracts and toxicities of organic compounds in drinking water concentrated by single and composite XAD resins.

    Science.gov (United States)

    Zhou, Xue; Xiang, Lunhui; Wu, Fenghong; Peng, Xiaoling; Xie, Hong; Wang, Jiachun; Yang, Kedi; Lu, Wenqing; Wu, Zhigang

    2013-12-01

    We compared extracts and toxicities of organic compounds (OCs) in drinking water concentrated by composite XAD-2/8 resin (mixed with an equal volume of XAD-2 and XAD-8 resins) with those extracted by single XAD-2 (non-polar) and XAD-8 (polar) resins. Drinking water was processed from raw water of the Han River and the Yangtze River in Wuhan section, China. The extraction efficiency of all resins was controlled at 30%. The types of extracted OCs were detected by gas chromatography-mass spectrometry, and the cytotoxicity and genotoxicity were assessed by MTT (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) and comet assays, respectively, in human hepatoma HepG2 cells. Our results showed that XAD-2/8 extracted a larger variety of OCs, compared with XAD-8 and XAD-2. The cytotoxicity and genotoxicity of extracted OCs were in the order of XAD-8> XAD-2/8> XAD-2 at almost all tested concentrations after 24 h treatment (P < 0.05). Our findings suggest that single XAD resin selectively extracts either polar or non-polar OCs, which would lead to over- or under-estimation of the toxicity of drinking water. Nevertheless, composite resin extracts both polar and non-polar OCs, and could be utilized as a useful extraction technique to evaluate the level and toxicity of OCs in drinking water.

  15. Effect of hawthorn (Crataegus oxycantha) crude extract and chromatographic fractions on multiple activities in a cultured cardiomyocyte assay.

    Science.gov (United States)

    Long, S R; Carey, R A; Crofoot, K M; Proteau, P J; Filtz, T M

    2006-11-01

    Extracts of hawthorn (Crataegus oxycantha) have become popular herbal supplements for their well-recognized cardiotonic effects. Many commercial preparations have been used successfully in the treatment of congestive heart failure, although the active principles within these extracts have yet to be conclusively identified. Several hawthorn preparations were studied and found to have negative chronotropic effects in a cultured neonatal murine cardiomyocyte assay using unpaced cells. As compared to conventional cardiac drugs (i.e., epinephrine, milrinone, ouabain, or propranolol), hawthorn extract has a unique activity profile. Hawthorn extract appears to be anti-arrhythmic and capable of inducing rhythmicity in quiescent cardiomyocytes. Hawthorn extract does not cause beta-adrenergic receptor blockade at concentrations which cause negative chronotropic effects. Commercial hawthorn preparations, extracts prepared from dried leaves and those made from dried berries have similar chronotropic activities. When crude extracts are separated using size-exclusion chromatography, several fractions retain multiple cardiac activities. Assays with chromatographic fractions reveal that multiple dissimilar cardioactive components may exist within the extract, making the identification of individual active constituents more challenging.

  16. Extractant selection strategy for solvent-impregnated resins in fermentations

    NARCIS (Netherlands)

    Berg, C. van den; Roelands, C.P.M.; Bussmann, P.J.Th.; Goetheer, E.L.V.; Verdoes, D.; Wielen, L. van der

    2008-01-01

    The application of extractants in whole-cell biocatalysis can have a positive impact on industrial fermentations, in terms of productivity, total amount of product produced, and cell growth. When a product is continuously removed from the microorganism surroundings, product inhibition will be dimini

  17. Gas purge microsyringe extraction for quantitative direct gas chromatographic-mass spectrometric analysis of volatile and semivolatile chemicals.

    Science.gov (United States)

    Yang, Cui; Piao, Xiangfan; Qiu, Jinxue; Wang, Xiaoping; Ren, Chunyan; Li, Donghao

    2011-03-25

    Sample pretreatment before chromatographic analysis is the most time consuming and error prone part of analytical procedures, yet it is a key factor in the final success of the analysis. A quantitative and fast liquid phase microextraction technique termed as gas purge microsyringe extraction (GP-MSE) has been developed for simultaneous direct gas chromatography-mass spectrometry (GC-MS) analysis of volatile and semivolatile chemicals without cleanup process. Use of a gas flowing system, temperature control and a conventional microsyringe greatly increased the surface area of the liquid phase micro solvent, and led to quantitative recoveries of both volatile and semivolatile chemicals within short extraction time of only 2 min. Recoveries of polycyclic aromatic hydrocarbons (PAHs), organochlorine pesticides (OCPs) and alkylphenols (APs) determined were 85-107%, and reproducibility was between 2.8% and 8.5%. In particular, the technique shows high sensitivity for semivolatile chemicals which is difficult to achieve in other sample pretreatment techniques such as headspace-liquid phase microextraction. The variables affecting extraction efficiency such as gas flow rate, extraction time, extracting solvent type, temperature of sample and extracting solvent were investigated. Finally, the technique was evaluated to determine PAHs, APs and OCPs from plant and soil samples. The experimental results demonstrated that the technique is economic, sensitive to both volatile and semivolatile chemicals, is fast, simple to operate, and allows quantitative extraction. On-site monitoring of volatile and semivolatile chemicals is now possible using this technique due to the simplification and speed of sample treatment.

  18. A salting out and resin procedure for extracting Schistosoma mansoni DNA from human urine samples

    Directory of Open Access Journals (Sweden)

    Rodrigues Nilton B

    2010-04-01

    Full Text Available Abstract Background In this paper a simple and cheap salting out and resin (InstaGene matrix® resin - BioRad DNA extraction method from urine for PCR assays is introduced. The DNA of the fluke Schistosoma mansoni was chosen as the target since schistosomiasis lacks a suitable diagnostic tool which is sensitive enough to detect low worm burden. It is well known that the PCR technique provides high sensitivity and specificity in detecting parasite DNA. Therefore it is of paramount importance to take advantage of its excellent performance by providing a simple to handle and reliable DNA extraction procedure, which permits the diagnosis of the disease in easily obtainable urine samples. Findings The description of the extraction procedure is given. This extraction procedure was tested for reproducibility and efficiency in artificially contaminated human urine samples. The reproducibility reached 100%, showing positive results in 5 assay repetitions of 5 tested samples each containing 20 ng DNA/5 ml. The efficiency of the extraction procedure was also evaluated in a serial dilution of the original 20 ng DNA/5 ml sample. Detectable DNA was extracted when it was at a concentration of 1.28 pg DNA/mL, revealing the high efficiency of this procedure. Conclusions This methodology represents a promising tool for schistosomiasis diagnosis utilizing a bio-molecular technique in urine samples which is now ready to be tested under field conditions and may be applicable to the diagnosis of other parasitic diseases.

  19. Preparation of extractive resins for producing terbium-161; Preparacion de resinas extractivas para produccion de terbio-161

    Energy Technology Data Exchange (ETDEWEB)

    De la Cruz B, C. C.; Monroy G, F. [ININ, Carretera Mexico-Toluca s/n, 52750 Ocoyoacac, Estado de Mexico (Mexico)], e-mail: fabiola.monroy@inin.gob.mx

    2009-10-15

    This paper presents the development of a methodology for extractive resins preparation to base of HDEHP, which allows to separation of Tb from Gd generating an own technology of preparation of these resins. The study included the extractive resins preparation from 6 different supports: kieselguhr Dg, alumina, red volcanic rock, chiluca, quarry and fluorite; two treatment types of of supports and varied concentrations of HDEHP extractant (di(2-etil hexyl) orthophosphoric acid), in order to determine which resin has improved efficiency of Gd and Tb separation, and radionuclide purity of {sup 161}Tb. Resins were prepared to base of kieselguhr to determine the most appropriate silicon deposition process. Two silicon deposition treatments were realized: treatment I , by contact with silicon deposition solution (dimethyldichlorosilane / heptane 1:30) and treatment II by contact with vapors of dimethyldichlorosilane in vacuum. The extractant retention was carried out to different concentrations of HDEHP / acetone: 1:4, 1:8, 1:15, 1:20, 1:30 and 1:40. According to the results, there is not direct relation of HDEHP concentration used in extractive resins preparation to base of kieselguhr over the efficiency of Gd and Tb separation and of radionuclide purity of {sup 161}Tb. The effect of support in the efficiency of Gd and Tb separation was studied to prepare resins with the supports kieselguhr, alumina, quarry, chiluca, volcanic rock and fluorite, using the silicon deposition treatment II for the supports and a concentration of HDEHP / acetone 1:20, for extractant retention. Only resins based on kieselguhr could separate to Gd from Tb quantitatively, the resin at a concentration of HDEHP / Acetone 1:20 was the best results obtained in Gd and Tb separation, achieving a separation efficiency greater than 90% and a radionuclide purity higher than 99%. (Author)

  20. Experiments on decolourization with 122-resin for extraction of gibberellins from solid medium under different conditions

    Institute of Scientific and Technical Information of China (English)

    WUHong-sheng; FANJia-qing; SHIGuang-hui; ZHAONan-hai

    2004-01-01

    The extracting liquid of gibberellins (Gibberella fujikurol) from solid medium for was decolorized separately with 75%,95% alcohol, and distilled water in static adsorption and vibrating way for different durations. The results showed that the content of GA3 in efflux extracted with alcohol is 10% higher than that with distilled water. With the increase of the durations of extraction,the content of GA3 increases and the dissolution of pigments also increase. For extraction of GA3 cultured in solid medium, the best decolorizing result was obtained when it was extracted with 75%-95% alcohol in static way for 1-3 h, or in a vibrating way for 30-60 min, and then to decolor in a static way for 30-60 min in 122 resin column.

  1. The extraction and chromatographic determination of the essentials oils from Ocimum basilicum L. by different techniques

    Energy Technology Data Exchange (ETDEWEB)

    Soran, Maria Loredana; Varodi, Codruta; Lung, Ildiko; Surducan, Emanoil; Surducan, Vasile [National Institute for Research and Development of Isotopic and Molecular Technologies, 65-103 Donath, 400293 Cluj-Napoca (Romania); Cobzac, Simona Codruta, E-mail: loredana.soran@itim-cj.r [Babes-Bolyai University, Faculty of Chemistry and Chemical Engineering, 11 Arany Janos, 400028 Cluj-Napoca (Romania)

    2009-08-01

    Three different techniques (maceration, sonication and extraction in microwave field) were used for extraction of essential oils from Ocimum basilicum L. The extracts were analyzed by TLC/HPTLC technique and the fingerprint informations were obtained. The GC-FID was used to characterized the extraction efficiency and for identify the terpenic bioactive compounds. The most efficient extraction technique was maceration followed by microwave and ultrasound. The best extraction solvent system was ethyl ether + ethanol (1:1, v/v). The main compounds identified in Ocimum basilicum L. extracts were: {alpha} and {beta}-pinene (mixture), limonene, citronellol, and geraniol.

  2. The extraction and chromatographic determination of the essentials oils from Ocimum basilicum L. by different techniques

    Science.gov (United States)

    Loredana Soran, Maria; Codruta Cobzac, Simona; Varodi, Codruta; Lung, Ildiko; Surducan, Emanoil; Surducan, Vasile

    2009-08-01

    Three different techniques (maceration, sonication and extraction in microwave field) were used for extraction of essential oils from Ocimum basilicum L. The extracts were analyzed by TLC/HPTLC technique and the fingerprint informations were obtained. The GC-FID was used to characterized the extraction efficiency and for identify the terpenic bioactive compounds. The most efficient extraction technique was maceration followed by microwave and ultrasound. The best extraction solvent system was ethyl ether + ethanol (1:1, v/v). The main compounds identified in Ocimum basilicum L. extracts were: α and β-pinene (mixture), limonene, citronellol, and geraniol.

  3. THE EXTRACTION OF GOLD FROM CYANIDE SOLUTION BY α—ALKYL SUBSTITUTED PYRIDINE RESIN

    Institute of Scientific and Technical Information of China (English)

    GANWeitang; LIUYouying; 等

    1992-01-01

    In this paper,we have studied the adsorption properties of gold by α-alkyl substituted pyridine resin( BPR) in alkaline solution.The single and dual component kinetic mass transfer process of Au(I),Ag(I) and other metal cyanide ions were also investigated.The results obtained show that the mass transfer rates of the cyanide ions in the resin phase are closely related to the molar ratio and the configuration of metal cyanide ions. The elution kinetics of Au(I) and other cyanide ions by NH4SCN has been investigated systematically.The intraparticle diffusion coefficient and activation energy of Au(I),Ag(I),Ni(I) Fe(Ⅲ) cyanide anions were determined in CI,NO3,OH-type BPR resin at different temperatures.It is found from the experimental results that the mechanism for extracting Au(I),Ag(I) and other metal cyanide anions by BPR resin belongs to ion exchange process.The difference of activation entropy of some metal cyanide anions(ΔS-ΔS-) was evaluated.

  4. Extraction behaviour of Am(III) and Eu(III) from nitric acid medium in TEHDGA-HDEHP impregnated resins

    Energy Technology Data Exchange (ETDEWEB)

    Saipriya, G.; Kumar, T. [Bhabha Atomic Research Centre Facilities, Kalpakkam (India). Kalpakkam Reprocessing Plant; Kumaresan, R.; Nayak, P.K.; Venkatesan, K.A.; Antony, M.P. [Indira Gandhi Center for Atomic Research, Kalpakkam (India). Fuel Chemistry Div.

    2016-07-01

    The extraction behaviour of Am(III) and Eu(III) from nitric acid medium was studied in the solvent impregnated resins containing extractants such as tetra-bis(2-ethylhexyl)diglycolamide (TEHDGA) or bis-(2-ethylhexyl)phosphoric acid (HDEHP) or mixture of TEHDGA+HDEHP. The rate of extraction of Am(III) and Eu(III) from 1 M nitric acid and the effect of various parameters, such as the concentration of nitric acid in aqueous phase and concentration of TEHDGA and HDEHP in resin phase, on the distribution coefficient of Am(III) and Eu(III) was studied. The distribution coefficient of Am(III) and Eu(III) in HDEHP-impregnated resin decreased and that in TEHDGA-impregnated resin increased, with increase in the concentration of nitric acid. However, in (TEHDGA+HDEHP) - impregnated resin, synergic extraction was observed at lower nitric acid concentration and antagonism at higher nitric acid concentration. The mechanism of Am(III) and Eu(III) extraction in the combined resin was investigated by slope analysis method. The extraction of various metal ions present in the fast reactor simulated high-level liquid waste was studied. The separation factor of Am(III) over Eu(III) was studied using citrate-buffered diethylenetriaminepentaacetic acid (DTPA) solution.

  5. Fluorination Chromatographic Resin and Its Application in the Separation of Fructose%改性色谱分离树脂的制备及在果糖分离中应用

    Institute of Scientific and Technical Information of China (English)

    王金明; 刘文飞; 刘宁

    2011-01-01

    通过直接对KRS-1色谱分离树脂进行表面氟化改性,调节氟的加量,使氟原子在树脂骨架上分布,在树脂表层形成橡胶弹性体,试验证明,该氟化改性色谱分离树脂用于果葡糖浆中果糖分离,果糖质量分数及分离度均高于未氟化树脂,力学性能也得到提高,树脂破碎率远低于未氟化树脂.最适宜氟化试验反应条件为:V(N2)∶V(F2)为9∶1,氟气流量为10 mL/min,通氟气时间为2h,做出KRS-1色谱分离树脂吸附性能高,机械性能好,使用寿命长.%In this paper, direct surface fluorination treatment were conducted on chromatographic separation of KRS-1 resin, by adjusting the amount of fluoride added, fluorine atoms distributed in the resin skeleton and formed a rubber elastomer on the surface of resin. The fluorination treated resins were used to separate fructose glucose syrup, and the results showed that fluorination treated chromatography separation resin had a higher fructose concentration and separation when compared with untreated resin. The mechanical properties are improved, and the breakage rate is far lower than the resin without fluorinated. Optimum experimental conditions were obtained; volume ratio of N2 and F2 was 9:1, fluorine gas flow of 10 mL/min, fluorine gas treatment time of 2 h. KRS-1 resin treated under above condition has high-performance in chromatographic separation, good mechanical properties and long service life.

  6. Comparison of various extraction methods for policosanol from rice bran wax and establishment of chromatographic fingerprint of policosanol.

    Science.gov (United States)

    Wang, Mei-Fei; Lian, Hong-Zhen; Mao, Li; Zhou, Jing-Ping; Gong, Hui-Juan; Qian, Bao-Yong; Fang, Yan; Li, Jie

    2007-07-11

    A capillary gas chromatographic (GC) method has been developed for the separation and determination of policosanol components extracted from rice bran wax. A Varian CP-sil 8 CB column was employed, and an oven temperature was programmed. Gas chromatography-mass spectrometry (GC-MS) was used to identify the composition of policosanol. Quantitative analysis was carried out by means of hydrogen flame ionization detector (FID) with dinonyl phthalate (DNP) as internal standard. The results indicated that the extract obtained by dry saponification has the highest contents of octacosanol and triacontanol among extracts by all used extraction methods including dry saponification, saponification in alcohol, saponification in water (neutralized and non-neutralized), and transesterification. Meanwhile, the GC-MS fingerprint of policosanol extracted by dry saponification has been established. Euclidean distance similarity calculation showed remarkable consistency of compositions and contents among 12 batches of policosanol from a rice bran wax variety. This protocol provided a rapid and feasible method for quality control of policosanol products.

  7. Chromatographic and mass spectrometric characterization of essential oils and extracts from Lippia (Verbenaceae) aromatic plants.

    Science.gov (United States)

    Stashenko, Elena E; Martínez, Jairo R; Cala, Mónica P; Durán, Diego C; Caballero, Deyanira

    2013-01-01

    Analytical methodologies based on GC and HPLC were developed for the separation and quantification of carnosic acid, ursolic acid, caffeic acid, p-coumaric acid, rosmarinic acid, apigenin, luteolin, quercetin, kaempferol, naringenin, and pinocembrin. These methods were used to characterize essential oils and extracts obtained by solvent (methanol) and by supercritical fluid (CO(2)) extraction from stems and leaves of Lippia (Verbenaceae family) aromatic plants (Lippia alba, Lippia origanoides, Lippia micromera, Lippia americana, Lippia graveolens, and Lippia citriodora). Supercritical CO(2) extraction isolated solely pinocembrin and narigenin from three L. origanoides chemotypes. Solvent extracts possessed a more varied composition that additionally included apigenin, quercetin, and luteolin. Solvent extraction afforded higher overall flavonoid yields from all species in comparison with supercritical CO(2) extraction. Pinocembrin was determined in L. origanoides extract at a concentration of 30 mg/g of plant material, which is more than ten times higher than the amount at which polyphenols are regularly found in aromatic plant extracts.

  8. Extraction of Tc(VII) and Re(VII) on TRU resin

    Energy Technology Data Exchange (ETDEWEB)

    Guerin, Nicolas; Riopel, Remi; Kramer-Tremblay, Sheila [Canadian Nuclear Laboratories (CNL), Chalk River, ON (Canada). Radiobiology and Health Branch; De Silva, Nimal; Cornett, Jack [Ottawa Univ., ON (Canada). Dept. of Earth and Environmental Sciences; Dai, Xiongxin [China Institute for Radiation Protection, Beijing (China)

    2017-06-01

    TRU resin can be used to rapidly and selectively extract Tc(VII) and Re(VII). The retention capacity curves of Tc(VII) and Re(VII) for HNO{sub 3}, HCl, H{sub 2}SO{sub 4} and H{sub 3}PO{sub 4} solutions were studied and prepared. Tc(VII) and Re(VII) were simultaneously extracted in 2 M H{sub 2}SO{sub 4} and 1.5 M H{sub 3}PO{sub 4} and were effectively separated from Mo(VI) and Ru(III). Tc(VII) and Re(VII) remained strongly bonded to the resin even after washing using a large volume of 2 M H{sub 2}SO{sub 4} at a relatively high flow rate. Also, they were both completely eluted from the resin using 15 mL of near boiling water, an eluent directly compatible for ICP-MS instrument measurements.

  9. Chromatographic evaluation of polymers imprinted with analogs of chloramphenicol and application to selective solid-phase extraction.

    Science.gov (United States)

    Schirmer, Christina; Meisel, Hans

    2009-08-01

    To obtain a highly selective material for the antibiotic chloramphenicol, which has several harmful side effects in humans, different molecularly imprinted polymers (MIPs) were prepared. In order to avoid a major traditional drawback associated with MIPs of residual template bleeding, molecules that are structurally related to chloramphenicol were used as templates for polymer synthesis. Chromatographic evaluation indicated that the employed template imparted a significant influence on the recognition properties of the corresponding polymer. A strong retention of chloramphenicol under nonpolar elution conditions (k = 68.03, IF = 17.72) and under aqueous elution conditions (k = 92.44, IF = 1.35) was achieved. After chromatographic evaluation, the MIP was utilized as the recognition sorbent in a solid-phase extraction to determine chloramphenicol using either an organic or aqueous washing solvent. Recoveries of nearly 100% from the chloramphenicol standard solution and nearly 90% from honey samples spiked with chloramphenicol were attained. Furthermore, the applicability of the MIP for sample cleanup was demonstrated.

  10. Extraction of Carbon Dioxide From Seawater by Ion Exchange Resin. Part 2. Using Strong Base Anion Exchange Resin

    Science.gov (United States)

    2009-09-29

    Figure 1. Table 2 - Resin Properties of Static Experiments Using Amberjet 4400 in OH Form (150 minute contact time). Sample Concentration (Molar...0.271 1 36 17.9 0.0075 150 0.267 134 19.0 Table 4 - Resin Properties of Static Experiments Using Amberjet 4400 in Cl Form (150 minute contact time

  11. Detection of geosmin and 2-methylisoborneol by liquid-liquid extraction-gas chromatograph mass spectrum (LLE-GCMS)and solid phase extraction-gas chromatograph mass spectrum (SPE-GCMS)

    Institute of Scientific and Technical Information of China (English)

    MA Xiaoyan; GAO Naiyun; CHEN Beibei; LI Qingsong; ZHANG Qiaoli; GU Guofen

    2007-01-01

    Two sample preparation methods were introduced and compared in this paper to establish a simple,quick and exact analysis of geosmin and 2-methylisoborneol.LC-18 column was employed in solid phase extraction (SPE),1.0 mL of hexane was adopted in liquid-liquid extraction(LLE),and the extracts were analyzed by gas chromatograph mass spectrum (GCMS) in selected ion mode.Mean recoveries of SPE were low for 2-methylisoborneol (2-MIB)and geosmin (GSM) with values below 50%.For LLE,the recoveries were satisfyingly above 50% for 2-MIB and 80% for GSM.Detection limits of the LLE method were as low as 1.0 ng/L for GSM and 5.0 ng/L for 2-MIB.A year-long investigation on odor chemicals of drinking water in Shanghai demonstrated that in the summer,there was a serious odor problem induced by a high concentration of 2-MIB.The highest concentration of 152.82 ng/L appeared in July in raw water,while GSM flocculation was minimal with concentrations below odor threshold.

  12. Evaluation of extraction procedures for the ion chromatographic determination of arsenic species in plant materials.

    Science.gov (United States)

    Schmidt, A C; Reisser, W; Mattusch, J; Popp, P; Wennrich, R

    2000-08-11

    The determination of arsenic species in plants grown on contaminated sediments and soils is important in order to understand the uptake, transfer and accumulation processes of arsenic. For the separation and detection of arsenic species, hyphenated techniques can be applied successfully in many cases. A lack of investigations exists in the handling (e.g., sampling, pre-treatment and extraction) of redox- and chemically labile arsenic species prior to analysis. This paper presents an application of pressurized liquid extraction (PLE) using water as the solvent for the effective extraction of arsenic species from freshly harvested plants. The method was optimized with respect to extraction time, number of extraction steps and temperature. The thermal stability of the inorganic and organic arsenic species under PLE conditions (60-180 degrees C) was tested. The adaptation of the proposed extraction method to freeze-dried, fine-grained material was limited because of the insufficient reproducibility in some cases.

  13. Rapid Determination of Technetium-99 in Large Volume Seawater Samples Using Sequential Injection Extraction Chromatographic Separation and ICP-MS Measurement

    DEFF Research Database (Denmark)

    Shi, Keliang; Qiao, Jixin; Wu, Wangsuo

    2012-01-01

    acidity (or concentration of H+) of the loading or eluting solution affect the adsorption and desorption of TcO4– on TEVA resin. Decontamination factors of more than 1 × 106 for ruthenium and 5 × 105 for molybdenum are achieved. Chemical yields of technetium in the overall procedure range from 60% to 75......, and measurement of 99Tc by inductively coupled plasma mass spectrometry (ICP-MS). Chromatographic behaviors of technetium, molybdenum, and ruthenium were investigated, and the mechanism of adsorption and elution of TcO4– on a TEVA column using HNO3 was explored. The results show that not only NO3– but also...

  14. Study of behaviour of Biobeds SM No.7 and Amberlite XAD No.7 chromatographic resins containing di-2-ethyl-hexilphosphoric acid in Eu{sup 3+} and Am{sup 3+} extraction and concentration; Estudo do comportamento das resinas cromatograficas bio-beds SM No.7 e amberlite XAD No.7 contendo o acido di-2-etilexilfosforico na extracao e concentracao de Eu{sup 3+} e Am{sup 3+}

    Energy Technology Data Exchange (ETDEWEB)

    Kuada, Terezinha A.; Felinto, Maria Claudia F. Cunha; Yamaura, Mitiko; Lobao, Afonso S.T. [Instituto de Pesquisas Energeticas e Nucleares (IPEN), Sao Paulo, SP (Brazil)

    1996-07-01

    The extraction of Eu(III) and Am (III) in extraction chromatograpy has been investigated on the basis of partition and infrared studies. The stationary phases were DHEPA supported on Biobeads SM7 and Amberlite XAD7 and the mobile phase was nitric acid solutions. The system seems to be very good for extraction of Eu and Am. The results obtained shown that the capacity factor of these columns were 251.95 and 3039.15 for Eu and Am respectively for DEHPA/Amberlite XAD No.7 and 349.69 and 3132.79 for Eu and An respectively for DEHPA/Biobeads SM No.7. (author)

  15. Chemically modified polymeric resins for solid-phase extraction and group separation prior to analysis by liquid or gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Schmidt, L.W.

    1993-07-01

    Polystyrene divinylbenzene was modified by acetyl, sulfonic acid, and quaternary ammonium groups. A resin functionalized with an acetyl group was impregnated in a PTFE membrane and used to extract and concentrate phenolic compounds from aqueous samples. The acetyl group created a surface easily wetted, making it an efficient adsorbent for polar compounds in water. The membrane stabilized the resin bed. Partially sulfonated high surface area resins are used to extract and group separate an aqueous mixture of neutral and basic organics; the bases are adsorbed electrostatically to the sulfonic acid groups, while the neutraons are adsorbed hydrophobically. A two-step elution is then used to separate the two fractions. A partially functionalized anion exchange resin is used to separate organic acids and phenols from neutrals in a similar way. Carboxylic acids are analyzed by HPLC and phenols by GC.

  16. Extraction of antioxidative principles of Achillea biserrata M. Bieb. and chromatographic analyses

    Directory of Open Access Journals (Sweden)

    Gönül SERDAR

    2015-07-01

    Full Text Available In this study, hexane, chloroform and water extracts were prepared by making consecutive extraction of Achillea  biserrata from the family Asteraceae. Volatile oil of the same types was obtained by water distillation that was continued 4 hours in the Clevenger fixture and dried by adding anhydrous sodium sulfate. After GS/MS analysis, volatile oil of the same types was kept at 4 ºC in the refrigerator and dark until the work activity was performed. Volatile oil yield that was obtained from mixture of all dried flower and plant leaves were determined for Achillea biserrata 0.4%(v/w The antioxidant activities of extracts, total phenol, flavonoid, proanthocyanidin and anthocyanin amounts were determined. Two different tests were performed for measurements of antioxidant activities.1 Especially, for the purpose of meeting the general properties of good additives’ free radical cleaning activity was done by DPPH method and the inhibition of oxidation activity was done by with β-carotene method. The 50% inhibition (IC50 values of the water, methanol:water and chloroform extracts were 19.6, 37.9 and 114 μg /mL, respectively ın DPPH test. Besıdes, the nonpolar extracts were active in β-carotene/linoleic acid test system. Total phenolics and total flavonoid contents were highest in the water extract possessing 3.39% and 1.12%, respectively. Methanolic extract showed the presence of antioxidant phenolic compounds such as protocatecuic acid (177.83 g/g and chlorogenic acid (164.78 g/g ın HPLC analsıs. Automated extraction system obtained better separation of the active principles from plant tissues than conventional extraction procedures.

  17. EXTRACTION-CHROMATOGRAPHIC DETERMINATION OF GLUCOSE AND FRUCTOSE IN THE PRESENCE OF AROMATIC AMINO ACIDS

    Directory of Open Access Journals (Sweden)

    Y. I. Korenman

    2012-01-01

    Full Text Available The extraction of glucose and fructose from aqueous salt solutions containing aromatic amino acids (phenylalanine, tryptophan, tyrosine, hydrophilic solvents (aliphatic alcohols, alkyl acetates, ketones have been studied. The quantitative characteric of the process (the distribution coefficients, the degree of extraction, separation factors are calculeted. The dependence of distribution ratios of monosaccharides from the amino acid content in the solution has been established. A mobile phase for analysis of the concentrate by ascending thin layer chromatography have been developed.

  18. Ethanol extract and chromatographic fractions of Tamarindus indica stem bark inhibits Newcastle disease virus replication.

    Science.gov (United States)

    Okoh, Omobola O; Obiiyeke, Grace E; Nwodo, Uchechukwu U; Okoh, Anthony I

    2017-12-01

    The plethora of ethnomedicinal applications of Tamarindus indica Linn. (Leguminosae), tamarind, includes treatment of human and livestock ailments; preparations are recognized antipyretics in fevers, laxatives and carminatives. African folklore has various applications of tamarind. However, in Nyasaland, domestic fowl are fed with preparations for prophylactic properties. The objective of this study is to evaluate the antiviral properties of T. indica extract. Tamarindus indica stem bark was extracted through ethanol maceration over 24 h, and the crude extract was fractionated by gravity-propelled column chromatography. Newcastle disease virus (NDV) inhibitory activity of extract and fractions were evaluated in vivo using 10-d-old embryonated chicken egg (ECE) as the medium for virus cultivation and antivirus assay. About 240 ECE were grouped into eight (three controls and five experimental) and, 200 μL of the extract and fractions respectively inoculated into NDV pre-infected eggs and incubated at 37 °C. Allantoic fluid was harvested 5 d post-virus infection and assayed for haemagglutination (HA). Anti-NDV assessment showed 62.5 mg/mL of crude extract and fractions: TiA, TiC and TiD to yield a HA titre of 1:128 each, while TiB showed 1:64 HA titre. At 125 mg/mL, a titre of 1:16 was recorded against TiB and TiD and, 1:8 against TiA. Similarly, crude extract and TiC, each recorded 1:4 HA titre. However, the minimum concentrations of extract and fraction for virus inactivation were 0.24 mg/mL and 0.49 mg/mL, respectively. The antiviral activity shown by T. indica portends novel antiviral drugs and, perhaps, as scaffold for new drugs.

  19. Extraction of ranitidine and nizatidine with using imidazolium ionic liquids prior spectrophotometric and chromatographic detection.

    Science.gov (United States)

    Kiszkiel, Ilona; Starczewska, Barbara; Leśniewska, Barbara; Późniak, Patrycja

    2015-03-15

    A new extraction medium was proposed for liquid-liquid extraction of the histamine H2 receptor antagonists ranitidine (RNT) and nizatidine (NZT). The ionic liquids with low vapor pressure and favorable solvating properties for a range of compounds such as 1-butyl-3-methylimidazolium hexafluorophosphate [C4mim][PF6] and 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide [C4mim][Tf2N] were tested for isolation of analytes. The extraction parameters of RNT and NZT, namely, amount of ionic liquid, pH of sample solution, shaking and centrifugation time were optimized. The isolation processes were performed with 1 mL of the ionic liquids. The extracted samples (pH values near 4) were shaken at 1750 rpm. The influence of interfering substances on the efficiency of extraction process was also studied. Methods for the histamine H2 receptor antagonists (ranitidine and nizatidine) determination after their separation using imidazolium ionic liquids by high performance liquid chromatography (HPLC) combined with UV spectrophotometry were developed. The application of ionic liquids in extraction step allows for selective isolation of analytes from aqueous matrices and their preconcentration. The above methods were applied to the determination of RNT and NZT in environmental samples (river water and wastewater after treatment).

  20. Decoding glycome of Astragalus membranaceus based on pressurized liquid extraction, microwave-assisted hydrolysis and chromatographic analysis.

    Science.gov (United States)

    Lv, G P; Hu, D J; Cheong, K L; Li, Z Y; Qing, X M; Zhao, J; Li, S P

    2015-08-28

    Carbohydrates in herbs are a relatively untapped source of new drugs and health beneficial ingredients. Their analysis has been developed as a novel aspect in quality control and herbal glycomics. In this study, glycome of Astragalus membranaceus was decoded based on optimized pressurized liquid extraction (PLE), microwave-assisted acidic hydrolysis (MAAH) and comprehensive chromatographic approaches. Twelve saccharides including sucrose, galacturonic acid, mannitol, fructose, rhamnose, ribose, arabinose, fucose, xylose, mannose, glucose and galactose were quantitatively analyzed by GC-MS and HPLC-CAD (charged aerosol detectors). Different columns, including Prevail Carbohydrate ES, XBridge Amide and CARBOSep CHO-820 CA for HPLC-CAD analysis, were compared for evaluation of oligosaccharides. The polysaccharides in water extract of Astragalus membranaceus were characterized by high performance size exclusive chromatography (HPSEC) combined with multiple angle light scattering detection (MALSD) and refractive index detection (RID). The results showed that A. membranaceus contained more than 108.5mgg(-1) free sucrose and small amounts of glucose 9.6-26.0mgg(-1) and fructose 8.7-22.9mgg(-1). While its polymeric carbohydrates were composed of glucose 71.0-162.3mgg(-1), galacturonic acid 52.0-113.4mgg(-1), arabinose 22.8-54.4mgg(-1) and small amounts of galactose, rhamnose, xylose and mannose. CARBOSep CHO-820 CA showed its potential in simultaneously analyzing oligosaccharides and uronic acid, especially only the environment-friendly water mobile phase was used. HPSEC-MALSD-RID showed that there were three different molecular weight distributions of polysaccharides in A. membranaceus and the average molecular weight were 21901.1, 2038.5, and 353.4kDa. Hierarchical clustering analysis and principal component analysis demonstrated that A. membranaceus from different regions showed variations both in free and polymeric carbohydrates, which indicated that carbohydrates

  1. Chromatographic Evaluation and Characterization of Components of Gentian Root Extract Used as Food Additives.

    Science.gov (United States)

    Amakura, Yoshiaki; Yoshimura, Morio; Morimoto, Sara; Yoshida, Takashi; Tada, Atsuko; Ito, Yusai; Yamazaki, Takeshi; Sugimoto, Naoki; Akiyama, Hiroshi

    2016-01-01

    Gentian root extract is used as a bitter food additive in Japan. We investigated the constituents of this extract to acquire the chemical data needed for standardized specifications. Fourteen known compounds were isolated in addition to a mixture of gentisin and isogentisin: anofinic acid, 2-methoxyanofinic acid, furan-2-carboxylic acid, 5-hydroxymethyl-2-furfural, 2,3-dihydroxybenzoic acid, isovitexin, gentiopicroside, loganic acid, sweroside, vanillic acid, gentisin 7-O-primeveroside, isogentisin 3-O-primeveroside, 6'-O-glucosylgentiopicroside, and swertiajaposide D. Moreover, a new compound, loganic acid 7-(2'-hydroxy-3'-O-β-D-glucopyranosyl)benzoate (1), was also isolated. HPLC was used to analyze gentiopicroside and amarogentin, defined as the main constituents of gentian root extract in the List of Existing Food Additives in Japan.

  2. A tool to evaluate correspondence between extraction ion chromatographic peaks and peptide-spectrum matches in shotgun proteomics experiments.

    Science.gov (United States)

    Ruse, Cristian I; Peacock, Samantha; Ghiban, Cornel; Rivera, Keith; Pappin, Darryl J; Leopold, Peter

    2013-08-01

    Chromatographed peptide signals form the basis of further data processing that eventually results in functional information derived from data-dependent bottom-up proteomics assays. We seek to rank LC/MS parent ions by the quality of their extracted ion chromatograms. Ranked extracted ion chromatograms act as an intuitive physical/chemical preselection filter to improve the quality of MS/MS fragment scans submitted for database search. We identify more than 4900 proteins when considering detector shifts of less than 7 ppm. High quality parent ions for which the database search yields no hits become candidates for subsequent unrestricted analysis for PTMs. Following this rational approach, we prioritize identification of more than 5000 spectrum matches from modified peptides and confirmed the presence of acetylaldehyde-modified His/Lys. We present a logical workflow that scores data-dependent selected ion chromatograms and leverage information about semianalytical LC/LC dimension prior to MS. Our method can be successfully used to identify unexpected modifications in peptides with excellent chromatography characteristics, independent of fragmentation pattern and activation methods. We illustrate analysis of ion chromatograms detected in two different modes by RF linear ion trap and electrostatic field orbitrap.

  3. Novel polymeric resin for solid phase extraction and determination of lead in waters

    Energy Technology Data Exchange (ETDEWEB)

    Karaaslan, Nagihan M.; Cengiz, Emine; Yaman, Mehmet [Science Faculty, Department of Chemistry, Firat University, Elazig (Turkey); Senkal, B. Filiz [Science and Arts Faculty, Department of Chemistry, Istanbul Technical University, Istanbul (Turkey)

    2010-11-15

    Interest in preconcentration techniques for the determination of metals at ultratrace levels still continues increasingly because of some disadvantages of flameless atomic absorption spectrometry and the high costs of other sensitive methods in compared to flame atomic absorption spectrometry (FAAS). Among preconcentration techniques, solid-phase extraction is the most popular because of a number of advantages. In this work, thiol-containing sulfonamide resin was synthesized, characterized, and applied as a new sorption material for solid phase extraction and determination of lead in natural water samples. The optimization of experimental conditions was performed using the parameters including pH, contact time, and volumes of initial and elution solutions. After preconcentration procedure, FAAS was used for determinations. The synthesized resin exhibits the superiority in compared to the other adsorption reagents because of the fact that there is no necessity of any complexing reagent as well as high sorption capacity. Consequently, 280-fold improvement in the sensitivity of analytical scheme was achieved by combining the slotted tube atom trap-atomic absorption spectrometry (STAT-FAAS) and the developed preconcentration method. The limit of detection was found to be 0.15 ng mL{sup -1}. The Pb{sup 2+} concentrations in the studied water samples were found to be in the range of 0.9-6.7 ng mL{sup -1}. (Copyright copyright 2010 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  4. A method for analyzing the δ18O of resin-extractable soil inorganic phosphate.

    Science.gov (United States)

    Weiner, Tal; Mazeh, Shunit; Tamburini, Federica; Frossard, Emmanuel; Bernasconi, Stefano M; Chiti, Tommaso; Angert, Alon

    2011-03-15

    Improved tools for tracing phosphate transformations in soils are much needed, and can lead to a better understanding of the terrestrial phosphorus cycle. The oxygen stable isotopes in soil phosphate are still not exploited in this regard. Here we present a method for measuring the oxygen stable isotopes in a fraction of the soil phosphate which is rapidly available to plants, the resin-extractable P. This method is based on extracting available phosphate from the soil with anion-exchange membranes, soil organic matter removal by a resin, purification by precipitation as cerium phosphate, and finally precipitation as silver phosphate. The purified silver phosphate samples are then measured by a high-temperature elemental analyzer (HT-EA) coupled in continuous flow mode to an isotope ratio mass spectrometer. Testing the method with Mediterranean and semi-arid soils showed no artifacts, as well as good reproducibility in the same order as that of the HT-EA analytical uncertainty (0.3‰). Copyright © 2011 John Wiley & Sons, Ltd.

  5. Extraction and preparation of high-aroma and low-caffeine instant green teas by the novel column chromatographic extraction method with gradient elution.

    Science.gov (United States)

    Li, Qing-Rong; Wu, Min; Huang, Rui-Jie; Chen, Ya-Fei; Chen, Chan-Jian; Li, Hui; Ni, He; Li, Hai-Hang

    2017-06-01

    The lack of aroma and natural taste is a critical problem in production and consumption of instant green teas. A method to prepare instant green teas high in-natural-aroma and low-caffeine by the novel column chromatographic extraction with gradient elution is reported. This method simultaneously extracted aroma (or volatile) and non-aroma compounds from green tea. Green tea was loaded into columns with 2.0-fold of petroleum ether (PE): ethanol (8:2). After standing for 3 h until the aroma compounds dissolved, the column was sequentially eluted with 3.0-fold 40% ethanol and 3.5-fold water. The eluant was collected together and automatically separated into PE and ethanol aqueous phases. The aroma extracts was obtained by vacuum-evaporation of PE phase at 45 °C. The ethanol aqueous phase was vacuum-concentrated to aqueous and partially or fully decaffeinated with 4% or 9% charcoal at 70 °C. A regular instant green tea with epigallocatechin-3-gallate: caffeine of 3.5:1 and a low-caffeine instant green tea (less than 1% caffeine) with excellent aroma and taste were prepared, by combining the aroma and non-aroma extracts at a 1:10 ratio. This work provides a practical approach to solve the low-aroma and low-taste problems in the production of high quality instant green teas.

  6. Miniaturized molecularly imprinted polymer extraction method for the gas chromatographic analysis of flavonoids.

    Science.gov (United States)

    Nolvachai, Yada; Kulsing, Chadin; Boysen, Reinhard I; Hearn, Milton T W; Marriott, Philip J

    2014-04-01

    In this study, the use of monolithic molecularly imprinted polymers in a micropipette tip format allowing the simple and fast extraction of flavonoids from standard solutions and a black tea sample is demonstrated. The imprinted polymer employed quercetin, methacrylic acid or 4-vinylpyridine, and ethylene glycol dimethacrylate as template, functional monomer, and cross-linker, respectively. Surface morphologies of the quercetin-imprinted polymers and the corresponding nonimprinted polymers were characterized by SEM. Extraction of flavonoid standards was performed to evaluate the selectivity and recovery with these imprinted and nonimprinted polymers. Flavonoid compositions in aliquots eluted from the tips were identified using fast GC with flame ionization detection. Maximum specific capacities of 0.2, 5.7, and 16.0 mg/g for catechin, morin, and quercetin, respectively, were obtained with the imprinted polymer prepared with methacrylic acid, with the corresponding recoveries of 99.8, 98.8, and 95.4%, respectively. Efficient extraction by the quercetin-imprinted polymer of epicatechin, catechin, and quercetin from an apple-flavored black tea sample was achieved, with GC-MS employed for compound identification for both the tea and extracted samples.

  7. Chromatographic analysis of Polygalae Radix by online hyphenating pressurized liquid extraction

    Science.gov (United States)

    Song, Yuelin; Song, Qingqing; Li, Jun; Shi, Shepo; Guo, Liping; Zhao, Yunfang; Jiang, Yong; Tu, Pengfei

    2016-06-01

    Practicing “green analytical chemistry” is of great importance when profiling the chemical composition of complex matrices. Herein, a novel hybrid analytical platform was developed for direct chemical analysis of complex matrices by online hyphenating pressurized warm water extraction followed by turbulent flow chromatography coupled with high performance liquid chromatography-tandem mass spectrometry (PWWE-TFC-LC-MS/MS). Two parallel hollow guard columns acted as extraction vessels connected to a long narrow polyether ether ketone tube, while warm water served as extraction solvent and was delivered at a flow rate of 2.5 mL/min to generate considerable back pressure at either vessel. A column oven heated both the solvent and crude materials. A TFC column, which is advantageous for the comprehensive trapping of small molecular substances from fluids under turbulent flow conditions, was employed to transfer analytes from the PWWE module to LC-MS/MS. Two electronic valves alternated each vessel between extraction and elution phases. As a proof-of-concept, a famous herbal medicine for the treatment of neurodegenerative disorders, namely Polygalae Radix, was selected for the qualitative and quantitative analyses. The results suggest that the hybrid platform is advantageous in terms of decreasing time, material, and solvent consumption and in its automation, versatility, and environmental friendliness.

  8. Chromatographic separation process with pellicular ion exchange resins that can be used for ion or isotope separation and resins used in this process. Procede de separation chromatographique au moyen de resines echangeuses d'ions pelliculaires, utilisable notamment pour la separation des isotopes ou des ions, et resines utilisables dans ce procede

    Energy Technology Data Exchange (ETDEWEB)

    Carles, M.; Neige, R.; Niemann, C.; Michel, A.; Bert, M.; Bodrero, S.; Guyot, A.

    1989-01-06

    For separation of uranium, boron or nitrogen isotopes, an isotopic exchange is carried out betwen an isotope fixed on an ion exchange resin and another isotope of the same element in the liquid phase contacting the resin. Pellicular resins are used comprising composite particulates with an inert polymeric core and a surface layer with ion exchange groups.

  9. Extraction chromatographic separation of uranium (VI) with amberlite LA-1 from malonic acid

    Energy Technology Data Exchange (ETDEWEB)

    Narayanan, P.; Khopkar, S.M.

    1985-12-01

    Uranium(VI) was extracted between pH 2.5 to 6.0 from 0.01 mol dm/sup -3/ malonic acid on a column of silica gel with Aberlite LA-1 as the extractant. It was stripped from the column with 1-2 mol dm/sup -3/ of hydrochloric, sulfuric, and nitric acids. Uranium(VI) was separated from alkali, alkaline earths, manganese, iron, cobalt, nickel, zinc, yttrium, lanthanum, cerium in binary mixtures by exploiting the difference in the pH of formation of malonato complexes. Uranium was separated from zirconium, hafnium, thorium, scandium, and titanium by taking its advantage of stability of chloro or sulfato complexes. The method was tested for the standard reference rock samples. 15 references, 4 figures, 1 table.

  10. Partial least squares model and design of experiments toward the analysis of the metabolome of Jatropha gossypifolia leaves: Extraction and chromatographic fingerprint optimization.

    Science.gov (United States)

    Pilon, Alan Cesar; Carnevale Neto, Fausto; Freire, Rafael Teixeira; Cardoso, Patrícia; Carneiro, Renato Lajarim; Da Silva Bolzani, Vanderlan; Castro-Gamboa, Ian

    2016-03-01

    A major challenge in metabolomic studies is how to extract and analyze an entire metabolome. So far, no single method was able to clearly complete this task in an efficient and reproducible way. In this work we proposed a sequential strategy for the extraction and chromatographic separation of metabolites from leaves Jatropha gossypifolia using a design of experiments and partial least square model. The effect of 14 different solvents on extraction process was evaluated and an optimized separation condition on liquid chromatography was estimated considering mobile phase composition and analysis time. The initial conditions of extraction using methanol and separation in 30 min between 5 and 100% water/methanol (1:1 v/v) with 0.1% of acetic acid, 20 μL sample volume, 3.0 mL min(-1) flow rate and 25°C column temperature led to 107 chromatographic peaks. After the optimization strategy using i-propanol/chloroform (1:1 v/v) for extraction, linear gradient elution of 60 min between 5 and 100% water/(acetonitrile/methanol 68:32 v/v with 0.1% of acetic acid), 30 μL sample volume, 2.0 mL min(-1) flow rate, and 30°C column temperature, we detected 140 chromatographic peaks, 30.84% more peaks compared to initial method. This is a reliable strategy using a limited number of experiments for metabolomics protocols.

  11. Separation of rare earth by column chromatography using organic resins XAD/DEPHA

    Energy Technology Data Exchange (ETDEWEB)

    Zini, J.; Ferreira, J.C.; Bergamaschi, V.S.; Santos, I.; Carvalho, F.M.S., E-mail: jcferrei@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (CCCH/IPEN/CNEN-SP), Sao Paulo, SP (Brazil). Centro de Celulas a Combustivel e Hidrogenio

    2013-07-01

    The designation of light and heavy rare earth was used the fractionation used in separation processes. In this study the process of separation of rare earth, in groups, by chromatographic column consisting in fixing of cations these elements in an organic resin Amberlite XAD16 functionalized with the extracting agent DEPHA and another portion functionalized with a mixture of extractors DEPHA/TOP. The preparation of these resins was performed in two forms, one directly as the extracting agent to the resin and the other to be used in ethyl alcohol. Conditioned resins were introduced in chromatographic columns in separation of groups, light and heavy, using a standard solution of cerium nitrate and standard solution of holmium nitrate groups to represent light and heavy respectively. The characterization technique used to identify the rare earth elements was Spectrometry X-Ray Fluorescence (XRF). The results using the technique of chromatography were satisfactory, obtaining 100% separation of the elements. (author)

  12. Reversed phase extraction chromatographic separation of scandium with amberlite LA-1 from malonate solutions

    Energy Technology Data Exchange (ETDEWEB)

    Narayanan, P.; Khopkar, S.M.

    1983-01-01

    Scandium was extracted at pH 5.0 from 0.01 M malonic acid on silica gel column impregnated with Amberlite LA-1. Nickel, zinc, cadmium, mercury, lead, tin, aluminium, and lanthanum in binary mixtures passed through the cadmium because they could not form malonato complexes. It was separated by the process of selective elution from elements such as zirconium, thorium, uranium, iron(III), gallium, indium, cerium(III), and titanium by exploiting difference in stability of malonato complexes. Scandium was separated from multicomponent mixture containing yttrium, titanium, zirconium, thorium, uranium and aluminium by a process of selective sorbtion and selective elution.

  13. Reversed phase extraction chromatographic separation of thorium with Amberlite LA-1 from malonate solutions

    Energy Technology Data Exchange (ETDEWEB)

    Narayanan, P.; Khopkar, S.M. (Indian Inst. of Tech., Bombay. Dept. of Chemistry)

    1984-10-01

    Thorium was extracted at pH 5.0 from 0.01M malonic acid on a column of silica gel coated with Amberlite LA-1. Thorium was separated from alkali and alkaline earths, manganese, iron, cobalt, nickel, zinc, tin, in binary mixtures by taking advantage of the pH differences in the formation of malonato complexes. Thorium was separated from zirconium, uranium, scandium, molybdenum, titanium by exploiting the differences in the stability of malonato complexes. The method was extended to the analysis of thorium in monazite.

  14. QbD-oriented development and validation of a bioanalytical method for nevirapine with enhanced liquid-liquid extraction and chromatographic separation.

    Science.gov (United States)

    Beg, Sarwar; Chaudhary, Vandna; Sharma, Gajanand; Garg, Babita; Panda, Sagar Suman; Singh, Bhupinder

    2016-06-01

    The present studies describe the systematic quality by design (QbD)-oriented development and validation of a simple, rapid, sensitive and cost-effective reversed-phase HPLC bioanalytical method for nevirapine in rat plasma. Chromatographic separation was carried out on a C18 column using isocratic 68:9:23% v/v elution of methanol, acetonitrile and water (pH 3, adjusted by orthophosphoric acid) at a flow rate of 1.0 mL/min using UV detection at 230 nm. A Box-Behnken design was applied for chromatographic method optimization taking mobile phase ratio, pH and flow rate as the critical method parameters (CMPs) from screening studies. Peak area, retention time, theoretical plates and peak tailing were measured as the critical analytical attributes (CAAs). Further, the bioanalytical liquid-liquid extraction process was optimized using an optimal design by selecting extraction time, centrifugation speed and temperature as the CMPs for percentage recovery of nevirapine as the CAA. The search for an optimum chromatographic solution was conducted through numerical desirability function. Validation studies performed as per the US Food and Drug Administration requirements revealed results within the acceptance limit. In a nutshell, the studies successfully demonstrate the utility of analytical QbD approach for the rational development of a bioanalytical method with enhanced chromatographic separation and recovery of nevirapine in rat plasma. Copyright © 2015 John Wiley & Sons, Ltd.

  15. SYNTHESES OF RESINS IMPREGNATED WITH POLYETHER OR POLYTHIOETHER OLIGOMERS AND THEIR EXTRACTION FOR GOLD(Ⅲ) and palladium(Ⅱ)

    Institute of Scientific and Technical Information of China (English)

    DONGShihua; LIUShi; 等

    1992-01-01

    Six novel resins impregnated with polyether or polythioether oligomers have been synthesized and their extraction properties have also been investigated.Gold(Ⅲ) and /or palladium (Ⅱ) coulld be extracted repidly by the resins with high percentage and capacities from aqueous solution but most of the co-existing base metal ions were remained.The extraction capacities and stripping percentage were approximately unchanged after four extraction-elution cycles and the resins also showed excellent column extraction-elution properties.

  16. HPTLC profile of aqueous extract of different chromatographic fractions of Aloe barbadensis Miller

    Directory of Open Access Journals (Sweden)

    Nishant Kumar Ojha

    2012-05-01

    Full Text Available Objective: To establish the fingerprint profile of Aloe barbadensis Miller by using High Performance Thin Layer Chromatography (HPTLC technique. Methods: after optimization of solvent system by Thin Layer Chromatography, different fractions of aqueous extract of Aloe was collected by column chromatography and the fingerprinting was done by High Performance Thin Layer Chromatography (HPTLC Results: solvent system of methanol:chloroform :: 1:1 was found appropriate for fractionation by column chromatography. Total seven fractions were collected and they were analysed by HPTLC. Distinct spectra of different constituents were obtained for each fraction. Conclusions: HPTLC fingerprinting of Aloe barbadensis Miller may be useful in characterization of different phytochemicals found in this species. It may also be useful in differentiating the species from the adulterant and act as a biochemical marker for this medicinally important plant in the pharmaceutical industry.

  17. Headspace Solid Phase Micro Extraction Gas Chromatographic Determination of Fenthion in Human Serum

    Directory of Open Access Journals (Sweden)

    Kyriaki Machera

    2008-05-01

    Full Text Available A simple and effective analytical procedure was developed for the determination of fenthion residues in human serum samples. The sample treatment was performed using the headspace solid-phase micro extraction with polyacrylate fiber, which has the advantage to require low amount of serum (1 mL without tedious pre-treatment. The quantification of fenthion was carried out by gas chromatography-mass spectrometry and the recoveries ranged from 79 to 104% at two spiking levels for 6 replicates. Detection and quantification limits were calculated as 1.51 and 4.54 ng/mL of serum respectively. Two fenthion metabolites − fenoxon and fenthion–sulfoxide − were also identified.

  18. Determination of Trace Amount of Polycyclic Aromatic Hydrocarbons in Urban Sewage by Solid-phase Extraction Coupled with High Performance Liquid Chromatograph

    Institute of Scientific and Technical Information of China (English)

    2011-01-01

    [Method] This study aimed to determine trace amount of polycyclic aromatic hydrocarbons(PAHs) in urban sewage by using solid-phase extraction(SPE) coupled with high performance liquid chromatograph(HPLC).[Method] From the aspects of solid-phase extraction column,elution solvent,elution volume,elution speed and so forth,the test conditions of SPE-HPLC method were optimized,and trace amount of PAHs in urban sewage was determined.[Result] The optimized solid-phase extraction conditions were SUPELCLEAN LC-18 so...

  19. Flow system for optical activity detection of vegetable extracts employing molecular exclusion continuous chromatographic detection

    Science.gov (United States)

    Fajer, V.; Rodríguez, C.; Naranjo, S.; Mesa, G.; Mora, W.; Arista, E.; Cepero, T.; Fernández, H.

    2006-02-01

    The combination of molecular exclusion chromatography and laser polarimetric detection has turned into a carbohydrate separation and quantification system for plant fluids of industrial value, making it possible the evaluation of the quality of sugarcane juices, agave juices and many other plant extracts. Some previous papers described a system where liquid chromatography separation and polarimetric detection using a LASERPOL 101M polarimeter with He-Ne light source allowed the collection and quantification of discrete samples for analytical purposes. In this paper, the authors are introducing a new improved system which accomplishes polarimetric measurements in a continuous flux. Chromatograms of several carbohydrates standard solutions were obtained as useful references to study juice quality of several sugarcane varieties under different physiological conditions. Results by either discrete or continuous flux systems were compared in order to test the validation of the new system. An application of the system to the diagnostics of scalded foliar is described. A computer program allowing the output of the chromatograms to a display on line and the possibility of digital storing, maxima detections, zone integration, and some other possibilities make this system very competitive and self-convincing.

  20. The Effects of Boswellia Resin Extract on Dopaminergic Cell line, SK-N-SH, against MPP+-Induced Neurotoxicity

    Directory of Open Access Journals (Sweden)

    Sareh Kazmi

    2011-10-01

    Full Text Available Introduction: Oxidative stress and neuroinflammation are involved in neurodegeneration procedure in Parkinson’s disease. Recently, neuroprotective potential of Boswellia resin has been demonstrated. Therefore, this study examined whether administration of Boswellia resin would attenuate MPP+- induced neuronal death in SK-N-SH- cell line, a human dopaminergic neurons- in vitro. Methods: Boswellia resin extract was added to culture medium (10μg/ml before and after exposure of SK-N-SH cell line to MPP+ (1000μM. Cell viability and apoptosis features were assessed using MTT and Hoechst staining, respectively. Results: Treatment with Boswellia resin 2 and 3h prior to MPP ° exposure and up to 60 minutes after MPP ° exposure significantly increased cell viability compare to untreated cells. Apoptotic features were also reduced significantly by Boswellia resin (10 μg/ml compare to that of control untreated cells. Discussion: Boswellia resin has neuroprotective effects on dopaminergic neurons which can be applicable in Parkinson’s disease.

  1. EXTRACTION AND SEPARATION OF RADISH RED PIGMENT FROM A WASTE WATER OF SALTING RADISH BY D61 RESIN

    Institute of Scientific and Technical Information of China (English)

    ZhouXiaohua; KangJajie; 等

    1996-01-01

    Extraction and separation of Radish red pigment from a waste water of salting Radish was studied on D61 resin.The exchange capacity of adsorption the pigment was equal to 60.91mg·g-1 wet resin,and the equilibium time only 40mins.All Radish red pigment adsorbed on D61 resin was eluted using a eluent in which concentraction of HCl or alcohol was 0.1mol·L-1 or 80% at 50℃ when the flow rate was at 2BV·hm-1.Stability of D61 resin was very well,and while the resin was recycled fifteen times, the exchange capacity was only decreased 11.9%,and the exchange capacity didn′t changed.Because of negative ion of mustard oil,it could′t be adsorbed on the resin.Finally, a paste product with yield of 1.96mg·100ml-1 waste water was obtained after alcohol evaporation and vacuum drying.

  2. Review: Resin Composite Filling

    OpenAIRE

    Desmond Ng; Jimmy C. M. Hsiao; Keith C. T. Tong; Harry Kim; Yanjie Mai; Keith H. S. Chan

    2010-01-01

    The leading cause of oral pain and tooth loss is from caries and their treatment include restoration using amalgam, resin, porcelain and gold, endodontic therapy and extraction. Resin composite restorations have grown popular over the last half a century because it can take shades more similar to enamel. Here, we discuss the history and use of resin, comparison between amalgam and resin, clinical procedures involved and finishing and polishing techniques for resin restoration. Although resin ...

  3. Meta-analysis of dragon’s blood resin extract as radio-protective agent

    Directory of Open Access Journals (Sweden)

    Subaika Mahmood

    2017-09-01

    Full Text Available In health sciences, much efforts had been made in past years to explore the radio-protective agents from natural resources due to rapid exposure of radiations to environment such as space traveling, radiotherapy and largely growing telecommunication industry. It becomes crucial to find natural sources for radio-protection. In correspondence, dragon’s blood (DB is a traditional Chinese medicinal plant that possesses great medicinal values due to the presence of several phenolic compounds. For a long time, DB has been used in treatment of blood stasis, inflammation, oxidative stress, immune suppression and tumors, but recently it has been extensively used as radio-protective agent. There is no comprehensive review on radio- protective characterization of DB resin extract in literature. In our review, an attempt has been made to highlight unique and inherent radio-protection in liver, brain, kidney, lung, spleen and cerebrum. This review will help people in exploring the radioactive protectants from natural resources.

  4. Effect of grape seed extract against biodegradation of composite resin-dentin shear bond strength

    Science.gov (United States)

    Generosa, D. M.; Suprastiwi, E.; Asrianti, D.

    2017-08-01

    This study aimed to analyze the effect of grape seed extract (GSE) on resin-dentin shear bond strength. A group of 48 dentin samples were divided into 6 groups. The six groups, each with eight specimens, included group 1 (control), group 2 (control + NaOCl 10%), group 3 (2.9% GSE application before etching), group 4 (2.9% GSE application before etching + NaOCl 10%), group 5 (2.9% GSE application after etching), and group 6 (2.9% GSE application after etching + NaOCl 10%). Shear bond strengths were measured using a universal testing machine. Statistical analysis was done with the Kruskal-Wallis test and the Mann-Whitney U test. The highest median value was in group 3, and the lowest value was in group 5. GSE can improve the shear bond strength (p = 0.002 and 0.001), but it has no effect on reducing biodegradation (p = 0.141).

  5. Two novel extraction chromatography resins containing multiple diglycolamide-functionalized ligands: preparations, characterization and actinide uptake properties

    NARCIS (Netherlands)

    Ansari, S.A.; Mohapatra, P.K.; Iqbal, M.; Huskens, Jurriaan; Verboom, Willem

    2014-01-01

    Two extraction chromatography resins were prepared for the first time by impregnating multiple diglycolamide-functionalized ligands such as diglycolamide-calix[4]arene (C4DGA) and tripodal diglycolamide (T-DGA) on Chromosorb-W, an inert solid support, for the removal of hazardous actinides like Am(I

  6. One-step column chromatographic extraction with gradient elution followed by automatic separation of volatiles, flavonoids and polysaccharides from Citrus grandis.

    Science.gov (United States)

    Han, Han-Bing; Li, Hui; Hao, Rui-Lin; Chen, Ya-Fei; Ni, He; Li, Hai-Hang

    2014-02-15

    Citrus grandis Tomentosa is widely used in traditional Chinese medicine and health foods. Its functional components include volatiles, flavonoids and polysaccharides which cannot be effectively extracted through traditional methods. A column chromatographic extraction with gradient elution was developed for one-step extraction of all bioactive substances from C. grandis. Dried material was loaded into a column with petroleum ether: ethanol (8:2, PE) and sequentially eluted with 2-fold PE, 3-fold ethanol: water (6:4) and 8-fold water. The elutes was separated into an ether fraction containing volatiles and an ethanol-water fraction containing flavonoids and polysaccharides. The later was separated into flavonoids and polysaccharides by 80% ethanol precipitation of polysaccharides. Through this procedure, volatiles, flavonoids and polysaccharides in C. grandis were simultaneously extracted at 98% extraction rates and simply separated at higher than 95% recovery rates. The method provides a simple and high-efficient extraction and separation of wide range bioactive substances.

  7. Recent Development Prospect of Adsorbing and Extracting Gold with Extraction Resins%萃取树脂吸萃金研究进展

    Institute of Scientific and Technical Information of China (English)

    李海梅; 高学珍; 袁延旭; 刘军深

    2011-01-01

    Extraction resins are participate adsorbers which are based on the incorporation of extractants into porous carriers such as polymer supports by physical adsorption. They possess a combination of the advantageous features of both liquid - liquid extraction and ion exchange. This paper reviews the current situation and prospect of adsorbing and extracting gold with extraction resins process according to the types of extraction resins. The mechanism of sorption is basically similar to the case of solvent extraction. The effective separation of gold can be obtained under properly - controlled conditions. This technology will open up a new approach for the separation of gold.%萃取树脂是通过物理方式将萃取剂固定于某种适宜的多孔载体(如聚合物)上的吸附剂.它具有液液萃取和离子交换的优点.文章按萃取树脂的类型对其吸萃金的研究现状进行了综述.萃取树脂吸萃金离子的机理与溶剂萃取法相似,控制合适的条件可以实现金的有效分离.预计萃取树脂技术将为金分离开拓一条新途径.

  8. A review on solid phase extraction of actinides and lanthanides with amide based extractants.

    Science.gov (United States)

    Ansari, Seraj A; Mohapatra, Prasanta K

    2017-05-26

    Solid phase extraction is gaining attention from separation scientists due to its high chromatographic utility. Though both grafted and impregnated forms of solid phase extraction resins are popular, the later is easy to make by impregnating a given organic extractant on to an inert solid support. Solid phase extraction on an impregnated support, also known as extraction chromatography, combines the advantages of liquid-liquid extraction and the ion exchange chromatography methods. On the flip side, the impregnated extraction chromatographic resins are less stable against leaching out of the organic extractant from the pores of the support material. Grafted resins, on the other hand, have a higher stability, which allows their prolong use. The goal of this article is a brief literature review on reported actinide and lanthanide separation methods based on solid phase extractants of both the types, i.e., (i) ligand impregnation on the solid support or (ii) ligand functionalized polymers (chemically bonded resins). Though the literature survey reveals an enormous volume of studies on the extraction chromatographic separation of actinides and lanthanides using several extractants, the focus of the present article is limited to the work carried out with amide based ligands, viz. monoamides, diamides and diglycolamides. The emphasis will be on reported applied experimental results rather than on data pertaining fundamental metal complexation. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Effects of Balsamodendron mukul Gum Resin Extract on Articular Cartilage in Papain-induced Osteoarthritis.

    Science.gov (United States)

    Manjhi, Jayanand; Gupta, Maneesh; Sinha, Anvesha; Rawat, Beena; Rai, Durg V

    2016-07-01

    Context • Osteoarthritis (OA) is one of the most prevalent chronic diseases of the musculoskeleton, causing functional disability among older adults. Management of OA includes conventional pharmacological treatments consisting primarily of nonsteroidal anti-inflammatory drugs (NSAIDs), acetaminophen, physiotherapy, and surgical procedures. The medications are not ideal therapeutic agents; NSAIDs in particular can cause serious side effects. Objective • The study was conducted to investigate the effects of Balsamodendron mukul (BDM) gum resin extract on cartilage damage and microstructural changes in the subchondral bone of rats with papain-induced, osteoarthritic knee joints. Design • The authors designed a parallel randomized, controlled study to examine the effects of 3 concentrations of BDM on OA in a murine model. Setting • The present study was undertaken at the research laboratory, Faculty of Biological Engineering, Shobhit University (Modipuram, Meerut, India). Intervention • OA was induced by intra-articular injections of 0.2 mL of 4% papain solution and 0.1 mL of 0.03 M cysteine through the patellar ligament using a 26-gauge, 1.27-cm needle. The rats in the sham group received same volume of isotonic sodium chloride solution. The rats were divided into 6 groups : (1) control group-fresh rats, with ages and genders similar to those of the other groups but with no induction of OA and no treatments; (2) sham group-rats receiving a sham induction of OA using an intra-articular injection of saline of the same volume as the papain given to all OA rats but no treatments; (3) OA group-rats induced with OA but receiving no treatments; (4) OA + BDM (10%) group-rats induced with OA that received a 10% dose of BDM; (5) OA + BDM (20%) group-rats induced with OA that received a 20% dose of BDM; and (6) OA + BDM (40%) group-rats induced with OA that received a 40% dose of BDM. Rats in the treatment groups were fed their respective doses of BDM extract for 30 d

  10. Two solid-phase recycling method for basic ionic liquid [C4mim]Ac by macroporous resin and ion exchange resin from Schisandra chinensis fruits extract.

    Science.gov (United States)

    Ma, Chun-hui; Zu, Yuan-gang; Yang, Lei; Li, Jian

    2015-01-22

    In this study, two solid-phase recycling method for basic ionic liquid (IL) 1-butyl-3-methylimidazolium acetate ([C4mim]Ac) were studied through a digestion extraction system of extracting biphenyl cyclooctene lignans from Schisandra chinensis. The RP-HPLC detection method for [C4mim]Ac was established in order to investigate the recovery efficiency of IL. The recycling method of [C4mim]Ac is divided into two steps, the first step was the separation of lignans from the IL solution containing HPD 5000 macroporous resin, the recovery efficiency and purity of [C4mim]Ac achieved were 97.8% and 67.7%, respectively. This method cannot only separate the lignans from [C4mim]Ac solution, also improve the purity of lignans, the absorption rate of lignans in [C4mim]Ac solution was found to be higher (69.2%) than that in ethanol solution (57.7%). The second step was the purification of [C4mim]Ac by the SK1B strong acid ion exchange resin, an [C4mim]Ac recovery efficiency of 55.9% and the purity higher than 90% were achieved. Additionally, [C4mim]Ac as solvent extraction of lignans from S. chinensis was optimized, the hydrolysis temperature was 90°C and the hydrolysis time was 2h.

  11. Determination of copper, lead and iron in water and food samples after column solid phase extraction using 1-phenylthiosemicarbazide on Dowex Optipore L-493 resin.

    Science.gov (United States)

    Yildiz, Ozden; Citak, Demirhan; Tuzen, Mustafa; Soylak, Mustafa

    2011-02-01

    A novel solid phase extraction procedure for determination of copper, lead and iron in natural water and food samples has been established in the presented work. 1-Phenylthiosemicarbazide (1-PTSC) as ligand and Dowex Optipore L-493 resin as adsorbent were used in a mini chromatographic column. Various analytical conditions for the quantitative recoveries of analyte ions including pH, amounts of adsorbent, eluent, sample volume, etc. were investigated. The recovery values for analyte ions were higher than 95%. The determination of copper, lead and iron was performed by flame atomic absorption spectrometry. The influences of some alkali, alkali earth and transition metals on the recoveries of analyte ions were investigated. The preconcentration factor was 62.5. The limit of detections of the understudied analytes (k=3, N=21) were 0.64 μg L(-1) for copper, 0.55 μg L(-1) for lead and 0.82 μg L(-1) for iron. The relative standard deviation was found to be lower than 6%. The accuracy of the method was confirmed with certified reference material (GBW 07605 Tea). The method was successively applied for the determination of copper, lead and iron in water and some food samples including cheese, bread, baby food, pekmez, honey, milk and red wine after microwave digestion.

  12. Releasing Pattern of Applied Phosphorus and Distribution Change of Phosphorus Fractions in the Acid Upland Soils with Successive Resin Extraction

    Directory of Open Access Journals (Sweden)

    Arief Hartono

    2008-05-01

    Full Text Available The releasing pattern of applied P in the acid upland soils and the soil properties influencing the pattern were studied. Surface horizons of six acid upland soils from Sumatra, Java and Kalimantan were used in this study. The releasing pattern of applied P (300 mg P kg-1 of these soils were studied by successive resin extraction. P fractionation was conducted to evaluate which fractions released P to the soil solution after successive resin extraction. The cumulative of resin-Pinorganic (Pi release of soils was fitted to the first order kinetic. Regression analyses using factor scores obtained from the previous principal components analyses was applied to determine soil properties influencing P releasing pattern. The results suggested that the maximum P release was significantly (P < 0.05 increased by acidity plus 1.4 nm mineral-related factor (PC2 i.e. exchangeable Al and 1.4 nm minerals (smectite and vermiculite and decreased by oxide related factor (PC1 i.e. aluminum (Al plus 1/2 iron (Fe (by ammonium oxalate, crystalline Al and Fe oxides, cation exchange capacity, and clay content. P fractionation analysis after successive resin extraction showed that both labile and less labile in the form of NaHCO3-Pi and NaOH-Pi fractions, respectively, can be transformed into resin-Pi when in the most labile resin-Pi is depleted. Most of P released in high oxides soils were from NaOH-Pi fraction while in low oxides soils were from NaHCO3-Pi. P release from the former fraction resulted in the maximum P release lower than that of the latter one. When NaHCO3-Pi was high, NaOH-Pi was relatively more stable than NaHCO3-Pi despite resin-Pi removal. NaHCO3-Pi and NaOH-Pi are very important P fractions in replenishing resin-Pi in these acid upland soils.

  13. Development of Chromatographic Fingerprints of Eurycoma longifolia (Tongkat Ali) Roots Using Online Solid Phase Extraction-Liquid Chromatography (SPE-LC).

    Science.gov (United States)

    Zaini, Nor Nasriah; Osman, Rozita; Juahir, Hafizan; Saim, Norashikin

    2016-04-30

    E. longifolia is attracting interest due to its pharmacological properties and pro-vitality effects. In this study, an online SPE-LC approach using polystyrene divinyl benzene (PSDVB) and C18 columns was developed in obtaining chromatographic fingerprints of E. longifolia. E. longifolia root samples were extracted using pressurized liquid extraction (PLE) technique prior to online SPE-LC. The effects of mobile phase compositions and column switching time on the chromatographic fingerprint were optimized. Validation of the developed method was studied based on eurycomanone. Linearity was in the range of 5 to 50 µg∙mL(-1) (r² = 0.997) with 3.2% relative standard deviation of peak area. The developed method was used to analyze 14 E. longifolia root samples and 10 products (capsules). Selected chemometric techniques: cluster analysis (CA), discriminant analysis (DA), and principal component analysis (PCA) were applied to the fingerprint datasets of 37 selected peaks to evaluate the ability of the chromatographic fingerprint in classifying quality of E. longifolia. Three groups were obtained using CA. DA yielded 100% correlation coefficient with 19 discriminant compounds. Using PCA, E. longifolia root samples were clearly discriminated from the products. This study showed that the developed online SPE-LC method was able to provide comprehensive evaluation of E. longifolia samples for quality control purposes.

  14. Development of Chromatographic Fingerprints of Eurycoma longifolia (Tongkat Ali Roots Using Online Solid Phase Extraction-Liquid Chromatography (SPE-LC

    Directory of Open Access Journals (Sweden)

    Nor Nasriah Zaini

    2016-04-01

    Full Text Available E. longifolia is attracting interest due to its pharmacological properties and pro-vitality effects. In this study, an online SPE-LC approach using polystyrene divinyl benzene (PSDVB and C18 columns was developed in obtaining chromatographic fingerprints of E. longifolia. E. longifolia root samples were extracted using pressurized liquid extraction (PLE technique prior to online SPE-LC. The effects of mobile phase compositions and column switching time on the chromatographic fingerprint were optimized. Validation of the developed method was studied based on eurycomanone. Linearity was in the range of 5 to 50 µg∙mL−1 (r2 = 0.997 with 3.2% relative standard deviation of peak area. The developed method was used to analyze 14 E. longifolia root samples and 10 products (capsules. Selected chemometric techniques: cluster analysis (CA, discriminant analysis (DA, and principal component analysis (PCA were applied to the fingerprint datasets of 37 selected peaks to evaluate the ability of the chromatographic fingerprint in classifying quality of E. longifolia. Three groups were obtained using CA. DA yielded 100% correlation coefficient with 19 discriminant compounds. Using PCA, E. longifolia root samples were clearly discriminated from the products. This study showed that the developed online SPE-LC method was able to provide comprehensive evaluation of E. longifolia samples for quality control purposes.

  15. Solid phase extractive preconcentration of uranium(VI) using quinoline-8-ol anchored chloromethylated polymeric resin beads.

    Science.gov (United States)

    Praveen, R S; Metilda, P; Daniel, S; Rao, T Prasada

    2005-10-31

    A new chelating polymeric sorbent has been developed using Merrifield chloromethylated resin anchored with quinoline-8-ol (HQ). The modified polymeric resin was characterized by FT-IR spectroscopy and elemental analysis. The HQ anchored resin showed superior binding affinity for U(VI) over Th(IV) and La(III). The influence of various physicochemical parameters on the recovery of U(VI) were optimized by both static and dynamic methods. The phase exchange kinetic studies performed for U(VI) revealed that XAD-16. The developed HQ anchored polymeric resin is highly selective as none of the extraneous species were found to have any deleterious effect. Solid phase extraction (SPE) studies performed using HQ anchored polymeric resin offered enrichment factor of 100 and the lowest concentration below which recoveries become non-quantitative is 5mugl(-1). The accuracy of the developed SPE method in conjunction with Arsenazo III procedure was tested by analyzing marine sediment (MESS-3) and soil (IAEA-Soil 7) reference materials. Furthermore, the above procedure has been successfully employed for the analysis of real soil and sediment samples.

  16. Biobased carbon content of resin extracted from polyethylene composite by carbon-14 concentration measurements using accelerator mass spectrometry.

    Science.gov (United States)

    Taguchi, Kazuhiro; Kunioka, Masao; Funabashi, Masahiro; Ninomiya, Fumi

    2014-01-01

    An estimation procedure for biobased carbon content of polyethylene composite was studied using carbon-14 ((14)C) concentration ratios as measured by accelerated mass spectrometry (AMS). Prior to the measurement, additives and fillers in composites should be removed because they often contain a large amount of biobased carbon and may shift the estimation. Samples of resin with purity suitable for measurement were isolated from composites with a Soxhlet extractor using heated cyclohexanone. After cooling of extraction solutions, the resin was recovered as a fine semi-crystalline precipitate, which was easily filtered. Recovery rates were almost identical (99%), even for low-density polyethylene and linear low-density polyethylene, which may have lower crystallinity. This procedure could provide a suitable approach for estimation of biobased carbon content by AMS on the basis of the standard ASTM D 6866. The biobased carbon content for resin extracted from polyethylene composites allow for the calculation of biosynthetic polymer content, which is an indicator of mass percentage of the biobased plastic resin in the composite.

  17. Comparison in the extraction properties of Pu(IV) in piperidinium and pyrrolidinium nitrate anchored anion exchange resins

    Energy Technology Data Exchange (ETDEWEB)

    Selvan, B. Robert; Suneesh, A.S.; Venkatesan, K.A.; Antony, M.P.; Vasudeva Rao, P.R. [Indira Gandhi Centre for Atomic Research, Kalpakkam (India). Fuel Chemistry Div.

    2016-07-01

    Piperidinium nitrate (Pip-NO{sub 3}) and pyrrolidinium nitrate (Pyr-NO{sub 3}) functional groups were anchored on a poly(styrene-divinylbenzene) matrix and evaluated the resultant anion exchange resin for the extraction of plutonium from nitric acid medium. The distribution coefficient (K{sub d}, mL/g) of Pu(IV) in these resins increased with the concentration of nitric acid, reaching a maximum K{sub d} at 7 M nitric acid, followed by decrease. The extraction of Pu(IV) increased with the duration of equilibration followed by the establishment of equilibrium, occurred within four hours of equilibration. The kinetic data were fitted with pseudo-first order and pseudo-second order rate equations. The apparent plutonium exchange capacity was determined to be ∝256 mg/g for Pip-NO{sub 3} resin and 285 mg/g for Pyr-NO{sub 3} resin at 7 M nitric acid. The radiolytic degradation of Pip-NO{sub 3} and Pyr-NO{sub 3} in presence of nitric acid (7 M) was studied upto a dose of 200 KGy and the results are reported in this paper.

  18. Chemometric analysis of chromatographic fingerprints shows potential of Cyclopia maculata (Andrews) Kies for production of standardized extracts with high xanthone content.

    Science.gov (United States)

    Schulze, Alexandra E; de Beer, Dalene; de Villiers, André; Manley, Marena; Joubert, Elizabeth

    2014-10-29

    Cyclopia species are used for the production of honeybush tea and food ingredient extracts associated with many health benefits. A species-specific high-performance liquid chromatography (HPLC) method for Cyclopia maculata, developed and validated, allowed quantification of the major compounds in extracts from "unfermented" and fermented C. maculata. Two xanthones were tentatively identified for the first time in a Cyclopia species, whereas an additional four compounds were tentatively identified for the first time in C. maculata. "Fermentation" (oxidation) decreased the content of all compounds, with the exception of vicenin-2. Similarity analysis of the chromatographic fingerprints of unfermented C. maculata aqueous extracts showed extremely low variation (r ≥ 0.97) between samples. Some differences between wild-harvested and cultivated seedling plants were, however, demonstrated using principal component analysis. Quantitative data of selected compounds confirmed the low level of variation, making this Cyclopia species ideal for the production of standardized food ingredient extracts.

  19. Sensitive high-performance liquid chromatographic quantitation of gabapentin in human serum using liquid-liquid extraction and pre-column derivatization with 9-fluorenylmethyl chloroformate.

    Science.gov (United States)

    Bahrami, Gholamreza; Kiani, Amir

    2006-05-01

    Most of the published methods for analysis of gabapentin, an antiepileptic agent, in human serum are based on the same approach, involving o-phthaldialdehyde derivatization of deproteinized serum samples. The present paper however, describes a new, simple and sensitive high-performance liquid chromatographic method for determination of gabapentin in human serum using liquid-liquid extraction and 9-fluorenylmethyl chloroformate (FMOC-Cl) as pre-column labeling agent. The drug and an internal standard (azithromycin) were extracted from serum by salting-out approach using a mixture of dichloromethane-2 propanol (1:1, v/v) as the extracting solvent. The extracted analytes were subjected to derivatization with FMOC-Cl in the presence of phosphate buffer (pH 7). A mobile phase consisting of methanol-0.05 M sodium phosphate buffer (73/27, v/v; pH of 3.9) containing 1 ml/l triethylamine was eluted and chromatographic separation was performed on a Shimpack CLC-C18 (150 mm x 4.6 mm) column. The standard curve was linear over the range of 0.03-20 microg/ml and limit of quantification was 0.03 microg/ml. The performance of analysis was studied and the validated method showed excellent performance in terms of selectivity, specificity, sensitivity, precision and accuracy. No interferences were found from commonly co-administered antiepileptic agents.

  20. Curcumin and Boswellia serrata gum resin extract inhibit chikungunya and vesicular stomatitis virus infections in vitro.

    Science.gov (United States)

    von Rhein, Christine; Weidner, Tatjana; Henß, Lisa; Martin, Judith; Weber, Christopher; Sliva, Katja; Schnierle, Barbara S

    2016-01-01

    Chikungunya virus (CHIKV) is a mosquito-transmitted alphavirus that causes chikungunya fever and has infected millions of people mainly in developing countries. The associated disease is characterized by rash, high fever, and severe arthritis that can persist for years. CHIKV has adapted to Aedes albopictus, which also inhabits temperate regions including Europe and the United States of America. CHIKV has recently caused large outbreaks in Latin America. No treatment or licensed CHIKV vaccine exists. Traditional medicines are known to have anti-viral effects; therefore, we examined whether curcumin or Boswellia serrata gum resin extract have antiviral activity against CHIKV. Both compounds blocked entry of CHIKV Env-pseudotyped lentiviral vectors and inhibited CHIKV infection in vitro. In addition, vesicular stomatitis virus vector particles and viral infections were also inhibited to the same extent, indicating a broad antiviral activity. Although the bioavailability of these compounds is rather poor, they might be used as a lead structure to develop more effective antiviral drugs or might be used topically to prevent CHIKV spread in the skin after mosquito bites.

  1. Separation of vitexin-4″-O-glucoside and vitexin-2″-O-rhamnoside from hawthorn leaves extracts using macroporous resins.

    Science.gov (United States)

    Li, Hongjuan; Liu, Ying; Jin, Haizhu; Liu, Sujing; Fang, Shengtao; Wang, Chunhua; Xia, Chuanhai

    2015-12-15

    Vitexin-4″-O-glucoside and vitexin-2″-O-rhamnoside are the major flavonoids of hawthorn leaves. In this work, the adsorption and desorption characteristics of vitexin-4″-O-glucoside and vitexin-2″-O-rhamnoside on seven macroporous resins were evaluated. Among the tested resins, the HPD-400 resin showed the best adsorption and desorption capacities. Adsorption isotherms were constructed for the HPD-400 resin and well fitted to Langmuir and Freundlich models. Dynamic adsorption and desorption tests were performed on column packed with the HPD-400 resin to optimize the chromatographic parameters. After one run treatment with the HPD-400 resin, the contents of vitexin-4″-O-glucoside and vitexin-2″-O-rhamnoside in the product were increased 8.44-fold and 8.43-fold from 0.720% and 2.63% to 6.08% and 22.2% with recovery yields of 79.1% and 81.2%, respectively. These results show that the developed method is a promising basis for the large-scale purification of vitexin-4″-O-glucoside and vitexin-2″-O-rhamnoside from hawthorn leaves and other plant materials.

  2. High Throughput Method of Extracting and Counting Strontium-90 in Urine

    Energy Technology Data Exchange (ETDEWEB)

    Shkrob, I. [Argonne National Lab. (ANL), Argonne, IL (United States); Kaminski, M. [Argonne National Lab. (ANL), Argonne, IL (United States); Mertz, C. [Argonne National Lab. (ANL), Argonne, IL (United States); Hawkins, C. [Argonne National Lab. (ANL), Argonne, IL (United States); Dietz, M. [Argonne National Lab. (ANL), Argonne, IL (United States); Tisch, A. [Argonne National Lab. (ANL), Argonne, IL (United States)

    2016-03-01

    A method has been developed for the rapid extraction of Sr-90 from the urine of individuals exposed to radiation in a terrorist attack. The method employs two chromatographic ion-exchange materials: Diphonix resin and Sr resin, both of which are commercially available. The Diphonix resin reduces the alkali ion concentrations below 10 mM, and the Sr resin concentrates and decontaminates strontium-90. Experimental and calculational data are given for a variety of test conditions. On the basis of these results, a flowsheet has been developed for the rapid concentration and extraction of Sr-90 from human urine samples for subsequent beta-counting.

  3. Effects of croton urucurana extracts and crude resin on Anagasta kuehniella (Lepidoptera: Pyralidae

    Directory of Open Access Journals (Sweden)

    Luciana Barboza Silva

    2009-06-01

    Full Text Available Hundreds of plant species have been studied in order to find out the active ingredient responsible for their insecticidal activity against the pests of economic importance. To verify the insecticidal activity in the husk of stem of Croton urucurana Baillon 1864 (Euphorbiaceae against Anagasta kuehniella Zeller 1879 (Lepidoptera: Pyralidae, the methanolic (EMeOH extract, dichloromethane fraction (FDM, ethyl acetate fraction (FAE and crude resin, incorporated into an artificial diet were evaluated. EMeOH (0.5, 1.0 and 2.0% and crude resin (2.0% interfered with neither the weight nor the survival of fourth instar larvae and other analyzed parameters. FDM (2.0% fraction caused mortality of 65%, and the artificial diet containing 2.0, 1.0 and 0.5% FAE caused 100, 55 and 68% mortality respectively when compared with the control, confirming the least efficiency rates of food conversion for FDM(2.0% and FAE(1.0%. The tryptic analysis performed with the midgut fluid of fourth-instar larvae demonstrated that tryptic and chymiotryptic activities for the larvae fed artificial diet containing EMeOH and crude resin were not different.Atualmente centenas de plantas são investigadas para se conhecer os princípios ativos responsáveis pela atividade inseticida contra as diversas pragas de importância econômica. Com o objetivo de verificar a atividade inseticida das cascas do caule de Croton urucurana Baillon 1864 (Euphorbiaceae em relação a Anagasta kuehniella Zeller 1879 (Lepidoptera: Pyralidae, avaliou-se o extrato metanólico (EMeOH, fração diclorometano (FDM, a fração acetato de etila (FAE e a resina in natura, os quais foram adicionados à dieta artificial. O EMeOH (0,5, 1,0 e 20,% e a resina in natura (2,0%, não interferiram no peso, sobrevivência das larvas de 4ª ínstar, bem como nos demais parâmetros analisados. A fração FDM (2,0% causou mortalidade de 65%, e a dieta artificial contendo 2,0, 1,0, e 0,5% de FAE causou 100, 55 e 68% de

  4. Enrichment and Purification of Deoxyschizandrin and γ-Schizandrin from the Extract of Schisandra chinensis Fruit by Macroporous Resins

    Directory of Open Access Journals (Sweden)

    Ying Zhang

    2012-03-01

    Full Text Available In present study, the performance and separation characteristics of 21 macroporous resins for the enrichment and purification of deoxyschizandrin and γ-schizandrin, the two major lignans from Schisandra chinensis extracts, were evaluated. According to our results, HPD5000, which adsorbs by the molecular tiers model, was the best macroporous resin, offering higher adsorption and desorption capacities and higher adsorption speed for deoxyschizandrin and γ-schizandrin than other resins. Columns packed with HPD5000 resin were used to perform dynamic adsorption and desorption tests to optimize the technical parameters of the separation process. The results showed that the best adsorption time is 4 h, the rate of adsorption is 0.85 mL/min (4 BV/h and the rate of desorption is 0.43 mL/min (2 BV/h. After elution with 90% ethanol, the purity of deoxy-schizandrin increased 12.62-fold from 0.37% to 4.67%, the purity of γ-schizandrin increased 15.8-fold from 0.65% to 10.27%, and the recovery rate was more than 80%.

  5. Separation and purification of both tea seed polysaccharide and saponin from camellia cake extract using macroporous resin.

    Science.gov (United States)

    Yang, Pengjie; Zhou, Mingda; Zhou, Chengyun; Wang, Qian; Zhang, Fangfang; Chen, Jian

    2015-02-01

    A novel method to separate and purify tea seed polysaccharide and tea seed saponin from camellia cake extract by macroporous resin was developed. Among four kinds of resins (AB-8, NKA-9, XDA-6, and D4020) tested, AB-8 macroporous resin possessed optimal separating capacity for the two substances and thus was selected for the separation, in which deionized water was used to elute tea seed polysaccharide, 0.25% NaOH solution to remove the undesired pigments, and 90% ethanol to elute tea seed saponin. Further dynamic adsorption/desorption experiments on AB-8 resin-based column chromatography were conducted to obtain the optimal parameters. Under optimal dynamic adsorption and desorption conditions, 18.7 and 11.8% yield of tea seed polysaccharide and tea seed saponin were obtained with purities of 89.2 and 96.0%, respectively. The developed method provides a potential approach for the large-scale production of tea seed polysaccharide and tea seed saponin from camellia cake. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Preparation of extraction resin for radio lanthanides separation; Preparacion de resina de extraccion para separacion de radiolantanidos

    Energy Technology Data Exchange (ETDEWEB)

    Cruz B, C.C. de la; Monroy G, F. [ININ, 52750 La Marquesa, Estado de Mexico (Mexico)]. e-mail: delacruzbc@hotmail.com

    2008-07-01

    The present work presents the methodology that was developed for the preparation of one extractant resin with the aim of HDEHP, to separate radio lanthanides with serial atomic numbers. In this case it is exemplified with the separation of the following elements: Gadolinium-161 and the Terbium-161; this last radioisotope it is a beta emitting ({beta}{sup -}) that has a great potential to be used in therapy, also in nuclear medicine and in oncology, this is due to the high penetration power of their {beta}{sup -} particles that can kill to the cancerous cells and to inhibit the growth of the same ones. To be able to separate them it is necessary to appeal to extremely selective separation techniques, since the chemical properties of these elements are very similar. The chromatography is one of the more used analytical tools, this is due to its great sensibility and the selectivity in the compounds separation, in particular the use of the extractive chromatography has shown the feasibility of carrying out this type of separations for this type of elements. The resin with base of HDEHP was absorbed in an inert support under diverse preparation conditions. The extractant properties of the resin, in relation to the elements Gd and Tb (distribution coefficients), its were determined by means of the dynamic method, using as eluent solutions of nitric acid. The Gd-159 was prepared by irradiation of Gd-168 with thermal neutrons and the Tb-161 it is the result of the radioactive decay of the Gd-161 that is produced in turn with the irradiation with neutrons of Gd-160. The coefficients of distribution of Gd and Tb, using the prepared resin under diverse conditions are presented. (Author)

  7. Efficiency of Polyphenol Extraction from Artificial Honey Using C18 Cartridges and Amberlite® XAD-2 Resin: A Comparative Study

    Directory of Open Access Journals (Sweden)

    Chua Yung An

    2016-01-01

    Full Text Available A comparative study of the extraction efficiency of nine known polyphenols [phenolic acids (benzoic acid, dihydroxybenzoic acid, gallic acid, trans-cinnamic acid, and vanillic acid and flavonoids (naringenin, naringin, quercetin, and rutin] was conducted by deliberately adding the polyphenols to an artificial honey solution and performing solid phase extraction (SPE. Two SPE methods were compared: one using Amberlite XAD-2 resin and another one using a C18 cartridge. A gradient high performance liquid chromatography system with an RP18 column and photodiode array detector was utilized to analyze the extracted polyphenols. The mean percent of recovery from the C18 cartridges was 74.2%, while that from the Amberlite XAD-2 resin was 43.7%. The recoveries of vanillic acid, naringin, and rutin were excellent (>90%; however, gallic acid was not obtained when C18 cartridges were used. Additionally, the reusability of Amberlite XAD-2 resin was investigated, revealing that the mean recovery of polyphenols decreased from 43.7% (1st extraction to 29.3% (3rd extraction. It was concluded that although Amberlite XAD-2 resin yielded a higher number of compounds, C18 cartridges gave a better extraction recovery. The lower recovery seen for the Amberlite XAD-2 resin also cannot be compensated by repeated extractions due to the gradual decrease of extraction recovery when reused.

  8. Improved method for the extraction and chromatographic analysis on a fused-core column of ellagitannins found in oak-aged wine.

    Science.gov (United States)

    Navarro, María; Kontoudakis, Nikolaos; Canals, Joan Miquel; García-Romero, Esteban; Gómez-Alonso, Sergio; Zamora, Fernando; Hermosín-Gutiérrez, Isidro

    2017-07-01

    A new method for the analysis of ellagitannins observed in oak-aged wine is proposed, exhibiting interesting advantages with regard to previously reported analytical methods. The necessary extraction of ellagitannins from wine was simplified to a single step of solid phase extraction (SPE) using size exclusion chromatography with Sephadex LH-20 without the need for any previous SPE of phenolic compounds using reversed-phase materials. The quantitative recovery of wine ellagitannins requires a combined elution with methanol and ethyl acetate, especially for increasing the recovery of the less polar acutissimins. The chromatographic method was performed using a fused-core C18 column, thereby avoiding the coelution of main ellagitannins, such as vescalagin and roburin E. However, the very polar ellagitannins, namely, the roburins A, B and C, still partially coeluted, and their quantification was assisted by the MS detector. This methodology also enabled the analysis of free gallic and ellagic acids in the same chromatographic run. Copyright © 2017 Elsevier Ltd. All rights reserved.

  9. Preliminary extraction of tannins by 1-butyl-3-methylimidazole bromide and its subsequent removal from Galla chinensis extract using macroporous resins.

    Science.gov (United States)

    Lu, Chunxia; Luo, Xiaoling; Lu, Liliang; Li, Hongmin; Chen, Xia; Ji, Yong

    2013-03-01

    In recent years, ionic liquids have become increasingly attractive as 'green solvents' used in the extraction of bioactive compounds from natural plant. However, the separation of ionic liquid from the target compounds was difficult, due to their low vapour pressure and high stabilities. In our study, ionic liquid-based ultrasonic and microwave-assisted extraction was used to obtain the crude tannins, then the macroporous resin adsorption technology was further employed to purify the tannins and remove the ionic liquid from crude extract. The results showed that XDA-6 had higher separation efficiency than other tested resins, and the equilibrium experimental data were well fitted to Langmuir isotherms. Dynamic adsorption and desorption were performed on XDA-6 packed in glass columns to optimise the separation process. The optimum conditions as follows: the ratio of column height to diameter bed was 1:8, flow rate 1 BV/h (bed volume per hour), 85% ethanol was used as eluant while the elution volume was 2 BV. Under the optimised conditions, the adsorption and desoption rate of tannins in XDA-6 were 94.81 and 91.63%, respectively. The content of tannins was increased from 70.24% in Galla chinensis extract to 85.12% with a recovery of 99.06%. The result of ultra-performance liquid chromatography (UPLC)-MS/MS analysis showed that [bmim]Br could be removed from extract.

  10. Partitioning of U, Np, Th, and Eu between acidic aqueous Al(NO3)3 solutions and various TOPO extraction chromatographic materials

    Science.gov (United States)

    Shafer, Jenifer C.; Sulakova, Jana; Ogden, Mark D.; Nash, Kenneth L.

    2010-03-01

    As the Hanford site undergoes remediation, it is noted that significant economies could be realized by minimizing the amount of aluminum deposited in High-Level Waste glass. Though such a step is not planned, an acidic scrub of the Hanford sludge could enhance Al removal. It is likely that the resulting Al(NO3)3 solution would contain measurable amounts of transuranic elements, thus the solution might require some secondary treatment to remove TRU contamination. Thus far, extraction chromatography (EXC) has shown promise [1] as an alternative to a liquid-liquid remediation of the Hanford site. Previous EXC studies have shown >99% of the Eu can be extracted from simulated Al/Cr waste. This study continues an examination of a hypothetical secondary cleanup of the waste by studying the removal of UO22+, NpO2+, NpO22+ and Th4+ from using tri-n-octyl phospine oxide (TOPO) impregnated XAD7 resins. Neptunium was held in the V and VI oxidation states using ascorbic acid and chromate, respectively. Initial results show extraction following classical metal recovery trends, wherein an increased Zeff correlates with increased distribution of the metal into the organic resin phase. The uptake of Eu3+ (representative of An3+) on a column of the same material was also investigated. Uptake kinetics were improved by wetting the TOPO-XAD7 resin with n-dodecane (TOPO-XAD7n). The presence of n-dodecane also provided consistency between batch mode and column mode metal recovery. Preliminary data show >99% recovery of metal ions with a Zeff >= 3 under various simulated conditions.

  11. New methods and materials for solid phase extraction and high performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Dumont, Philip John [Iowa State Univ., Ames, IA (United States)

    1996-04-23

    This paper describes methods for solid phase extraction and high performance liquid chromatography (HPLC). The following are described: Effects of Resin Sulfonation on the Retention of Polar Organic Compounds in Solid Phase Extraction; Ion-Chromatographic Separation of Alkali Metals In Non-Aqueous Solvents; Cation-Exchange Chromatography in Non-Aqueous Solvents; and Silicalite As a Stationary Phase For HPLC.

  12. SEQUENTIAL EXTRACTION OF PHOSPHORUS BY MEHLICH-1 AND ION EXCHANGE RESIN FROM B HORIZONS OF FERRIC AND PERFERRIC LATOSOLS (OXISOLS

    Directory of Open Access Journals (Sweden)

    Danilo de Lima Camêlo

    2015-08-01

    Full Text Available In general, Latosols have low levels of available P, however, the influence of the parent material seems to be decisive in defining the pool and predominant form of P in these soils. This study evaluated P availability by extraction with Mehlich-1 (M-1 and Ion Exchange Resin (IER, from samples of B horizons of Ferric and Perferric Latosols developed from different parent materials. To this end, in addition to the physical and chemical characterization of soils, 10 sequential extractions were performed with M-1 and IER from samples of B horizons (depth between 0.8 and 1.0 m. Total contents of Ca, P, Fe, Al, and Ti were determined after digestion with nitric, hydrofluoric and perchloric acids. The effects of sequential P extractions on Fe oxides were also evaluated from the analyses of dithionite-citrate-bicarbonate and ammonium acid oxalate. The high similarity between contents of P accumulated after sequential extractions with M-1 and IER in soils developed on tuffite indicated a predominance of P-Ca. Higher contents of P after a single IER extraction show greater efficiency in P removal from highly weathered soils, as from the Latosols studied here. The P contents also show the high sensitivity of extractant M-1 in highly buffered soils. Furthermore, a single extraction with extractant M-1 or IER is not sufficient to estimate the amount of labile P in these soils.

  13. Solid-liquid extraction of Gd(Ⅲ) and separation possibilities of rare earths from phosphoric acid solutions using Tulsion CH-93 and Tulsion CH-90 resins

    Institute of Scientific and Technical Information of China (English)

    S.Radhika; V.Nagaraju; B.Nagaphani Kumar; M.Lakshmi Kantam; B.Ramachandra Reddy

    2012-01-01

    Solid-liquid extraction of gadolinium was investigated from phosphoric acid medium using commercial amino phosphonic acid resin,Tulsion CH-93.The experimental conditions studied included equilibration time,acid concentration,mass of the resin,metal concentration,loading and elution.The percent extraction of Gd(Ⅲ) was studied as a function of phosphoric acid (0.05-3 mol/L) using Tulsion CH-93 resin.The corresponding lgD vs.equilibrium pH plot gave straight line with a slope of 1.8.The percent extraction decreased with acid concentration increasing,conforming ion exchange mechanism.Under observed experimental conditions the loading capacity of Tulsion CH-93 for gadolinium was 10.6 mg/g.Among several eluants screened,the quantitative elution of Gd(Ⅲ) from loaded Tulsion CH-93 was obtained with ammonium oxalate (0.15 mol/L).The extraction behavior of commonly associated metals with gadolinium was studied as a function of phosphoric acid concentration.Tulsion CH-93 resin showed selective extraction towards heavy rare earths (Lu and Yb) which could be separated from other rare earths at 3 mol/L H3PO4,similar to wet phosphoric acid (3-5 mol/L).On the other hand Gd(Ⅲ) and other rare earths were studied with chelating resin Tulsion CH-90.Light rare earths were highly extracted and these could be separated from heavy rare earths and Gd.

  14. Characterization of Group V Dubnium Homologs on DGA Extraction Chromatography Resin from Nitric and Hydrofluoric Acid Matrices

    Energy Technology Data Exchange (ETDEWEB)

    Despotopulos, J D; Sudowe, R

    2012-02-21

    somewhere between Nb and Pa. Much more recent studies have examined the properties of Db from HNO{sub 3}/HF matrices, and suggest Db forms complexes similar to those of Pa. Very little experimental work into the behavior of element 114 has been performed. Thermochromatography experiments of three atoms of element 114 indicate that the element 114 is at least as volatile as Hg, At, and element 112. Lead was shown to deposit on gold at temperatures about 1000 C higher than the atoms of element 114. Results indicate a substantially increased stability of element 114. No liquid phase studies of element 114 or its homologs (Pb, Sn, Ge) or pseudo-homologs (Hg, Cd) have been performed. Theoretical predictions indicate that element 114 is should have a much more stable +2 oxidation state and neutral state than Pb, which would result in element 114 being less reactive and less metallic than Pb. The relativistic effects on the 7p{sub 1/2} electrons are predicted to cause a diagonal relationship to be introduced into the periodic table. Therefore, 114{sup 2+} is expected to behave as if it were somewhere between Hg{sup 2+}, Cd{sup 2+}, and Pb{sup 2+}. In this work two commercially available extraction chromatography resins are evaluated, one for the separation of Db homologs and pseudo?homologs from each other as well as from potential interfering elements such as Group IV Rf homologs and actinides, and the other for separation of element 114 homologs. One resin, Eichrom's DGA resin, contains a N,N,N',N'-tetra-n-octyldiglycolamide extractant, which separates analytes based on both size and charge characteristics of the solvated metal species, coated on an inert support. The DGA resin was examined for Db chemical systems, and shows a high degree of selectivity for tri-, tetra-, and hexavalent metal ions in multiple acid matrices with fast kinetics. The other resin, Eichrom's Pb resin, contains a di-t-butylcyclohexano 18-crown-6 extractant with isodecanol solvent

  15. Extraction of anthocyanins from black bean canning wastewater with macroporous resins.

    Science.gov (United States)

    Wang, Xiaoxi; Hansen, Conly; Allen, Karin

    2014-02-01

    This study investigated purification of anthocyanins from black bean canning wastewater by column chromatography with 5 types of macroporous resins (Diaion Hp20, Sepabeads Sp70, Sepabeads Sp207, Sepabeads Sp700, and Sepabeads Sp710). By-product of canned black beans was partially purified by filtration, in anticipation of higher performance during column chromatography. Equilibrium adsorption isotherms were measured and analyzed using Langmuir and Freundlich isotherm models. Both Langmuir (all R² ≥ 0.98) and Freundlich (all R² ≥ 0.97) models can describe the adsorption process of anthocyanins from black bean canning wastewater using the tested resins. The adsorption and desorption behaviors of anthocyanins were studied using a dynamic method on the 5 types of resins, and Sp700 presented the highest adsorption capacity (39 ± 4 mg/g; P canning wastewater.

  16. Purification of gamma-amino butyric acid (GABA) from fermentation of defatted rice bran extract by using ion exchange resin

    Science.gov (United States)

    Tuan Nha, Vi; Phung, Le Thi Kim; Dat, Lai Quoc

    2017-09-01

    Rice bran is one of the significant byproducts of rice processing with 10 %w/w of constitution of whole rice grain. It is rich in nutrient compounds, including glutamic acid. Thus, it could be utilized for the fermentation with Lactobateria for synthesis of GABA, a valuable bioactive for antihypertensive effects. However, the concentration and purity of GABA in fermentation broth of defatted rice bran extract is low for production of GABA drug. This research focused on the purification of GABA from the fermentation broth of defatted rice bran extract by using cation exchange resin. The results indicate that, the adsorption isotherm of GABA by Purelite C100 showed the good agreement with Freundlich model, with high adsorption capacity. The effects of pH and concentration of NaCl in eluent on the elution were also investigated. The obtained results show that, at the operating conditions of elution as follows: pH 6.5, 0.8 M of NaCl in eluent, 0.43 of bed volume; concentration of GABA in accumulative eluent, the purity and recovery yield of GABA were 743.8 ppm, 44.0% and 84.2%, respectively. Results imply that, it is feasible to apply cation exchange resin for purification of GABA from fermentation broth of defatted rice bran extract.

  17. Review: Resin Composite Filling

    Science.gov (United States)

    Chan, Keith H. S.; Mai, Yanjie; Kim, Harry; Tong, Keith C. T.; Ng, Desmond; Hsiao, Jimmy C. M.

    2010-01-01

    The leading cause of oral pain and tooth loss is from caries and their treatment include restoration using amalgam, resin, porcelain and gold, endodontic therapy and extraction. Resin composite restorations have grown popular over the last half a century because it can take shades more similar to enamel. Here, we discuss the history and use of resin, comparison between amalgam and resin, clinical procedures involved and finishing and polishing techniques for resin restoration. Although resin composite has aesthetic advantages over amalgam, one of the major disadvantage include polymerization shrinkage and future research is needed on reaction kinetics and viscoelastic behaviour to minimize shrinkage stress.

  18. Enrichment and purification of total flavonoids from Flos Populi extracts with macroporous resins and evaluation of antioxidant activities in vitro.

    Science.gov (United States)

    Wan, Pengfei; Sheng, Zunlai; Han, Qiang; Zhao, Yulin; Cheng, Guangdong; Li, Yanhua

    2014-01-15

    Enrichment and purification of total flavonoids from Flos Populi extracts were studied using five macroporous resins. The static tests indicated that NKA-9 resin was appropriate and its adsorption data were well fitted to the Langmuir and Freundlich isotherms. To optimize the separation process, dynamic adsorption and desorption tests were carried out. The optimal adsorption parameters were initial concentrations in sample solution of 7.64mg/mL, pH of 5.0, sample loading amount of 2.3BV, flow rate of 2BV/h, temperature of 25°C. The optimal desorption parameters were deionized water and 20% ethanol each 5BV, then 60% ethanol of 10 BV, flow rate of 2BV/h. After one run treatment with NKA-9 resin, the content of total flavonoids in the product increased from 11.38% to 53.41%, and the recovery yield was 82.24%. The results showed that NKA-9 resin revealed a good ability to enrichment total flavonoids from Flos Populi, and the method can be referenced for the enrichment of total flavonoids from other materials. The antioxidant activities of the purified flavonoids were further evaluated in vitro. It showed that the DPPH radical scavenging increased from 59.46% to 82.63% at different concentrations (0.06-0.14mg/mL). At different concentrations (0.6-1.4mg/mL), the hydroxyl radical scavenging increased from 35.39% to 74.12%. Moreover, the reducing ability and total oxidant capacity appeared to be dose-dependent of flavonoids. It indicated that the purified flavonoids can be used as a source of potential antioxidant.

  19. THE THERMAL AND ABLATIVE DEGRADATION OF SOME EPOXY RESINS CURED WITH METHYL BICYCLO(2.2.1)HEPTENE-2,3-DICARBOXYLIC ANHYDRIDE (NMA).

    Science.gov (United States)

    ABLATION), (* EPOXY RESINS , (*PYROLYSIS, EPOXY RESINS ), CYCLOALKENES, ANHYDRIDES, CATALYSTS, ADDITIVES, CROSSLINKING(CHEMISTRY), REACTION KINETICS, DEGRADATION, AGING(MATERIALS), INFRARED SPECTRA, CHROMATOGRAPHIC ANALYSIS.

  20. Supercritical fluid extraction and chromatographic analysis (HRGC-FID and HRGC-MS) of Lupinus spp. alkaloids

    OpenAIRE

    Nossack,Ana C.; Janete H.Y. VILEGAS; Baer,Dietrich von; Fernando M. LANÇAS

    2000-01-01

    The alkaloid extracts from Lupinus spp., obtained by conventional methods (maceration/sonication - solid phase extraction; maceration/sonication - liquid-liquid extraction) and SFE (supercritical fluid extraction) using CO2 and modified CO2 (CO2/MeOH, CO2/EtOH, CO2/iPrOH and CO2/H2O) were analysed by HRGC-FID (high resolution gas chromatography - flame ionization detector) and HRGC-MS (high resolution gas chromatography - mass spectrometry). The HRGC-FID quantitative analyses were performed w...

  1. Sperm motility inhibitory effect of the benzene chromatographic fraction of the chloroform extract of the seeds of Carica papaya in langur monkey, Presbytis entellus entellus

    Institute of Scientific and Technical Information of China (English)

    Nirmal K.Lohiya; Boomi Manivannan; Shipra Goyal; Abdul S.Ansari

    2008-01-01

    Aim: To assess the contraceptive efficacy of the benzene chromatographic fraction of the chloroform extract of the seeds of Carica papaya in langur monkeys. Methods: The test substance was given p.o. to five monkeys at 50 mg/kg body weight/day for 360 days. Control animals (n = 3) received olive oil as vehicle. Sperm parameters as per World Health Organization standards, sperm functional tests, morphology of testis and epididymis, haematology, clinical biochemistry, serum testosterone and libido were evaluated. Following completion of 360 days treatment the animals were withdrawn from the treatment and the recovery pattern was assessed by semen analysis and sperm functional tests. Results: Total inhibition of sperm motility was observed following 60 days of treatment that continued until 360 days study period. Sperm count, percent viability and percent normal spermatozoa showed a drastic decline following 30 days of treatment. Sperm morphology showed predominant mid piece abnormalities. Sperm functional tests scored in sterile range. Histology and ultrastructure of testis revealed vacuolization in the Sertoli cells and germ cells. Loss of cytoplasmic organelles was evident in spermatocytes and round spermatids. Histology and ultrastruc-ture of epididymis of treated animals were comparable to those of control animals. Hematological and serum clinicalparameters and testosterone levels fluctuated within the control range throughout the study period. Recovery was evident following 60-120 days of treatment withdrawal. Conclusion: The results suggest that the benzene chro-matographic fraction of the chloroform extract of the seeds of Carica papaya shows contraceptive efficacy without adverse toxicity, mediated through inhibition of sperm motility.

  2. The effect of Psidium guajava Linn leaf extract on Candida albicans adherence and the transversal strength of acrylic resin

    Directory of Open Access Journals (Sweden)

    Amiyatun Naini

    2008-03-01

    Full Text Available Denture stomatitis is an inflammation of oral cavity due to removable denture wearing. Prevention of denture stomatitis can be effectively done by using mouth rinsing. Currently, Indonesian government is actively promoting traditional herbal medicine as an alternative medicine such as Psidium guajava Linn leaf which has an anti bacterial and anti fungal ability. The purpose of this study was to know the effective concentration and soaking duration to reduce Candida albicans without lowering transversal strength of acrylic resin. This experimental laboratory study was using heat cured acrylic resin plate without surface polishing. The concentration of Psidium guajava Linn leaf extract used in this study were 32%, 34%, 36%, and 38% respectively with 15 minutes, 30 minutes, 1 hour and 8 hours soaking duration. The transversal strength was measured in the same concentration with 2 days, 10 days and 60 days soaking duration. Sterile aquadest was used as control. Two direction ANOVA and LSD test were used in data analysis. The result showed significant difference in the number of Candida albicans colony among concentrations and soaking durations. Significant difference was also found in transversal strength among concentrations and soaking durations. It is concluded that the extract of Psidium guajava Linn leaf in 38% concentration with 8 hours soaking duration will lower the Candida albicans colony, whereas 38% concentration with 60 days soaking duration will lower the transversal strength but it is still above the standard value.

  3. High-performance liquid chromatographic (HPLC) separation and quantitation of endogenous glucocorticoids after solid-phase extraction from plasma.

    Science.gov (United States)

    Dawson, R; Kontur, P; Monjan, A

    1984-01-01

    This study describes a method for the extraction and simultaneous measurement of cortisone, cortisol and corticosterone using dexamethasone as an internal standard. Solid-phase extraction of plasma steroids with C18 columns allows the samples to be extracted, washed and concentrated in a single step with minimal sample handling and without the use of large volumes of organic solvents. HPLC separation of the steroids is accomplished within 10 min and the individual steroid peaks are quantitated by UV detection at 239 nm. This assay was examined for linearity, extraction efficiency, precision and potential interference by commonly used drugs. Plasma values of glucocorticoids are reported for samples obtained from human subjects as well as from rats. HPLC was also compared to RIA for the determination of plasma levels of corticosterone in the rat. Solid-phase extraction and assay by HPLC provides a rapid and specific method for the simultaneous determination of plasma glucocorticoids.

  4. Novel polysiloxane resin functionalized with dicyclohexano-18-crown-6 (DCH18C6): Synthesis, characterization and extraction of Sr(II) in high acidity HNO3 medium.

    Science.gov (United States)

    Ye, Gang; Bai, Feifei; Wei, Jichao; Wang, Jianchen; Chen, Jing

    2012-07-30

    A novel kind of polysiloxane resin functionalized with dicyclohexano-18-crown-6 (DCH18C6) was synthesized through a post-modification approach. The DCH18C6 moieties bearing amino groups were firstly prepared, followed by covalent grafting to a silica precursor P-(CH(2))(3)-Cl (Where P represents a 3-dimentional polymerized silica matrix) based on nucleophilic substitution reaction. (29)Si and (13)C solid-state NMR, FT-IR, XPS, TGA, ESEM and elemental analysis were employed to systematically characterize the structure, thermal property and surface morphology of the functionalized resin. The results indicated that the DCH18C6 ligands were successfully bonded to the polysiloxane resin with a satisfactory grafting degree (33.6wt.%). Due to the robust organosilica framework and the covalent immobilization of the ligands, the functionalized resin had excellent thermal stability and acid resistance. Batch experiments showed that the resin could effectively separate Sr(II) in high acidity mediums. The distribution coefficient (K(d)) of 43.6cm(3)/g could be achieved in 5.0mol/L HNO(3) solution. The influences of contact time and acidity of HNO(3) on the resin's extraction performance were examined. The reusability and the selectivity to Sr(II) over interference ions were investigated. The DCH18C6-functionalized resin might be potentially applied for the radiostrontium removal in the high level liquid waste (HLLW).

  5. Countercurrent Chromatographic Separation of Lipophilic Ascorbic Acid Derivatives and Extract from Kadsura Coccinea Using Hydrophobic Organic-Aqueous Two-Phase Solvent Systems.

    Science.gov (United States)

    Shinomiya, Kazufusa; Li, Heran; Kitanaka, Susumu; Ito, Yoichiro

    2009-01-01

    Countercurrent chromatographic (CCC) separation of lipophilic ascorbic acid derivatives and the crude extract from Kadsura Coccinea was performed using the type-J multilayer coil planet centrifuge with a hydrophobic organic-aqueous two-phase solvent system composed of n-hexane/ethyl acetate/ethanol/aqueous 0.1% trifluoroacetic acid at the volume ratio of (5 : 5 : 6 : 2). The lipophilic ascorbic acid derivatives were separated in the order of L-ascrobyl 2,6-dibutyrate, L-ascorbyl 6-palmitate and L-ascorbyl 6-stearate by eluting the lower phase as the mobile phase, and L-ascorbyl 2,6-dipalmitate was separated by eluting the upper phase at the opposite direction. The above solvent system was then applied to the CCC separation of the extract prepared from K. coccinea. With lower phase mobile, the extract was mainly separated into two peaks corresponding to lignans and triterpenoids accordingly. The HPLC analysis of the fractions showed that the former peak contained Kadsulignan N, Schizandrin H and Neokadsuranin as lignans, and the latter peak, Micranoic acid A, Neokadsuranic acid B and beta-Sitosterol as triterpenoids. The overall results indicate that the hydrophobic organic-aqueous two-phase solvent system used in the present studies was useful for the CCC separation of lignans and triterpenoids present in the natural products.

  6. Antioxidant Activity and Gas Chromatographic-Mass Spectrometric Analysis of Extracts of the Marine Algae, Caulerpa peltata and Padina Gymnospora.

    Science.gov (United States)

    Murugan, Kavitha; Iyer, Vidhya V

    2014-01-01

    The results of our previous investigations on extracts of selected marine algae showed that Caulerpa peltata and Padina gymnospora had more promising antiproliferative and antioxidant activities than Gelidiella acerosa and Sargassum wightii. Based on these results, the more active chloroform extract of C. peltata and ethyl acetate extract of P. gymnospora were further analyzed for their constituents by using gas chromatography in tandem with mass spectrometry. The GC-MS analysis (GC % peak area given in parentheses) showed that fucosterol (12.45%) and L-(+)-ascorbic acid 2, 6-dihexadecanoate (8.13%) were the major compounds present in P. gymnospora ethyl acetate extract. On the other hand, C. peltata chloroform extract had 1-heptacosanol (10.52%), hexacosanol acetate (9.28%), tetradecyl ester of chloroacetic acid (7.22%), Z,Z-6, 28-heptatriactontadien-2-one (6.77%) and 10, 13-dimethyl-methyl ester of tetradecanoic acid (5.34%) as major compounds. Also described in the report are the beta-carotene bleaching inhibitory and total reducing activities of the chloroform and ethyl acetate extracts of C. peltata and P. gymnospora, respectively, relative to the other three extracts (aqueous, methanol, chloroform or ethyl acetate) of the two algae.

  7. Antioxidant activity and gas chromatographic-mass spectrometric analysis of extracts of the marine algae, caulerpa peltata and padina gymnospora

    Directory of Open Access Journals (Sweden)

    Kavitha Murugan

    2014-01-01

    Full Text Available The results of our previous investigations on extracts of selected marine algae showed that Caulerpa peltata and Padina gymnospora had more promising antiproliferative and antioxidant activities than Gelidiella acerosa and Sargassum wightii. Based on these results, the more active chloroform extract of C. peltata and ethyl acetate extract of P. gymnospora were further analyzed for their constituents by using gas chromatography in tandem with mass spectrometry. The GC-MS analysis (GC % peak area given in parentheses showed that fucosterol (12.45% and L-(+-ascorbic acid 2,6-dihexadecanoate (8.13% were the major compounds present in P. gymnospora ethyl acetate extract. On the other hand, C. peltata chloroform extract had 1-heptacosanol (10.52%, hexacosanol acetate (9.28%, tetradecyl ester of chloroacetic acid (7.22%, Z,Z-6,28-heptatriactontadien-2-one (6.77% and 10,13-dimethyl-methyl ester of tetradecanoic acid (5.34% as major compounds. Also described in the report are the beta-carotene bleaching inhibitory and total reducing activities of the chloroform and ethyl acetate extracts of C. peltata and P. gymnospora, respectively, relative to the other three extracts (aqueous, methanol, chloroform or ethyl acetate of the two algae.

  8. Rational design and chromatographic evaluation of histamine imprinted polymers optimised for solid-phase extraction of wine samples.

    Science.gov (United States)

    Basozabal, Itsaso; Gomez-Caballero, Alberto; Diaz-Diaz, Goretti; Guerreiro, António; Gilby, Stuart; Goicolea, M Aranzazu; Barrio, Ramón J

    2013-09-20

    This article reports on the computational design, development and application of a molecularly imprinted polymer (MIP) with specific affinity towards histamine. Computational modelling was used to screen a monomer library in order to select the monomers able to form the strongest complex with the target analyte. These were subsequently used for MIP synthesis by radical polymerisation initiated by UV. MIPs were then evaluated by liquid chromatography and solid phase extraction (SPE) and best MIP behaviour was observed when itaconic acid was used as functional monomer. Finally, after optimisation of the polymer composition, MIPs were used as adsorbents for SPE and clean-up of histamine in wine samples. The proposed histamine extraction method with the MIP-SPE cartridge was found to be reproducible (wine extracts. The described methodology is simple and fast and is suitable for the selective histamine extraction and its subsequent quantification by HPLC-DAD from complex matrices such as wine samples.

  9. Effects of an acetone extract of Boswellia carterii Birdw. (Burseraceae) gum resin on adjuvant-induced arthritis in lewis rats.

    Science.gov (United States)

    Fan, A Y; Lao, L; Zhang, R X; Zhou, A N; Wang, L B; Moudgil, K D; Lee, D Y W; Ma, Z Z; Zhang, W Y; Berman, B M

    2005-10-03

    Ruxiang (Gummi olibanum), the dried gum resin of Boswellia carterii (BC), has been used in traditional Chinese medicine to alleviate pain and inflammation for thousands of years. In this random, blinded study, the anti-arthritic effects of a BC extract were observed and compared to vehicle control in a Lewis rat adjuvant arthritis model (n=8/group). Arthritis was induced by injecting CFA subcutaneously into the base of the tail, and the extract was administered orally (i.g.) for 10 consecutive days beginning on day 16 after the injection. Arthritic scores, paw edema, and the local tissue pro-inflammatory cytokines tumor necrosis factor alpha (TNF-alpha) and interleukin-1 beta (IL-1beta) were assessed. Toxicity and adverse effects of the extract were evaluated. At 0.90 g/kg per day, BC significantly decreased arthritic scores between days 20 and 25 (p<0.05) and reduced paw edema on days 18, 20 and 22 compared to control (p<0.05). It also significantly suppressed local tissue TNF-alpha and IL-1beta (p<0.05). No major adverse effects were observed in animals during the repeated-dose treatment profile although mild fur discoloration was noted. The data show that BC extract has significant anti-arthritic and anti-inflammation effects and suggest that these effects may be mediated via the suppression of pro-inflammatory cytokines.

  10. Chromatographic fingerprinting and free-radical scavenging activity of ethanol extracts of Muntingia calabura L. leaves and stems

    Directory of Open Access Journals (Sweden)

    William Patrick Cruiz Buhian

    2017-02-01

    Conclusions: M. calabura exhibited very high antioxidant activity in its leaves and stems ethanol extracts, both of which are used in traditional medicine. The TLC results demonstrated the presence of diverse secondary metabolites in the leaf and stem ethanol extracts, indicating that the antioxidant activity, including other bioactivities may be attributed to these phytochemical constituents. This paper has reported for the first time the TLC fingerprinting of M. calabura using visible light, UV 254 nm, UV 366 and post-derivatization with vanillin-spray to visualize separate spots on TLC plates.

  11. Hyphenated chromatographic techniques for the rapid screening and identification of antioxidants in methanolic extracts of pharmaceutically used plants .

    NARCIS (Netherlands)

    Exarchou, V.; Fiamegos, Y.C.; Beek, van T.A.; Nanos, C.G.; Vervoort, J.J.M.

    2006-01-01

    Phytochemical analysis is an important scientific research area, which normally relies on a number of rather laborious and time-consuming techniques for compound identification. Isolation of the ingredients of plant extracts in adequate quantities for spectral and biological analysis was the basis o

  12. Chromatographic separation of fructose from date syrup.

    Science.gov (United States)

    Al Eid, Salah M

    2006-01-01

    The objective of this study is to provide a process for separating fructose from a mixture of sugars containing essentially fructose and glucose, obtained from date palm fruits. The extraction procedure of date syrup from fresh dates gave a yield of 86.5% solids after vacuum drying. A process for separating fructose from an aqueous solution of date syrup involved adding the date syrup solutions (20, 30 and 40% by weight) to a chromatographic column filled with Dowex polystyrene strong cation exchange gel matrix resin Ca2 + and divinylbenzene, a functional group, sulfonic acid, particle size 320 microm, with a flow rate of 0.025 and 0.05 bed volume/min, under 30 and 70 degrees C column temperature. After the date sugar solution batch, a calculated quantity of water was added to the column. Glucose was retained by the resin more weakly than fructose and proceeded faster into the water batch flowing ahead. Three fractions were collected: a glucose-rich fraction, a return fraction, and a fructose-rich fraction. The return fraction is based on when the peaks of fructose and glucose were reached, which could be determined by means of an analyzer (polarimeter) based on the property of glucose and fructose solutions to turn the polarization level of polarized light. A high yield of fructose is obtained at 70 degrees C column temperature with a flow rate of 0.025 bed volume/min and date syrup solution containing 40% sugar concentration. The low recovery by weight obtained using date syrup solutions having a sugar concentration of 20 and 30%, encourages the use of a concentration of 40%. However, with the 40% date syrup supply the average concentrations of glucose and fructose in the return fractions were more than 40%, which can be used for diluting the thick date syrup solution extracted from dates.

  13. Preparative separation and purification of Rebaudioside A from Stevia rebaudiana Bertoni crude extracts by mixed bed of macroporous adsorption resins.

    Science.gov (United States)

    Li, Jie; Chen, Zhenbin; Di, Duolong

    2012-05-01

    The separation and purification of Rebaudioside A (RA) from Stevia rebaudiana Bertoni crude extracts (Steviosides) by macroporous adsorption resin (MAR) mixed bed were systematically investigated. MAR mixed bed of HPD750-LSA40-LSA30-DS401 was selected due to its better separation degree. Based on the kinetics/thermodynamics experiment of the mixed bed, it was found that the experimental data fitted better to the pseudo-second-order model, and intra-particle diffusion was rate-limiting step. The adsorption isotherm was consistent with IV equilibrium adsorption isotherm classified by Brunauer. Furthermore, the influencing factors for the separation of RA based on HPLC were also investigated. Under the optimal conditions, the separation degree for RA (DAS) increased from 0.771 to 1.54. Moreover, the experimental results showed that the purity of the obtained product increased from 60% to 97%.

  14. Flavonoid dimers from the total phenolic extract of Chinese dragon's blood, the red resin of Dracaena cochinchinensis.

    Science.gov (United States)

    Pang, Dao-Ran; Su, Xiao-Qin; Zhu, Zhi-Xiang; Sun, Jing; Li, Yue-Ting; Song, Yue-Lin; Zhao, Yun-Fang; Tu, Peng-Fei; Zheng, Jiao; Li, Jun

    2016-12-01

    Eight new flavonoid dimers, named cochinchinenins I-M (1-5), including three pairs of enantiomers (1a/1b-3a/3b) and two optically pure flavonoid dimers (4-5), along with a known analogue (6), were isolated from total phenolic extract of the red resin of Dracaena cochinchinensis (Chinese dragon's blood). The planar structures of 1-5 were elucidated by extensive spectroscopic analysis including HRESIMS and 1D/2D NMR. Their absolute configurations were determined on the basis of experimental and calculated electronic circular dichroism (ECD) data. Compounds 4 and 5 exhibited significant inhibition of nitric oxide production in lipopolysaccharide-stimulated BV-2 microglial cells with IC50 value of 4.9±0.4 and 5.4±0.6μM, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Chromatographic finger print analysis of anti-inflammatory active extract fractions of aerial parts of Tribulus terrestris by HPTLC technique

    Institute of Scientific and Technical Information of China (English)

    Mona Salih Mohammed; Mohamed Fahad Alajmi; Perwez Alam; Hassan Subki Khalid; Abelkhalig Muddathir Mahmoud; Wadah Jamal Ahmed

    2014-01-01

    Objective:To develop HPTLC fingerprint profile of anti-inflammatory active extract fractions of Tribulus terrestris (family Zygophyllaceae). Methods:The anti-inflammatory activity was tested for the methanol and its fractions (chloroform, ethyl acetate, n-butanol and aqueous) and chloroform extract of Tribulus terrestris (aerial parts) by injecting different groups of rats (6 each) with carrageenan in hind paw and measuring the edema volume before and 1, 2 and 3 h after carrageenan injection. Control group received saline i.p. The extracts treatment was injected i.p. in doses of 200 mg/kg 1 h before carrageenan administration. Indomethacin (30 mg/kg) was used as standard. HPTLC studies were carried out using CAMAG HPTLC system equipped with Linomat IV applicator, TLC scanner 3, Reprostar 3, CAMAG ADC 2 and WIN CATS-4 software for the active fractions of chloroform fraction of methanol extract. Results:The methanol extract showed good antiedematous effect with percentage of inhibition more than 72%, indicating its ability to inhibit the inflammatory mediators. The methanol extract was re-dissolved in 100 mL of distilled water and fractionated with chloroform, ethyl acetate and n-butanol. The four fractions (chloroform, ethyl acetate, n-butanol and aqueous) were subjected to anti-inflammatory activity. Chloroform fraction showed good anti-inflammatory activity at dose of 200 mg/kg. Chloroform fraction was then subjected to normal phase silica gel column chromatography and eluted with petroleum ether-chloroform, chloroform-ethyl acetate mixtures of increasing polarity which produced 15 fractions (F1-F15). Only fractions F1, F2, F4, F5, F7, F9, F11 and F14 were found to be active, hence these were analyzed with HPTLC to develop their finger print profile. These fractions showed different spots with different Rf values. Conclusions:The different chloroform fractions F1, F2, F4, F5, F7, F9, F11 and F14 revealed 4, 7, 7, 8, 9, 7, 7 and 6 major spots, respectively. The

  16. Hydrophobic features of EPS extracted from anaerobic granular sludge: an investigation based on DAX-8 resin fractionation and size exclusion chromatography.

    Science.gov (United States)

    Cao, Feishu; Bourven, Isabelle; Lens, Piet N L; van Hullebusch, Eric D; Pechaud, Yoan; Guibaud, Gilles

    2017-04-01

    The hydrophobic fractionation of extracellular polymeric substances (EPS) extracted from anaerobic granular sludge was performed on the DAX-8 resin (two elution pH conditions, i.e., pH 2 and pH 5 were tested). The impact of seven different EPS extraction methods on EPS hydrophobicity features was assessed. The results showed that the extraction methods and bulk solution pH influenced dramatically the biochemical composition of the EPS, and in turn, the hydrophobicity determined. Besides, EPS extracting reagents i.e., formaldehyde, ethanol, sodium dodecyl sulfate (SDS), and Tween 20 not only introduced extra carbon content in the total organic carbon (TOC) measurement but also interacted with the DAX-8 resin. By comparing the apparent molecular weight (aMW) distribution of untreated and pH-adjusted EPS samples, more complete EPS aMW information was preserved at pH 5. Thus, elution at pH 5 was preferred in this study for the qualitative analysis of EPS hydrophobic features. The hydrophobic fraction of EPS retained by the resin at pH 5 was ascribed to a wide aMW range, ranging from >440 to 0.3 kDa. Within this range, EPS molecules ranging from 175 to 31 kDa were mostly retained by the DAX-8 resin, which indicates that these EPS molecules are highly hydrophobic.

  17. A systematic approach for the chromatographic fractionation and purification of major steroid saponins in commercial extracts of Yucca schidigera Roezl.

    Science.gov (United States)

    Sastre, F; Ferreira, F; Pedreschi, F

    2017-03-01

    Yucca schidigera Roezl. (yucca) is one of the major industrial sources of steroid saponins used as animal and human food additives. This work describes a new, systematic and reproducible three-step method by medium and high-pressure liquid chromatography (under RP, NP and RP conditions), for the isolation and purification of three groups of saponins, which were further purified in six sub-fractions, and finally into twelve individual steroid saponins previously reported in Y. schidigera. In accordance to the increasing applications of yucca extracts, further analytical, biological and physicochemical studies are still required. The presented method is applicable to the preparation of steroids saponins previously reported in commercial extracts of Y. schidigera, both as highly purified mixtures of defined composition, including twelve pure components. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Efficient extraction and preparative separation of four main isoflavonoids from Dalbergia odorifera T. Chen leaves by deep eutectic solvents-based negative pressure cavitation extraction followed by macroporous resin column chromatography.

    Science.gov (United States)

    Li, Lu; Liu, Ju-Zhao; Luo, Meng; Wang, Wei; Huang, Yu-Yan; Efferth, Thomas; Wang, Hui-Mei; Fu, Yu-Jie

    2016-10-15

    In this study, green and efficient deep eutectic solvent-based negative pressure cavitation-assisted extraction (DES-NPCE) followed by macroporous resin column chromatography was developed to extract and separate four main isoflavonoids, i.e. prunetin, tectorigenin, genistein and biochanin A from Dalbergia odorifera T. Chen leaves. The extraction procedure was optimized systematically by single-factor experiments and a Box-Behnken experimental design combined with response surface methodology. The maximum extraction yields of prunetin, tectorigenin, genistein and biochanin A reached 1.204, 1.057, 0.911 and 2.448mg/g dry weight, respectively. Moreover, the direct enrichment and separation of four isoflavonoids in DES extraction solution was successfully achieved by macroporous resin AB-8 with recovery yields of more than 80%. The present study provides a convenient and efficient method for the green extraction and preparative separation of active compounds from plants.

  19. Molecularly Imprinted Polymers for Selective Extraction of Crystal Violet from Natural Seawater coupled with High- Performance Liquid Chromatographic Determination

    Institute of Scientific and Technical Information of China (English)

    LIAN Ziru; WANG Jiangtao

    2014-01-01

    Molecularly imprinted polymers (MIPs) were prepared by the bulk polymerization using crystal violet as the template molecule, and the methacrylic acid and ethylene glycol dimetheacrylate as functional monomer and cross-linker, respectively. Sys-tematic investigations of synthetic conditions were conducted. The surface morphology and recognition mechanism of the obtained polymers were studied using scanning electron microscope and spectrophotometric analysis. MIPs showed high affinity to template molecule and were successfully applied as special solid-phase extraction sorbent for selective extraction of crystal violet from natural seawater. An off-line molecularly imprinted solid-phase extraction (MISPE) method followed by high-performance liquid chroma-tography with diodearray detection for the analysis of crystal violet was also established. MISPE columns have good recoveries for crystal violet standard solutions and good linearity was obtained over the concentration range of 0-200μg L-1 (R2>0.99). Finally, two natural seawater samples were investigated. The recoveries of spiked seawater on the MISPE columns were from 44.47% to 62.34%, the relative standard deviation (n=3) being in the range of 2.89%-5.96%.

  20. Metal-organic framework mixed-matrix disks: Versatile supports for automated solid-phase extraction prior to chromatographic separation.

    Science.gov (United States)

    Ghani, Milad; Font Picó, Maria Francesca; Salehinia, Shima; Palomino Cabello, Carlos; Maya, Fernando; Berlier, Gloria; Saraji, Mohammad; Cerdà, Víctor; Turnes Palomino, Gemma

    2017-03-10

    We present for the first time the application of metal-organic framework (MOF) mixed-matrix disks (MMD) for the automated flow-through solid-phase extraction (SPE) of environmental pollutants. Zirconium terephthalate UiO-66 and UiO-66-NH2 MOFs with different size (90, 200 and 300nm) have been incorporated into mechanically stable polyvinylidene difluoride (PVDF) disks. The performance of the MOF-MMDs for automated SPE of seven substituted phenols prior to HPLC analysis has been evaluated using the sequential injection analysis technique. MOF-MMDs enabled the simultaneous extraction of phenols with the concomitant size exclusion of molecules of larger size. The best extraction performance was obtained using a MOF-MMD containing 90nm UiO-66-NH2 crystals. Using the selected MOF-MMD, detection limits ranging from 0.1 to 0.2μgL(-1) were obtained. Relative standard deviations ranged from 3.9 to 5.3% intra-day, and 4.7-5.7% inter-day. Membrane batch-to-batch reproducibility was from 5.2 to 6.4%. Three different groundwater samples were analyzed with the proposed method using MOF-MMDs, obtaining recoveries ranging from 90 to 98% for all tested analytes.

  1. Supercritical fluid extraction of amino acids from birch (Betula pendula Roth) leaves and their liquid chromatographic determination with fluorimetric detection.

    Science.gov (United States)

    Klejdus, Borivoj; Lojková, Lea; Kula, Emanuel; Buchta, Ivan; Hrdlicka, Petr; Kubán, Vlastimil

    2008-05-01

    A method for supercritical fluid extraction (SFE) of amino acids was adapted and optimal experimental conditions were selected for a matrix consisting of dry leaves. The matrix-dependent SFE method uses a mixture of MeOH-H(2)O-acetonitrile (10:10:1 v/v/v) as a modifier (0.5 mL in situ, 300 muL on-line) at 70 degrees C and 40 MPa and no HCl is needed as an entrainer. The amino acids were quantified using high-performance liquid chromatography with fluorimetric detection (HPLC/FLD) after gradient elution on Zorbax Eclipse AAA columns (4.6x150 mm, 3.5 mum) with aqueous Na(2)HPO(4 )buffer of pH 7.8 and ACN-MeOH-water as a mobile phase. In comparison with Soxhlet extraction, SFE gave higher recovery and selectivity, but it required longer extraction time (90 min) and it was more labor-intensive (clean-up step after the pre-concentration). Both methods should be used separately or in combination according to the matrix, number of samples, and levels of ballast compounds.

  2. Supercritical fluid carbon dioxide extraction and liquid chromatographic separation with electrochemical detection of methylmercury from biological samples

    Science.gov (United States)

    Simon, N.S.

    1997-01-01

    Using the coupled methods presented in this paper, methylmercury can be accurately and rapidly extracted from biological samples by modified supercritical fluid carbon dioxide and quantitated using liquid chromatography with reductive electrochemical detection. Supercritical fluid carbon dioxide modified with methanol effectively extracts underivatized methylmercury from certified reference materials Dorm-1 (dogfish muscle) and Dolt-2 (dogfish liver). Calcium chloride and water, with a ratio of 5:2 (by weight), provide the acid environment required for extracting methylmercury from sample matrices. Methylmercury chloride is separated from other organomercury chloride compounds using HPLC. The acidic eluent, containing 0.06 mol L-1 NaCl, insures the presence of methylmercury chloride and facilitates the reduction of mercury on a glassy carbon electrode. If dual glassy carbon electrodes are used, a positive peak is observed at -0.65 to -0.70 V and a negative peak is observed at -0.90V with the organomercury compounds that were tested. The practical detection limit for methylmercury is 5 X 10-8 mol L-1 (1 X 10-12 tool injected) when a 20 ??L injection loop is used.

  3. Development and validation of a high-performance liquid chromatographic assay for the determination of fluconazole in human whole blood using solid phase extraction.

    Science.gov (United States)

    Zhang, Shimin; Mada, Sripal Reddy; Torch, Marilyn; Goyal, Rakesh K; Venkataramanan, Raman

    2008-06-01

    A sensitive and specific high-performance liquid chromatographic ultraviolet method for the determination of fluconazole in human whole blood has been developed and validated. Whole blood samples were processed by a solid phase extraction procedure using an Oasis HLB extraction cartridge before chromatography. Phenacetin was used as the internal standard. Chromatography was performed using Waters C18 Symmetry analytical column, 5 microm, 4.6 x 250 mm, using an isocratic elution with a mobile phase consisting of acetonitrile and water (36:64, v/v) at a flow rate of 0.8 mL/min. The retention times of fluconazole and phenacetin were 4.7 and 8.3 minutes, respectively, and the total run time was 10 minutes. Quantitative analysis was performed using a Waters UV-VIS detector at a wavelength of 210 nm. The assay was linear over the concentration range of 0.5 to 15 microg/mL for fluconazole. The extraction recoveries at concentrations of 2.5, 5, and 10 microg/mL were 105.9%, 98.4%, and 95%, respectively. The method can quantify 0.5 microg/mL fluconazole using 300 microL of whole blood. At concentrations of 2.5, 5, and 10 microg/mL, the intraday precision expressed as coefficient of variation was 3.47%, 8.81%, and 1.14% and the interday precision was 5.21%, 5.48%, and 7.18%, respectively. This method is simple, uses a low blood volume for analysis, and allows reproducible and accurate measurement of fluconazole in whole blood samples from pediatric patients.

  4. Efficiency of Polyphenol Extraction from Artificial Honey Using C18 Cartridges and Amberlite® XAD-2 Resin: A Comparative Study

    OpenAIRE

    Chua Yung An; Md. Murad Hossain; Fahmida Alam; Md. Asiful Islam; Md. Ibrahim Khalil; Nadia Alam; Siew Hua Gan,

    2016-01-01

    A comparative study of the extraction efficiency of nine known polyphenols [phenolic acids (benzoic acid, dihydroxybenzoic acid, gallic acid, trans-cinnamic acid, and vanillic acid) and flavonoids (naringenin, naringin, quercetin, and rutin)] was conducted by deliberately adding the polyphenols to an artificial honey solution and performing solid phase extraction (SPE). Two SPE methods were compared: one using Amberlite XAD-2 resin and another one using a C18 cartridge. A gradient high perfor...

  5. Chromatographic finger print analysis and lysosomal membrane stabilisation activity of active fraction of Alstonia scholaris leaf extract in arthritic rats

    Directory of Open Access Journals (Sweden)

    Swapnil Goyal

    2014-01-01

    Full Text Available Object: The present study was aimed to assess the anti-arthritic activity of chloroform fraction of Alstonia scholaris leaf extract against Freund′s complete adjuvant (FCA-induced arthritis in rats. Materials and Methods: The anti-inflammatory activity of various fractions of ethanolic extract of Alstonia scholaris at concentration of 100 mg/kg was studied using the carrageenan-induced inflammatory models. The chloroform fraction shows significant anti-inflammatory activity. The chloroform fraction was further studied for anti-arthritic activity and HPTLC fingerprint analysis. For anti-arthritic activity, the active chloroform fraction was administered at the concentrations of 50 and 100 mg/kg body weight. The effect of chloroform fraction on liver ALP, ACP and LDH levels of lysosomal enzymes of FCA arthritic animals were studied. Indomethacin and prednisolone (10 mg/kg was used as standard. HPTLC studies were carried out using CAMAG HPTLC system equipped with linomat IV applicator, TLC scanner; Reprostar 3 and WIN CATS-4 software were used. Results: The chloroform fraction at 100 mg/kg, showed maximum inhibition (34.16% of inflammation induced by carrageenan. In FCA-induced arthritis, the chloroform fraction showed a highly significant reduction in paw volume (50 mg/kg-72.71%; 100 mg/kg-74.35%. The levels of lysosomal enzymes were significantly decreased in the chloroform fraction-treated groups. Conclusion: The possible mechanism of action of the chloroform fraction of Alstonia scholaris leaf extract may be through its stabilising action on lysosomal membranes. Future studies will provide new insights into the anti-arthritic activity of Alstonia scholaris and isolation of compound from it may eventually lead to development of a new class of anti-arthritic agent.

  6. Microemulsion liquid chromatographic method for simultaneous separation and determination of six flavonoids of Apocynum venetum leaf extract.

    Science.gov (United States)

    Song, Rui juan; Zhou, Jun

    2015-07-15

    A simple, cost-effective, and efficient method was developed for the rapid simultaneous separation and determination of six flavonoids (rutin, hyperoside, quercetin-3-O-sophoroside, isoquercitrin, astragalin and quercetin) of Apocynum venetum leaf extract by reversed phase high performance liquid chromatography using a microemulsion system mixture as the mobile phase. Separations were performed on the Zorbax Extend-C18 column with UV detection at 360nm. The flow rate was 0.8mLmin(-1). The optimized microemulsion mobile phase consisted of 2.5% (v/v) n-butanol, 1.2% (v/v) of Genapol X-080, 0.5% (v/v) ethyl acetate and 95.8% (w/v) of aqueous 20mM phosphoric acid, pH adjusted to 6.0 with 0.3% triethylamine. Under the optimized conditions, the calibration curve for six flavonoids was linear in the range of 5-1000μgmL(-1) with the correlation coefficients greater than 0.9994. The intra-day and inter-day precision (RSD) were below 8.11% and the limits of detection (LOD) for the six flavonoids were 1.7-6.0μgmL(-1) (S/N=3). The microemulsion liquid chromatography (MELC) method was successfully applied to separate and determine the six flavonoids of A. venetum leaf extract.

  7. Evaluation of tri-n-octylamine oxide as phenol extractant in a solvent impregnated resin

    NARCIS (Netherlands)

    Burghoff, B.; Cuypers, R.; Ettinger, van M.; Sudhölter, E.J.R.; Zuilhof, H.; Haan, de A.B.

    2009-01-01

    Tri-n-ocytlamine oxide (TOAO) is evaluated as alternative to the state-of-the-art phenol extractants tri-n-octylphosphine oxide (TOPO) and Cyanex 923. Liquid¿liquid equilibrium experiments show that TOAO in 1,3-dimethylnaphthalene achieves higher phenol distribution coefficients in an extractant con

  8. Evaluation of tri-n-octylamine oxide as phenol extractant in a solvent impregnated resin

    NARCIS (Netherlands)

    Burghoff, B.; Cuypers, R.; Ettinger, van M.; Sudhölter, E.J.R.; Zuilhof, H.; Haan, de A.B.

    2009-01-01

    Tri-n-ocytlamine oxide (TOAO) is evaluated as alternative to the state-of-the-art phenol extractants tri-n-octylphosphine oxide (TOPO) and Cyanex 923. Liquid¿liquid equilibrium experiments show that TOAO in 1,3-dimethylnaphthalene achieves higher phenol distribution coefficients in an extractant con

  9. Application of headspace sorptive extraction and gas chromatographic/mass spectrometric and chemometric methods to the quantification of pine nuts and pecorino in Pesto Genovese.

    Science.gov (United States)

    Zunin, Paola; Leardi, Riccardo; Boggia, Raffaella

    2009-01-01

    Headspace sorptive extraction and GC/MS, coupled with chemometric tools, were used to predict the amounts of pine nuts and Pecorino in Pesto Genovese, a typical Italian basil-based pasta sauce. Two groups of samples were prepared at different times and with ingredients from different batches for building the predicting models and testing their performances. Principal component analysis and partial least-squares regression (PLS) were applied to the chromatographic data. The 24 most-predictive variables were selected, and the application of PLS to the training set samples led to two models that explained approximately 70% of the variance in cross-validation, with prediction errors of 0.1 g for Pecorino and 0.6 g for pine nuts, thus confirming the reliability of the analytical method and the predicting ability of the models. The results obtained for the test set samples were not completely satisfactory, with a prediction error and a bias of 5.0 and -4.1 g, respectively, for Pecorino and corresponding values of 4.1 and 2.0 g for pine nuts. This preliminary study shows that the analytical methods used can allow construction of models with high predictive ability only if the great variability of the headspace composition of the ingredients and the effect of Twister are considered.

  10. Separation of cyclotron-produced 44Sc from a natural calcium target using a dipentyl pentylphosphonate functionalized extraction resin

    Science.gov (United States)

    Valdovinos, H.F.; Hernandez, R.; Barnhart, T.E.; Graves, S.; Cai, W.; Nickles, R.J.

    2014-01-01

    Significant interest in 44Sc as a radioactive synthon to label small molecules for positron emission tomography (PET) imaging has been recently observed. Despite the efforts of several research groups, the ideal 44Sc production and separation method remains elusive. Herein, we propose a novel separation method to obtain 44Sc from the proton irradiation of calcium targets based on extraction chromatography, which promises to greatly simplify current production methodologies. Using the commercially available Uranium and Tetravalent Actinides (UTEVA) extraction resin we were able to rapidly ( 80% of the activity generated at end of bombardment (EoB) in small ~1 M HCl fractions (400 μL). The chemical purity of the 44Sc eluates was evaluated through chelation with DOTA and DTPA, and by trace metal analysis using microwave induced plasma atomic emission spectrometry. The distribution coefficients (Kd) of Sc(III) and Ca(II) in UTEVA were determined in HCl medium in a range of concentrations from zero to 12.1 M The 44Sc obtained with our method proved to be suitable for the direct labeling of small biomolecules for PET imaging, with excellent specific activities and radiochemical purity. PMID:25464172

  11. Chromium speciation by solid phase extraction on Dowex M 4195 chelating resin and determination by atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Saygi, Kadriye Ozlem; Tuzen, Mustafa [Gaziosmanpasa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey); Soylak, Mustafa [Erciyes University, Faculty of Science and Arts, Chemistry Department, 38039 Kayseri (Turkey)], E-mail: msoylak@gmail.com; Elci, Latif [Pamukkale University, Faculty of Science and Arts, Chemistry Department, 20020 Denizli (Turkey)

    2008-05-30

    A solid phase extraction procedure has been established for chromium speciation in natural water samples prior to determination by atomic absorption spectrometry. The procedure is based on the solid phase extraction of the Cr(VI)- Dowex M 4195 chelating resin. After oxidation of Cr(III) to Cr(VI) by using H{sub 2}O{sub 2}, the presented method was applied to the determination of the total chromium. The level of Cr(III) is calculated by difference of total chromium and Cr(VI) levels. The procedure was optimized for some analytical parameters including pH, eluent type, flow rates of sample and eluent, matrix effects, etc. The presented method was applied for the speciation of chromium in natural water samples with satisfactory results (recoveries >95%, RSDs <10%). In the determinations of chromium species, flame atomic absorption spectrometer was used. The results were checked by using NIST SRM 2711 Montana soil and GBW 07603 Bush branched and leaves.

  12. Tunable aqueous polymer-phase impregnated resins-technology-a novel approach to aqueous two-phase extraction.

    Science.gov (United States)

    van Winssen, F A; Merz, J; Schembecker, G

    2014-02-14

    Aqueous Two-Phase Extraction (ATPE) represents a promising unit operation for downstream processing of biotechnological products. The technique provides several advantages such as a biocompatible environment for the extraction of sensitive and biologically active compounds. However, the tendency of some aqueous two-phase systems to form intensive and stable emulsions can lead to long phase separation times causing an increased footprint for the required mixer-settler devices or the need for additional equipment such as centrifuges. In this work, a novel approach to improve ATPE for downstream processing applications called 'Tunable Aqueous Polymer-Phase Impregnated Resins' (TAPPIR(®))-Technology is presented. The technology is based on the immobilization of one aqueous phase inside the pores of a solid support. The second aqueous phase forms the bulk liquid around the impregnated solids. Due to the immobilization of one phase, phase emulsification and phase separation of ATPE are realized in a single step. In this study, a biodegradable and sustainable aqueous two-phase system consisting of aqueous polyethylene glycol/sodiumcitrate solutions was chosen. The impregnation of different macroporous glass and ceramic solids was investigated and could be proven to be stable. Additionally, the separation of the dye Patent blue V was successfully performed with the TAPPIR(®)-Technology. Thus, the "proof of principle" of this technology is presented.

  13. Hydro-alcoholic Extract of Commiphora mukul Gum Resin May Improve Cognitive Impairments in Diabetic Rats

    Directory of Open Access Journals (Sweden)

    Salehi

    2015-02-01

    Full Text Available Background Diabetes causes cognitive impairment. Medicinal plants due to different mechanisms, such as antioxidant activities may improve diabetes and relieve its symptoms. Commiphora mukul (Burseraceae has a significant antioxidant activity. Objectives This study aimed to examine the effect of hydro- alcoholic extract of C. mukul on passive-avoidance learning and memory in streptozotocin (STZ induced diabetic male rats. Materials and Methods Thirty-two adult male Wistar rats were randomly allocated to four groups: normal, diabetic, normal + extract of C. mukul and diabetic + extract of C. mukul groups with free access to regular rat diet. Diabetes was induced in male rats by single interaperitoneal injection of 60 mg/kg STZ. After the confirmation of diabetes, 300 mg/kg C. mukul extract was orally administered to the extract-treated groups. Control groups received normal saline at the same time. Passive-avoidance memory was tested eight weeks after the STZ treatment, and blood glucose and body weight were measured in all groups at the beginning and end of the experiment. Results In the present study, diabetes decreased learning and memory. Although the administration of C. mukul extract did not affect the step-through latency (STLa and the number of trials of the diabetic groups during the first acquisition trial, a significant decrease was observed in STLr and also a significant increase in time spent in the dark compartment (TDC and number of crossing (NOC in the retention test (after 24 and 48 hours. Although no significant difference was observed in body weight of diabetic + extract of C. mukul (DE and diabetic control (DC groups, the plasma glucose of DE group was significantly lower in comparison to DC group. Conclusions Commiphora mukul extract can improve passive-avoidance learning and memory impairments in the STZ-induced diabetic rats. This improvement may be due to the antioxidant, acetylcholinesterase inhibitory activity, anti

  14. Mechanistic Study of Silver Nanoparticle's Synthesis by Dragon's Blood Resin Ethanol Extract and Antiradiation Activity.

    Science.gov (United States)

    Hasan, Murtaza; Iqbal, Javed; Awan, Umer; Saeed, Yasmeen; Ranran, Yuan; Liang, Yanli; Dai, Rongji; Deng, Yulin

    2015-02-01

    Biological synthesis of nanoparticles is best way to avoid exposure of hazardous materials as compared to chemical manufacturing process which is a severe threat not only to biodiversity but also to environment. In present study, we reported a novel method of finding antiradiation compounds by bioreducing mechanism of silver nanoparticles formation using 50% ethanol extract of Dragons blood, a famous Chinese herbal plant. Color change during silver nanoparticles synthesis was observed and it was confirmed by ultra violet (UV) visible spectroscopy at wave length at 430 nm after 30 min of reaction at 60 °C. Well dispersed round shaped silver nanoparticles with approximate size (4 nm to 50 nm) were measured by TEM and particle size analyser. Capping of biomolecules on Ag nanoparticles was characterized by FTIR spectra. HPLC analysis was carried out to find active compounds in the extract. Furthermore, antiradiation activity of this extract was tested by MTT assay in vitro after incubating the SH-SY5Y cells for 24 h at 37 °C. The results indicate that presence of active compounds in plant extract not only involves in bioreduction process but also shows response against radiation. The dual role of plant extract as green synthesis of nanoparticles and exhibit activity against radiation which gives a new way of fishing out active compounds from complex herbal plants.

  15. Accurate determination of ¹²⁹I concentrations and ¹²⁹I/¹³⁷Cs ratios in spent nuclear resins by Accelerator Mass Spectrometry.

    Science.gov (United States)

    Nottoli, Emmanuelle; Bienvenu, Philippe; Labet, Alexandre; Bourlès, Didier; Arnold, Maurice; Bertaux, Maité

    2014-04-01

    Determining long-lived radionuclide concentrations in radioactive waste has fundamental implications for the long-term management of storage sites. This paper focuses on the measurement of low (129)I contents in ion exchange resins used for primary fluid purification in Pressurised Water Reactors (PWR). Iodine-129 concentrations were successfully determined using Accelerator Mass Spectrometry (AMS) following a chemical procedure which included (1) acid digestion of resin samples in HNO3/HClO4, (2) radioactive decontamination by selective iodine extraction using a new chromatographic resin (CL Resin), and (3) AgI precipitation. Measured (129)I concentrations ranged from 4 to 12 ng/g, i.e. from 0.03 to 0.08 Bq/g. The calculation of (129)I/(137)Cs activity ratios used for routine waste management produced values in agreement with the few available data for PWR resin samples.

  16. Chromatographic Separation of Glucose and Fructose

    Science.gov (United States)

    Kuptsevich, Yu E.; Larionov, Oleg G.; Stal'naya, I. D.; Nakhapetyan, L. A.; Pronin, A. Ya

    1987-03-01

    The structures, mutarotation, and the physicochemical properties of glucose and fructose as well as methods for their separation are examined. Their chromatographic separation on cation exchangers in the calcium-form is discussed in detail. A theory of the formation of complexes of carbohydrates with metal cations is described and the mechanism of the separation of glucose and fructose on cation exchangers in the calcium-form is discussed in detail. Factors influencing the chromatographic separation of glucose and fructose on sulphonic acid cation-exchange resins are also considered. The bibliography includes 138 references.

  17. Chromatographic and Spectral Analysis of Two Main Extractable Compounds Present in Aqueous Extracts of Laminated Aluminum Foil Used for Protecting LDPE-Filled Drug Vials

    Directory of Open Access Journals (Sweden)

    Samuel O. Akapo

    2009-01-01

    Full Text Available Laminated aluminum foils are increasingly being used to protect drug products packaged in semipermeable containers (e.g., low-density polyethylene (LDPE from degradation and/or evaporation. The direct contact of such materials with primary packaging containers may potentially lead to adulteration of the drug product by extractable or leachable compounds present in the closure system. In this paper, we described a simple and reliable HPLC method for analysis of an aqueous extract of laminated aluminum foil overwrap used for packaging LDPE vials filled with aqueous pharmaceutical formulations. By means of combined HPLC-UV, GC/MS, LC/MS/MS, and NMR spectroscopy, the two major compounds detected in the aqueous extracts of the representative commercial overwraps were identified as cyclic oligomers with molecular weights of 452 and 472 and are possibly formed from poly-condensation of the adhesive components, namely, isophthalic acid, adipic acid, and diethylene glycol. Lower molecular weight compounds that might be associated with the “building blocks” of these compounds were not detected in the aqueous extracts.

  18. Effect of Green Tea Extract as Antioxidant on Shear Bond Strength of Resin Composite to in-Office and Home-Bleached Enamel.

    Science.gov (United States)

    F, Sharafeddin; F, Farshad; B, Azarian; A, Afshari

    2016-09-01

    Shear bond strength (SBS) of home and office bleached enamel will be compromised by immediate application of composite restoration. Antioxidant agent may overcome this problem. This in vitro study assessed the effect of green tea extract on shear bond strength of resin composite to in-office and home-bleached enamel. In this experimental study, 40 extracted intact human incisors were embedded in cylindrical acrylic resin blocks (2.5 ×1.5 cm), with the coronal portion above the cemento enamel junction out of the block. Then, after bleaching labial enamel surfaces of 20 teeth with 15% carbamide peroxide 6 hours a day for 5 days, they were randomly divided into two groups: A1 and A2 (n = 10), depending upon whether or not they are treated with antioxidant. Labial enamel surfaces of the remaining 20 teeth were bleached with 38% hydrogen peroxide before being randomly divided into groups B1 and B2 (n = 10), again depending on whether or not the antioxidant was used in their treatment . The experimental groups (A2,B2) were treated with 5% solution of green tea extract before resin composite restoration was done by a cylindrical Teflon mould (5×2 mm). Shear bond strength of the specimens was tested under a universal testing machine (Zwick/Roell Z020). The SBS data were analyzed by using One-way ANOVA and Tukey HSD tests (p < 0.05). There were no statistically significant differences between shear bond strength of the control group (A1) and treated group (A2), but there were statistically significant differences between the groups B1 and B2 (p < 0.05). Application of antioxidant did not increase the shear bond strength of home-bleached enamel to resin composite but its application increased the shear bond strength of in-office bleached enamel to resin composite.

  19. Effect of Green Tea Extract as Antioxidant on Shear Bond Strength of Resin Composite to in-Office and Home-Bleached Enamel

    Directory of Open Access Journals (Sweden)

    Sharafeddin F

    2016-09-01

    Full Text Available Statement of Problem: Shear bond strength (SBS of home and office bleached enamel will be compromised by immediate application of composite restoration. Antioxidant agent may overcome this problem. Objectives: This in vitro study assessed the effect of green tea extract on shear bond strength of resin composite to in-office and home-bleached enamel. Materials and Methods: In this experimental study, 40 extracted intact human incisors were embedded in cylindrical acrylic resin blocks (2.5 ×1.5 cm, with the coronal portion above the cemento enamel junction out of the block. Then, after bleaching labial enamel surfaces of 20 teeth with 15% carbamide peroxide 6 hours a day for 5 days, they were randomly divided into two groups: A1 and A2 (n = 10, depending upon whether or not they are treated with antioxidant. Labial enamel surfaces of the remaining 20 teeth were bleached with 38% hydrogen peroxide before being randomly divided into groups B1 and B2 (n = 10, again depending on whether or not the antioxidant was used in their treatment . The experimental groups (A2,B2 were treated with 5% solution of green tea extract before resin composite restoration was done by a cylindrical Teflon mould (5×2 mm. Shear bond strength of the specimens was tested under a universal testing machine (Zwick/Roell Z020. The SBS data were analyzed by using One-way ANOVA and Tukey HSD tests (p < 0.05. Results: There were no statistically significant differences between shear bond strength of the control group (A1 and treated group (A2 but there were statistically significant differences between the groups B1 and B2 (p < 0.05. Conclusions: Application of antioxidant did not increase the shear bond strength of home-bleached enamel to resin composite but its application increased the shear bond strength of in-office bleached enamel to resin composite.

  20. Sulfur geochemistry of hydrothermal waters in Yellowstone National Park, Wyoming, USA. III. An anion-exchange resin technique for sampling and preservation of sulfoxyanions in natural waters

    Science.gov (United States)

    Druschel, G.K.; Schoonen, M.A.A.; Nordstorm, D.K.; Ball, J.W.; Xu, Y.; Cohn, C.A.

    2003-01-01

    A sampling protocol for the retention, extraction, and analysis of sulfoxyanions in hydrothermal waters has been developed in the laboratory and tested at Yellowstone National Park and Green Lake, NY. Initial laboratory testing of the anion-exchange resin Bio-Rad??? AG1-X8 indicated that the resin was well suited for the sampling, preservation, and extraction of sulfate and thiosulfate. Synthetic solutions containing sulfate and thiosulfate were passed through AG1-X8 resin columns and eluted with 1 and 3 M KCl, respectively. Recovery ranged from 89 to 100%. Comparison of results for water samples collected from five pools in Yellowstone National Park between on-site IC analysis (U.S. Geological Survey mobile lab) and IC analysis of resin-stored sample at SUNY-Stony Brook indicates 96 to 100% agreement for three pools (Cinder, Cistern, and an unnamed pool near Cistern) and 76 and 63% agreement for two pools (Sulfur Dust and Frying Pan). Attempts to extract polythionates from the AG1-X8 resin were made using HCl solutions, but were unsuccessful. Bio-Rad??? AG2-X8, an anion-exchange resin with weaker binding sites than the AG1-X8 resin, is better suited for polythionate extraction. Sulfate and thiosulfate extraction with this resin has been accomplished with KCl solutions of 0.1 and 0.5 M, respectively. Trithionate and tetrathionate can be extracted with 4 M KCl. Higher polythionates can be extracted with 9 M hydrochloric acid. Polythionate concentrations can then be determined directly using ion chromatographic methods, and laboratory results indicate recovery of up to 90% for synthetic polythionate solutions using AG2-X8 resin columns. ?? The Royal Society of Chemistry and the Division of Geochemistry of the American Chemical Society 2003.

  1. Sulfur geochemistry of hydrothermal waters in Yellowstone National Park, Wyoming, USA. III. An anion-exchange resin technique for sampling and preservation of sulfoxyanions in natural waters

    Directory of Open Access Journals (Sweden)

    Ball James W

    2003-06-01

    Full Text Available A sampling protocol for the retention, extraction, and analysis of sulfoxyanions in hydrothermal waters has been developed in the laboratory and tested at Yellowstone National Park and Green Lake, NY. Initial laboratory testing of the anion-exchange resin Bio-Rad™ AG1-X8 indicated that the resin was well suited for the sampling, preservation, and extraction of sulfate and thiosulfate. Synthetic solutions containing sulfate and thiosulfate were passed through AG1-X8 resin columns and eluted with 1 and 3 M KCl, respectively. Recovery ranged from 89 to 100%. Comparison of results for water samples collected from five pools in Yellowstone National Park between on-site IC analysis (U.S. Geological Survey mobile lab and IC analysis of resin-stored sample at SUNY-Stony Brook indicates 96 to 100% agreement for three pools (Cinder, Cistern, and an unnamed pool near Cistern and 76 and 63% agreement for two pools (Sulfur Dust and Frying Pan. Attempts to extract polythionates from the AG1-X8 resin were made using HCl solutions, but were unsuccessful. Bio-Rad™ AG2-X8, an anion-exchange resin with weaker binding sites than the AG1-X8 resin, is better suited for polythionate extraction. Sulfate and thiosulfate extraction with this resin has been accomplished with KCl solutions of 0.1 and 0.5 M, respectively. Trithionate and tetrathionate can be extracted with 4 M KCl. Higher polythionates can be extracted with 9 M hydrochloric acid. Polythionate concentrations can then be determined directly using ion chromatographic methods, and laboratory results indicate recovery of up to 90% for synthetic polythionate solutions using AG2-X8 resin columns.

  2. A rapid, solid phase extraction (SPE technique for the extraction and gas chromatographic determination lindane pesticide residue in tissue and milk

    Directory of Open Access Journals (Sweden)

    Yuningsih

    2006-03-01

    Full Text Available Organochlorine pesticide contamination in feed can cause residue in animal product (tissue and milk, so its become a problem in food safety. Solid phase extraction (SPE has been carried out for determination organochlorine pesticide residues in food animal production. The technique was rapid, not costly and produce limited amount of hazardous-waste. Samples were homogenized with acetonitrile trough cartridge C18, eluted in fluorocyl column with 2% ether-petroleum or acetonitrile fortissue and milk samples respectively. The recoveries of tissue sample by addition lindane standard solution: 0.50 and 1.00 μg are 85.10 and 103.10% respectively, while that of milk with the addition of 0.50, 1.00 and 1.50 μg are 83.80, 88.69 and 91.24% respectively. Three replicates were carried out for every sample. According of validation criteria of FAO/IAEA the recovery for analysis of pesticide residues was 70-110%. Therefore, the method is applicable.

  3. Rapid and simultaneous determination of neptunium and plutonium isotopes in environmental samples by extraction chromatography using sequential injection analysis and ICP-MS

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per

    2010-01-01

    This paper reports an automated analytical method for rapid and simultaneous determination of plutonium isotopes (239Pu and 240Pu) and neptunium (237Np) in environmental samples. An extraction chromatographic column packed with TrisKem TEVA® resin was incorporated in a sequential injection (SI...

  4. Process for purification of monoclonal antibody expressed in transgenic Lemna plant extract using dextran-coated charcoal and hexamer peptide affinity resin.

    Science.gov (United States)

    Naik, Amith D; Menegatti, Stefano; Reese, Hannah R; Gurgel, Patrick V; Carbonell, Ruben G

    2012-10-19

    The production of therapeutic proteins using transgenic plants offers several advantages, including low production cost, absence of human pathogens, presence of glycosylation mechanisms, and the ability to fold complex therapeutic proteins into their proper conformation. However, impurities such as phenolic compounds and pigments encountered during purification are quite different from those faced during purification from mammalian cell culture supernatants. This paper deals with the development of a pretreatment and affinity separation process for the purification of a monoclonal antibody from transgenic Lemna plant extract. A pretreatment step is described using dextran-coated charcoal for the removal of pigments and phenolic compounds without reducing the antibody concentration. Then, the peptide affinity ligand HWRGWV coupled to a commercial polymethacrylate resin is used for the capture and purification of MAb from the pretreated plant extract. The final yield and purity of the MAb obtained were 90% and 96% respectively. The performance of the hexamer peptide resin after the pretreatment step was found to be similar to that obtained with a commercial Protein A resin.

  5. 21 CFR 862.2230 - Chromatographic separation material for clinical use.

    Science.gov (United States)

    2010-04-01

    ... chromatographic separation material for clinical use is a device accessory (e.g., ion exchange absorbents, ion exchagne resins, and ion papers) intended for use in ion exchange chromatography, a procedure in which...

  6. Determination of oil reservoir radiotracer (S{sup 14}CN{sup -}) in a single step using a plastic scintillator extractive resin

    Energy Technology Data Exchange (ETDEWEB)

    Bagan, H.; Tarancon, A. [Departament de Quimica Analitica, Universitat de Barcelona, Diagonal 645, E-08028 Barcelona (Spain); Stavsetra, L. [Department for Reservoir and Exploration Technology, Institute for Energy Technology (IFE), Instituttveien 18, N-2027 Kjeller (Norway); Rauret, G. [Departament de Quimica Analitica, Universitat de Barcelona, Diagonal 645, E-08028 Barcelona (Spain); Garcia, J.F., E-mail: jfgarcia@ub.edu [Departament de Quimica Analitica, Universitat de Barcelona, Diagonal 645, E-08028 Barcelona (Spain)

    2012-07-29

    Highlights: Black-Right-Pointing-Pointer A new procedure for S{sup 14}CN{sup -} radiotracer determination using PS resin was established. Black-Right-Pointing-Pointer The minimum detectable activity for a 100 mL sample is 0.08 Bq L{sup -1}. Black-Right-Pointing-Pointer The minimum quantifiable activity for a 100 mL sample is 0.31 Bq L{sup -1}. Black-Right-Pointing-Pointer PS resin is capable to quantify S{sup 14}CN{sup -} radiotracer samples with errors lower than 5%. Black-Right-Pointing-Pointer PS resin is also capable to quantify complex matrices obtained from oil reservoirs. - Abstract: The analysis of radiotracers is important in the study of oil reservoir dynamics. One of the most widely used radiotracer is S{sup 14}CN{sup -}. Prior to activity measurements by Liquid Scintillation (LS), routine determinations require the pretreatment steps of purification and concentration of the samples using anion exchange columns. The final elution media produces samples with high salt concentration that may lead to problems with phase separation during the LS measurement. Plastic Scintillation (PS) is an alternative technique that provides a solid surface that can be used as a platform for the immobilisation of selective extractants to obtain a PS resin. The proposed procedure unifies chemical separation and sample measurement preparation in a single step, serving to reduce the number of reagents needed and manpower required for the analysis while also avoiding mixed waste production by LS. The objective of this study is to develop a PS resin for the determination of {sup 14}C-labelled thiocyanate radiotracer in water samples. For this purpose, the immobilisation procedure was optimised, including optimisation of the proportion of PS microspheres:extractant and the use of a control blank to monitor the PS resin immobilisation process. The breakthrough volume was studied and the detection and quantification limits for 100 mL of sample were determined to be 0.08 Bq L{sup -1

  7. Release and protein binding of components from resin based composites in native saliva and other extraction media.

    Science.gov (United States)

    Rothmund, Lena; Shehata, Mostafa; Van Landuyt, Kirsten L; Schweikl, Helmut; Carell, Thomas; Geurtsen, Werner; Hellwig, Elmar; Hickel, Reinhard; Reichl, Franz-Xaver; Högg, Christof

    2015-05-01

    Unpolymerized (co)monomers and additives can be released from resin based composites (RBCs) and can enter the human organism. In this study, the binding of ingredients from composites to salivary proteins and plasma proteins was investigated. The composites investigated were Admira(®) flow, Venus(®) Diamond flow, Filtek™ Supreme XTE flow, Tetric EvoCeram(®), Tetric EvoFlow(®). The samples (n=4) were polymerized according to the instructions of the manufacturer of RBCs. The samples were immersed into native saliva, protein-free saliva (artificial saliva), water and ethyl acetate, and incubated at 37°C for 24h or 72h. The eluates were analyzed by gas chromatography/mass spectrometry. To determine the binding to salivary proteins, the concentration of (co)monomers and additives detected in native saliva was compared to the concentration of (co)monomers and additives detected in protein-free saliva, water and ethyl acetate respectively. To assess the affinity of TEGDMA, EGDMA, DEGDMA, PMGDMA, BPA, and DCHP to human serum albumin (HSA) and human α1-acid glycoprotein (AGP), a plasma protein binding assay (ABNOVA, Transil XL PPB Prediction Kit TMP-0212-2096) was performed. The statistical significance (psaliva was significantly lower than the concentration released in protein-free saliva or water (Admira(®) flow: concentration of TEGDMA after 72h: 0.08 mmol/L (native saliva), 0.34 mmol/L (protein-free saliva), 0.39 mmol/L (water)). The concentrations of HEMA, EGDMA, DDDMA and CQ released in native saliva remained even below the detection limit, compared to the other extraction media. Protein binding of the tested methacrylates to HSA+AGP was 82-85%, the binding of DCHP was 96.6%, and the binding of BPA was 95.2%. Artificial saliva or water as extraction medium does not reflect the real physiological situation in the body. Salivary and plasma proteins may bind (co)monomers and additives and may thereby contribute to a lower bioavailability of leachables from RBCs

  8. Phosphorus extracted by ion exchange resins and mehlich-1 from oxisols (latosols treated with different phosphorus rates and sources for varied soil-source contact periods

    Directory of Open Access Journals (Sweden)

    Irio Fernando de Freitas

    2013-06-01

    Full Text Available Despite the large number of studies addressing the quantification of phosphorus (P availability by different extraction methods, many questions remain unanswered. The aim of this paper was to compare the effectiveness of the extractors Mehlich-1, Anionic Resin (AR and Mixed Resin (MR, to determine the availability of P under different experimental conditions. The laboratory study was arranged in randomized blocks in a [(3 x 3 x 2 + 3] x 4 factorial design, with four replications, testing the response of three soils with different texture: a very clayey Red Latosol (LV, a sandy clay loam Red Yellow Latosol (LVA, and a sandy loam Yellow Latosol (LA, to three sources (triple superphosphate, reactive phosphate rock from Gafsa-Tunisia; and natural phosphate from Araxá-Minas Gerais at two P rates (75 and 150 mg dm-3, plus three control treatments (each soil without P application after four contact periods (15, 30, 60, and 120 days of the P sources with soil. The soil acidity of LV and LVA was adjusted by raising base saturation to 60 % with the application of CaCO3 and MgCO3 at a 4:1 molar ratio (LA required no correction. These samples were maintained at field moisture capacity for 30 days. After the contact periods, the samples were collected to quantify the available P concentrations by the three extractants. In general, all three indicated that the available P-content in soils was reduced after longer contact periods with the P sources. Of the three sources, this reduction was most pronounced for triple superphosphate, intermediate for reactive phosphate, while Araxá phosphate was least sensitive to the effect of time. It was observed that AR extracted lower P levels from all three soils when the sources were phosphate rocks, while MR extracted values close to Mehlich-1 in LV (clay and LVA (medium texture for reactive phosphate. For Araxá phosphate, much higher P values were determined by Mehlich-1 than by the resins, because of the acidity of

  9. Determination of some trace metals by FAAS after solid-phase extraction with amberlite XAD-1180/TAN chelating resin.

    Science.gov (United States)

    Yilmaz, Vedat; Kartal, Senol

    2012-01-01

    A new chelating resin was synthesized by immobilizing 1-(2-thiazolylazo)-2-naphthol through the -N=N- group on Amberlite XAD-1180. The resin was used for the preconcentration of Cd(II), Co(II), Cu(II), Mn(II), Ni(II), and Pb(II) ions and their determination by flame atomic absorption spectrometry (FAAS). The influences of some analytical parameters, such as the pH, volume of the sample, flow rates of the sample and eluent, matrix components, amount of the resin, and amount and type of the eluent on the recovery, were investigated. Those metals retained on the resin at pH 8.5 were eluted with 25 mL of 2 mol L(-1) HNO(3). The sorption capacity of the resin was determined, except for Pb(II). The recoveries were found to be ≥95%, and the relative standard-deviation values were ≤4.3%. The detection limits were in the range of 0.1 - 3.6 µg L(-1). For the accuracy of the method, the analysis of a certified reference material was performed. This method was applied to environmental water samples.

  10. Application of mixed mode resins for the purification of antibodies.

    Science.gov (United States)

    Voitl, Agnes; Müller-Späth, Thomas; Morbidelli, Massimo

    2010-09-10

    The downstream processing of monoclonal antibodies from cell culture supernatant is usually done by a number of chromatographic and non-chromatographic steps. Efforts are taken to reduce the costs associated to those steps, while maintaining a high product purity. A possibility to reach this goal is the reduction of the number of chromatographic steps using mixed mode resins that offer more than one functionality in one chromatographic step. In this work, a commercially available mixed mode resin was evaluated systematically with respect to the adsorption of proteins. The Henry coefficient, which quantifies the adsorption strength, was measured for the full working range of the stationary phase as a function of the salt concentration and the pH. The results were compared to a conventional anion exchange and a hydrophobic interaction resin. Furthermore, the resin was applied for the polishing step of an antibody from an industrial clarified cell culture supernatant.

  11. Pre-Harvest Dropped Kinnow ( Citrus reticulata Blanco) Waste Management through the Extraction of Naringin and Pectin from their Peels using Indigenous Resin

    Science.gov (United States)

    Laxmi Deepak Bhatlu, M.; Katiyar, Prashant; Singh, Satya Vir; Verma, Ashok Kumar

    2016-09-01

    About 10-20 % kinnow fruits are dropped in preharvest stage which are waste and are problem to farmer as these create nuisance by rotting and insect rearing ground. The peels of these dropped fruits as well as peels from kinnow processing may be good source of naringin and pectin. Naringin is used in pharmaseutics while pectin is used in food industry. For recovery of naringin and pectn, peels of preharvest dropped kinnow fruits were boiled in water. The extract was passed through macroporus polymeric adsorbent resin Indion PA 800, naringin was adsorbed on it. The adsorbed naringin was desorbed with ethanol. This solution was passed through membrane filter and filtrate was evaporated to obtain naringin. The extract remaining after adsorption of naringin was used to recover pectin using acid extraction method. The recovery of naringin and pectin was about 52 and 58 % respectively. The naringin finally obtained had 91-93 % purity.

  12. Pre-Harvest Dropped Kinnow (Citrus reticulata Blanco) Waste Management through the Extraction of Naringin and Pectin from their Peels using Indigenous Resin

    Science.gov (United States)

    Laxmi Deepak Bhatlu, M.; Katiyar, Prashant; Singh, Satya Vir; Verma, Ashok Kumar

    2016-09-01

    About 10-20 % kinnow fruits are dropped in preharvest stage which are waste and are problem to farmer as these create nuisance by rotting and insect rearing ground. The peels of these dropped fruits as well as peels from kinnow processing may be good source of naringin and pectin. Naringin is used in pharmaseutics while pectin is used in food industry. For recovery of naringin and pectn, peels of preharvest dropped kinnow fruits were boiled in water. The extract was passed through macroporus polymeric adsorbent resin Indion PA 800, naringin was adsorbed on it. The adsorbed naringin was desorbed with ethanol. This solution was passed through membrane filter and filtrate was evaporated to obtain naringin. The extract remaining after adsorption of naringin was used to recover pectin using acid extraction method. The recovery of naringin and pectin was about 52 and 58 % respectively. The naringin finally obtained had 91-93 % purity.

  13. Solid phase extraction of chromium(VI) from aqueous solutions by adsorption of its diphenylcarbazide complex on an Amberlite XAD-4 resin column.

    Science.gov (United States)

    Rajesh, N; Jalan, Rohit Kumar; Hotwany, Pinky

    2008-02-11

    A method has been developed for the solid phase extraction of chromium(VI) based on the adsorption of its diphenylcarbazide complex on an Amberlite XAD-4 resin column. The influence of acidity, stability of the column, sample volume, flow rate and interfering ions were studied in detail. The adsorbed complex could be eluted using acetone-sulfuric acid mixture and the concentration of chromium was determined using visible spectrophotometry. A detection limit of 6 microg L(-1) could be achieved. A preconcentration factor of 27 could be obtained for 400 mL sample volume. The validity of the method was checked in spiked water samples and electroplating wastewater.

  14. Industrial scale chromatographic separation of valuable compounds from biomass hydrolysates and side streams

    Energy Technology Data Exchange (ETDEWEB)

    Saari, P.

    2011-06-15

    Carbohydrates are composed of a number of various monosaccharides, glucose being the most abundant. Some of the monosaccharides are valuable compounds used in the food and pharmaceutical industries. They can be separated from biomass hydrolysates e.g. by chromatographic methods. In this thesis, chromatographic separation of valuable compounds using ion exchange resins was studied on an industrial scale. Of special interest were rare monosaccharides in biomass hydrolysates. A novel chromatographic separation process was developed for fucose, starting from pre-processed spent sulfite liquor. The core of the process consists of three chromatographic separations with different types of ion exchange resins. Chromatographic separation of galactose was tested with three biomass hydrolysates; lactose, gum arabic and hemicellulose hydrolysates. It was demonstrated that also galactose can be separated from complex carbohydrate mixtures. A recovery process for arabinose from citrus pectin liquid residual and for mannose from wood pulp hydrolysate were also developed and experimentally verified. In addition to monosaccharides, chromatographic separation of glycinebetaine from vinasse was examined with a hydrogen form weak acid cation exchange resin. The separation involves untypical peak formation depending, for example, on the pH and the cation composition. The retention mechanism was found to be hydrogen bonding between glycinebetaine and the resin. In the experimental part, all four resin types - strong acid cation, strong base anion, weak acid cation and weak base anion exchange resins - were used. In addition, adsorption equilibria data of seven monosaccharides and sucrose were measured with the resins in sodium and sulfate forms because such data have been lacking. It was found out that the isotherms of all sugars were linear under industrial conditions. A systematic method for conceptual process design and sequencing of chromatographic separation steps were developed

  15. Final report on the safety assessment of capsicum annuum extract, capsicum annuum fruit extract, capsicum annuum resin, capsicum annuum fruit powder, capsicum frutescens fruit, capsicum frutescens fruit extract, capsicum frutescens resin, and capsaicin.

    Science.gov (United States)

    2007-01-01

    Capsicum-derived ingredients function as skin-conditioning agents--miscellaneous, external analgesics, flavoring agents, or fragrance components in cosmetics. These ingredients are used in 19 cosmetic products at concentrations as high as 5%. Cosmetic-grade material may be extracted using hexane, ethanol, or vegetable oil and contain the full range of phytocompounds that are found in the Capsicum annuum or Capsicum frutescens plant (aka red chiles), including Capsaicin. Aflatoxin and N-nitroso compounds (N-nitrosodimethylamine and N-nitrosopyrrolidine) have been detected as contaminants. The ultraviolet (UV) absorption spectrum for Capsicum Annuum Fruit Extract indicates a small peak at approximately 275 nm, and a gradual increase in absorbance, beginning at approximately 400 nm. Capsicum and paprika are generally recognized as safe by the U.S. Food and Drug Administration for use in food. Hexane, chloroform, and ethyl acetate extracts of Capsicum Frutescens Fruit at 200 mg/kg resulted in death of all mice. In a short-term inhalation toxicity study using rats, no difference was found between vehicle control and a 7% Capsicum Oleoresin solution. In a 4-week feeding study, red chilli (Capsicum annuum) in the diet at concentrations up to 10% was relatively nontoxic in groups of male mice. In an 8-week feeding study using rats, intestinal exfoliation, cytoplasmic fatty vacuolation and centrilobular necrosis of hepatocytes, and aggregation of lymphocytes in the portal areas were seen at 10% Capsicum Frutescens Fruit, but not 2%. Rats fed 0.5 g/kg day-1 crude Capsicum Fruit Extract for 60 days exhibited no significant gross pathology at necropsy, but slight hyperemia of the liver and reddening of the gastric mucosa were observed. Weanling rats fed basal diets supplemented with whole red pepper at concentrations up to 5.0% for up to 8 weeks had no pathology of the large intestines, livers, and kidneys, but destruction of the taste buds and keratinization and erosion of

  16. Solid Phase Extraction and Determination of Nickel in Water Samples by Using Novel Thiol-Containing Sulfonamide Polymeric Resin and Atomic Absorption Spectrophotometer

    Institute of Scientific and Technical Information of China (English)

    Nagihan M Karaaslan; B Filiz Senkal; Cigdem Er; Halim Avci; Mehmet Yaman

    2011-01-01

    Interest in preconcentration techniques for the determination of metals at ultratrace levels still continues increasingly because of some disadvantages of flameless atomic absorption spectrometry as well as the high costs of other sensitive methods in compared to flame atomic absorption spectrometry.In this study,thiol-containing sulfonamide resin was synthesized,characterized and applied as a new sorption material for solid phase extraction of nickel in drinking water samples.After preconcentration procedure,flame atomic absorption spectrometry was used for determinations.Optimum parameters were found to be pH=3.2,contact time =20 min and eluate volume=3 mL.The limit of detection was found to be 0.75 ng · mL-1.The synthesized resin exhibits the superiority in compared to the other adsorption reagents because of the fact that there is no necessity of any complexing reagent,high sorption capacity as well as the relatively fast extraction rate.The Ni concentrations in the studied 21 kind of water samples were found to be in the range of BDL-4.0 ng ·mL-1.

  17. Improvement of skin condition in striae distensae: development, characterization and clinical efficacy of a cosmetic product containing Punica granatum seed oil and Croton lechleri resin extract

    Science.gov (United States)

    Bogdan, Cătălina; Iurian, Sonia; Tomuta, Ioan; Moldovan, Mirela

    2017-01-01

    Striae distensae are a frequent skin condition associated with pregnancy, weight change or lack of skin elasticity. The aim of this research was to obtain a topical product containing herbal active ingredients with documented antioxidant and anti-inflammatory activity (Punica granatum seed oil and Croton lechleri resin extract) and demonstrate its positive effect on prevention and treatment of striae distensae. First, the cream base formulation was optimized through experimental design. Secondly, the cream containing the two active ingredients was investigated in an interventional nonrandomized clinical trial. The clinical outcome was assessed through biophysical parameters and ultrasonographic evaluation. The state of the skin was evaluated by biophysical measurements and ultrasonography at the beginning of the study and after 3 and 6 weeks. The experimental design was successfully used to set the best ranges for the technological and formulation factors to obtain a cosmetic formulation with optimal characteristics. The study of clinical efficacy on the optimal formulation revealed an increase in the dermis thickness, hydration and elasticity values in both groups after 6 weeks of cream application. The new oil-in-water cream containing P. granatum seed oil and C. lechleri resin extract can be helpful in the prevention or improving of skin changes associated with striae. PMID:28280300

  18. Azocalix[4]pyrrole Amberlite XAD-2: new polymeric chelating resins for the extraction, preconcentration and sequential separation of Cu(II), Zn(II) and Cd(II) in natural water samples.

    Science.gov (United States)

    Jain, Vinod K; Mandalia, Hiren C; Gupte, Hrishikesh S; Vyas, Disha J

    2009-10-15

    Two novel azocalix[4]pyrrole Amberlite XAD-2 polymeric chelating resins were synthesized by covalently linking diazotized Amberlite XAD-2 with calix[4]pyrrole macrocycles. The chelating resins were used for extraction, preconcentration and sequential separation of metal ions such as Cu(II), Zn(II) and Cd(II) by column chromatography prior to their determination by UV/vis spectrophotometry or flame atomic absorption spectrophotometry (FAAS) or inductively coupled plasma atomic emission spectroscopy (ICP-AES). Various parameters such as effect of pH on absorption, concentration of eluting agents, flow rate, total sorption capacity, exchange kinetics, preconcentration factor, distribution coefficient, breakthrough capacity and resin stability, were optimized for effective separation and preconcentration. The resin showed good ability for the separation of metal ions from binary and ternary mixture on the basis of pH of absorption and concentration of eluting agents. The newly synthesized resins showed good potential for trace enrichment of Cu(II), Zn(II) and Cd(II) metal ions, especially for Cu(II), as compared to the earlier reported resins. The synthesized resins were recycled at least 8-10 times without much affecting column sorption capacity. The presented method was successfully applied for determination of Cu(II), Zn(II) and Cd(II) in natural and ground water samples.

  19. Economic analysis of uricase production under uncertainty: Contrast of chromatographic purification and aqueous two-phase extraction (with and without PEG recycle).

    Science.gov (United States)

    Torres-Acosta, Mario A; Aguilar-Yáñez, José M; Rito-Palomares, Marco; Titchener-Hooker, Nigel J

    2016-01-01

    Uricase is the enzyme responsible for the breakdown of uric acid, the key molecule leading to gout in humans, into allantoin, but it is absent in humans. It has been produced as a PEGylated pharmaceutical where the purification is performed through three sequential chromatographic columns. More recently an aqueous two-phase system (ATPS) was reported that could recover Uricase with high yield and purity. Although the use of ATPS can decrease cost and time, it also generates a large amount of waste. The ability, therefore, to recycle key components of ATPS is of interest. Economic modelling is a powerful tool that allows the bioprocess engineer to compare possible outcomes and find areas where further research or optimization might be required without recourse to extensive experiments and time. This research provides an economic analysis using the commercial software BioSolve of the strategies for Uricase production: chromatographic and ATPS, and includes a third bioprocess that uses material recycling. The key parameters that affect the process the most were located via a sensitivity analysis and evaluated with a Monte Carlo analysis. Results show that ATPS is far less expensive than chromatography, but that there is an area where the cost of production of both bioprocesses overlap. Furthermore, recycling does not impact the cost of production. This study serves to provide a framework for the economic analysis of Uricase production using alternative techniques.

  20. Chelating resin-based extraction of DNA from dental pulp and sex determination from incinerated teeth with Y-chromosomal alphoid repeat and short tandem repeats.

    Science.gov (United States)

    Tsuchimochi, Tsukasa; Iwasa, Mineo; Maeno, Yoshitaka; Koyama, Hiroyoshi; Inoue, Hiroyuki; Isobe, Ichiro; Matoba, Ryoji; Yokoi, Motoo; Nagao, Masataka

    2002-09-01

    A procedure utilizing Chelex 100, chelating resin, was adapted to extract DNA from dental pulp. The procedure was simple and rapid, involved no organic solvents, and did not require multiple tube transfers. The extraction of DNA from dental pulp using this method was as efficient, or more so, than using proteinase K and phenol-chloroform extraction. In this study, the Chelex method was used with amplification and typing at Y-chromosomal loci to determine the effects of temperature on the sex determination of the teeth. The extracted teeth were incinerated in a dental furnace for 2 minutes at 100 degrees C, 200 degrees C, 300 degrees C, 400 degrees C, and 500 degrees C. After the isolation of DNA from the dental pulp by the Chelex method, alphoid repeats, and short tandem repeats, the human Y chromosome (DYZ3), DYS19, SYS389, DYS390, and DYS393 could be amplified and typed in all samples incinerated at up to 300 degrees C for 2 minutes. The DYS389 locus in some samples could not be amplified at 300 degrees C for 2 minutes. An autopsy case is described in which genotypings of DYS19, DYS390, and DYS393 from dental pulp obtained from a burned body were needed. The data presented in this report suggest that Chelex 100-based DNA extraction, amplification, and typing are possible in burned teeth in forensic autopsy cases.

  1. Determination of distribution coefficients (K{sub d}) of various radionuclides on UTEVA resin

    Energy Technology Data Exchange (ETDEWEB)

    Marinov, Genko M.; Marinova, Atanaska P. [Joint Institute for Nuclear Research, DLNP, Dubna (Russian Federation); Sofia Univ. (Bulgaria). Faculty of Chemistry and Pharmacy; Medvedev, Dmitry V.; Filosofov, Dmitry V. [Joint Institute for Nuclear Research, DLNP, Dubna (Russian Federation); Dadakhanov, Jahangir A. [Joint Institute for Nuclear Research, DLNP, Dubna (Russian Federation); AS RUz, Tashkent (Uzbekistan). Inst. of Nuclear Physics; Milanova, Maria M. [Sofia Univ. (Bulgaria). Faculty of Chemistry and Pharmacy; Happel, Steffen [Triskem International, Bruz (France); Radchenko, Valery I. [Mainz Univ. (Germany)

    2016-07-01

    Using radioisotope markers the distribution coefficients (K{sub d}) of the following elements In, Sn, Sb, Te, Bi, Co, Fe, Nb, Sr, Ba, Ag, Cd, Zr, Hf and Ti were determined with different concentrations of HCl, H{sub 2}SO{sub 4} and HNO{sub 3} for the extraction chromatographic resin Uranium and TEtraValent Actinides (UTEVA). This data can be used for separation of elements in complex mixtures, as well as for correct assessment of the elements chemistry with higher valences such as 3, 4, 5 or 6.

  2. Biobased carbon content of resin extracted from polyethylene composite by carbon-14 concentration measurements using accelerator mass spectrometry

    OpenAIRE

    Taguchi, Kazuhiro; Kunioka, Masao; Funabashi, Masahiro; Ninomiya, Fumi

    2014-01-01

    An estimation procedure for biobased carbon content of polyethylene composite was studied using carbon-14 (14C) concentration ratios as measured by accelerated mass spectrometry (AMS). Prior to the measurement, additives and fillers in composites should be removed because they often contain a large amount of biobased carbon and may shift the estimation. Samples of resin with purity suitable for measurement were isolated from composites with a Soxhlet extractor using heated cyclohexanone. Afte...

  3. Ionic Liquid-Based Vacuum Microwave-Assisted Extraction Followed by Macroporous Resin Enrichment for the Separation of the Three Glycosides Salicin, Hyperin and Rutin from Populus Bark

    Directory of Open Access Journals (Sweden)

    Fengli Chen

    2014-07-01

    Full Text Available An effective ionic liquid vacuum microwave-assisted method was developed for extraction of the thermo- and oxygen-sensitive glycosides salicin, hyperin and rutin from Populus bark due to the strong solvating effects of ionic liquids on plant cell walls. In this study, [C4mim]BF4 solution was selected as the extracting solution for extraction of the target analytes. After optimization by single factor experiments and response surface methodology, the optimum condition parameters were achieved, which included 1.0 M [C4mim]BF4, 2 h soaking time, −0.08 MPa vacuum, 20 min microwave irradiation time, 400 W microwave irradiation power and 25 mL/g liquid/solid ratio. Under the optimum conditions, higher extraction yields of salicin (35.53 mg/g, hyperin (1.32 mg/g and rutin (2.40 mg/g were obtained. Compared with other extraction methods, the developed method provided higher yields of the three target components after a relatively shorter extraction time (20 min. No obvious degradation of the target analytes was observed under the optimum conditions in performed stability studies and the proposed method had a high reproducibility. Meanwhile, after adsorption and desorption on macroporous D101 resin, the target analytes can be effectively separated from the [C4mim]BF4 ionic liquid extraction solution and the yields of salicin, hyperin and rutin were 89%, 82% and 84%, respectively. The recovered [C4mim]BF4 ionic liquid presented a good extraction effect on the three analytes after recycling five times.

  4. Ionic liquid-based vacuum microwave-assisted extraction followed by macroporous resin enrichment for the separation of the three glycosides salicin, hyperin and rutin from Populus bark.

    Science.gov (United States)

    Chen, Fengli; Mo, Kailin; Liu, Zhaizhi; Yang, Fengjian; Hou, Kexin; Li, Shuangyang; Zu, Yuangang; Yang, Lei

    2014-07-07

    An effective ionic liquid vacuum microwave-assisted method was developed for extraction of the thermo- and oxygen-sensitive glycosides salicin, hyperin and rutin from Populus bark due to the strong solvating effects of ionic liquids on plant cell walls. In this study, [C4mim]BF4 solution was selected as the extracting solution for extraction of the target analytes. After optimization by single factor experiments and response surface methodology, the optimum condition parameters were achieved, which included 1.0 M [C4mim]BF4, 2 h soaking time, -0.08 MPa vacuum, 20 min microwave irradiation time, 400 W microwave irradiation power and 25 mL/g liquid/solid ratio. Under the optimum conditions, higher extraction yields of salicin (35.53 mg/g), hyperin (1.32 mg/g) and rutin (2.40 mg/g) were obtained. Compared with other extraction methods, the developed method provided higher yields of the three target components after a relatively shorter extraction time (20 min). No obvious degradation of the target analytes was observed under the optimum conditions in performed stability studies and the proposed method had a high reproducibility. Meanwhile, after adsorption and desorption on macroporous D101 resin, the target analytes can be effectively separated from the [C4mim]BF4 ionic liquid extraction solution and the yields of salicin, hyperin and rutin were 89%, 82% and 84%, respectively. The recovered [C4mim]BF4 ionic liquid presented a good extraction effect on the three analytes after recycling five times.

  5. Feasibility of the direct coupling of solid-phase extraction-pipette tips with a programmed-temperature vaporiser for gas chromatographic analysis of drugs in plasma

    NARCIS (Netherlands)

    van Hout, M.W J; van Egmond, W.M A; Franke, J.P.; de Zeeuw, R.A; de Jong, G.J.

    2002-01-01

    Solid-phase extraction-pipette tips (SPE-PTs) were used for micro solid-phase extraction of lidocaine and diazepam from plasma. Off-line extraction was followed by on-line desorption. On-line desorption was carried out by direct coupling of the SPE-PTs with the liner of the programmed-temperature va

  6. Radiotoxicological analyses of {sup 239+240}Pu and {sup 241}Am in biological samples by anion-exchange and extraction chromatography: a preliminary study for internal contamination evaluations

    Energy Technology Data Exchange (ETDEWEB)

    Ridone, S.; Arginelli, D.; Bortoluzzi, S.; Canuto, G.; Montalto, M.; Nocente, M.; Vegro, M. [Italian National Agency for New Technologies, Energy and the Environment (ENEA), Research Centre of Saluggia, Radiation Protection Institute, Saluggia, VC (Italy)

    2006-07-01

    Many biological samples (urines and faeces) have been analysed by means of chromatographic extraction columns, utilising two different resins (AG 1-X2 resin chloride and T.R.U.), in order to detect the possible internal contamination of {sup 239{sup +}}{sup 240}Pu and {sup 241}Am, for some workers of a reprocessing nuclear plant in the decommissioning phase. The results obtained show on one hand the great suitability of the first resin for the determination of plutonium, and on the other the great selectivity of the second one for the determination of americium.

  7. Micro-column solid phase extraction to determine uranium and thorium in environmental samples.

    Science.gov (United States)

    Tsai, Tsuey-Lin; Lin, Chun-Chih; Chu, Tieh-Chi

    2008-08-01

    Extraction chromatographic separation techniques based on U/TEVA and TEVA resins were utilized to separate uranium and thorium isotopes in complex matrices from environmental samples. This approach has the advantages of ease of quantitative analysis, small sample size, an absence of mixed waste solvents, complete separation of U/Th isotopes, acceptable chemical yields and good energy resolution in the alpha spectrum. The procedure for analyzing alpha-emitting isotopes of uranium and thorium in geothermal water from Peito, Taiwan, is illustrated in detail. It involves sample pre-concentration, filtration and separation by highly selective extraction chromatographic resins, followed by electroplating and alpha-spectroscopy. The analytical results show a chemical recovery exceeding 55% for U and 65% for Th, respectively, under optimized conditions. The efficient and cost-effective use of recyclable columns makes the analytical methods simple, accurate, rapid, reliable and robust.

  8. 萃取色谱法分离实际样品及伴生元素中的铂(Ⅳ)元素%Extraction chromatographic separation of platinum(Ⅳ) from real samples and associated elements

    Institute of Scientific and Technical Information of China (English)

    KOKATE Sudarshan Jagdish; KUCHEKAR Shashikant Raghunath

    2009-01-01

    The extraction behavior of platinum(Ⅳ) was studied with N-n-octylaniline as a function of different parameters,such as pH,concentrations of weak acids,mineral acids,reagents and elution time. A selective method was developed for the extraction chromatographic studies of platinum(Ⅳ) and its separation from several metal ions with N-n-octylaniline (liquid anion exchanger) as a stationary phase on silica gel. The quantitative extraction of platinum(Ⅳ) was observed with 0.067 mol/L N-n-octylaniline and 0.015 mol/L ascorbic acid at pH 1.0. Metal ion was stripped from the column with water and determined spectrophotometrically with stannous chloride method. The proposed method is free from the interference of a large number of cations and anions. Platinum(Ⅳ) was separated from pharmaceutical preparations,alloys and synthetic mixtures. Mutual separation scheme was developed for platinum(Ⅳ),palladium(Ⅱ) and gold(Ⅲ). The log-log plot of N-n-octylaniline concentration versus the distribution ratio indicates that the probable extracted species is [RR~′NH~+_2 ] · Pt(C_6H_7O_6)~-_3.

  9. Application of alkyl polyglycoside surfactant in ultrasonic-assisted extraction followed by macroporous resin enrichment for the separation of vitexin-2″-O-rhamnoside and vitexin from Crataegus pinnatifida leaves.

    Science.gov (United States)

    Han, Feng; Guo, Yupin; Gu, Huiyan; Li, Fenglan; Hu, Baozhong; Yang, Lei

    2016-02-15

    An alkyl polyglycoside (APG) surfactant was used in ultrasonic-assisted extraction to effectively extract vitexin-2″-O-rhamnoside (VOR) and vitexin (VIT) from Crataegus pinnatifida leaves. APG0810 was selected as the surfactant. The extraction process was optimized for ultrasonic power, the APG concentration, ultrasonic time, soaking time, and liquid-solid ratio. The proposed approach showed good recovery (99.80-102.50% for VOR and 98.83-103.19% for VIT) and reproducibility (relative standard deviation, n=5; 3.7% for VOR and 4.2% for VIT) for both components. The proposed sample preparation method is both simple and effective. The use of APG for extraction of key herbal ingredients shows great potential. Ten widely used commercial macroporous resins were evaluated in a screening study to identify a suitable resin for the separation and purification of VOR and VIT. After comparing static and dynamic adsorption and desorption processes, HPD100B was selected as the most suitable resin. After column adsorption and desorption on this resin, the target compounds VOR and VIT can be effectively separated from the APG0810 extraction solution. Recoveries of VOR and VIT were 89.27%±0.42% and 85.29%±0.36%, respectively. The purity of VOR increased from 35.0% to 58.3% and the purity of VIT increased from 12.5% to 19.9%. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Elaboration of extracting, incinerable and/or conducting resins, for the grouped conversion of actinides; Conception de resines extractantes, incinerables et/ou conductrices, pour la conversion groupee d'actinides

    Energy Technology Data Exchange (ETDEWEB)

    Mokhtari, H. [Paris-11 Univ., 91 - Orsay (France)]|[CEA Valrho, Lab. de Chimie des Actinides (LCA), 30 - Marcoule (France)

    2006-07-01

    The first results obtained in the framework of the study called PEACE (Process for the Elaboration of Actinide Carbide from ion Exchange resin) concern the fixation of neodymium(III) (simulating trivalent actinides) on two carboxylic resins: the first one is of gel type and the second one of macroporous type. A kinetic study of the exchange NH{sub 4}{sup +}/Nd{sup 3+} has shown that: 1)neodymium is fixed under the form of a complexed or hydrolyzed specie of neodymium of charge 2+ 2)a high charge rate is reached (40% in mass for the dried resin which corresponds to an exchange capacity of 11 meq/g dry of introduced resin) 3)the exchange kinetics is better for the macroporous resin than for the gel resin. A heat treatment of the macroporous resin charged in neodymium has been carried out until the carbonization by the mean of thermal gravimetric analyses carried out under air and argon. A carbon/neodymium ratio of about 5 is obtained after carbonization under argon. Scanning electron microscopy analyses carried out on the macroporous resin charged in neodymium have revealed a conservation of the sphericity and a consequent reduction of the resin balls diameter after heat treatment and an homogeneous distribution of neodymium inside the sphere. (O.M.)

  11. Improvement of skin condition in striae distensae: development, characterization and clinical efficacy of a cosmetic product containing Punica granatum seed oil and Croton lechleri resin extract

    Directory of Open Access Journals (Sweden)

    Bogdan C

    2017-02-01

    Full Text Available Cătălina Bogdan,1 Sonia Iurian,2 Ioan Tomuta,2 Mirela Moldovan1 1Department of Dermatopharmacy and Cosmetics, 2Department of Pharmaceutical Technology and Biopharmacy, Faculty of Pharmacy, University of Medicine and Pharmacy Iuliu Hatieganu, Cluj-Napoca, Romania Abstract: Striae distensae are a frequent skin condition associated with pregnancy, weight change or lack of skin elasticity. The aim of this research was to obtain a topical product containing herbal active ingredients with documented antioxidant and anti-inflammatory activity (Punica granatum seed oil and Croton lechleri resin extract and demonstrate its positive effect on prevention and treatment of striae distensae. First, the cream base formulation was optimized through experimental design. Secondly, the cream containing the two active ingredients was investigated in an interventional nonrandomized clinical trial. The clinical outcome was assessed through biophysical parameters and ultrasonographic evaluation. The state of the skin was evaluated by biophysical measurements and ultrasonography at the beginning of the study and after 3 and 6 weeks. The experimental design was successfully used to set the best ranges for the technological and formulation factors to obtain a cosmetic formulation with optimal characteristics. The study of clinical efficacy on the optimal formulation revealed an increase in the dermis thickness, hydration and elasticity values in both groups after 6 weeks of cream application. The new oil-in-water cream containing P. granatum seed oil and C. lechleri resin extract can be helpful in the prevention or improving of skin changes associated with striae. Keywords: stretch marks, ultrasonography, texture analysis, design of experiments, oil-in-water emulsion

  12. Ion-exclusion chromatographic behavior of aliphatic carboxylic acids and benzenecarboxylic acids on a sulfonated styrene--divinylbenzene co-polymer resin column with sulfuric acid containing various alcohols as eluent.

    Science.gov (United States)

    Ohta, Kazutoku; Towata, Atsuya; Ohashi, Masayoshi

    2003-05-16

    The addition of C1-C7 alcohols (methanol, ethanol, propanol, butanol, heptanol, hexanol and heptanol) to dilute sulfuric acid as eluent in ion-exclusion chromatography using a highly sulfonated styrene-divinylbenzene co-polymer resin (TSKgel SCX) in the H+ form as the stationary phase was carried out for the simultaneous separations of both (a) C1-C7 aliphatic carboxylic acids (formic, acetic, propionic, isobutyric, butyric, isovaleric, valeric, 2-methylvaleric, isocaproic, caproic, 2,2-dimethyl-n-valeric, 2-methylhexanoic, 5-methylhexanoic and heptanoic acids) and (b) benzenecarboxylic acids (pyromellitic, hemimellitic, trimellitic, o-phthalic, m-phthalic, p-phthalic, benzoic and salicylic acids and phenol). Heptanol was the most effective modifier in ion-exclusion chromatography for the improvement of peak shapes and a reduction in retention volumes for higher aliphatic carboxylic acids and benzenecarboxylic acids. Excellent simultaneous separation and relatively highly sensitive conductimetric detection for these C1-C7 aliphatic carboxylic acids were achieved on the TSKgel SCX column (150 x 6 mm I.D.) in 30 min using 0.5 mM sulfuric acid containing 0.025% heptanol as eluent. Excellent simultaneous separation and highly sensitive UV detection at 200 nm for these benzenecarboxylic acids were also achieved on the TSKgel SCX column in 30 min using 5 mM sulfuric acid containing 0.075% heptanol as eluent.

  13. Ion-exclusion chromatographic separations of C1-C6 aliphatic carboxylic acids on a sulfonated styrene-divinylbenzene co-polymer resin column with 5-methylhexanoic acid as eluent.

    Science.gov (United States)

    Ohta, Kazutoku; Towata, Atsuya; Ohashi, Masayoshi

    2003-05-16

    The application of C7 aliphatic carboxylic acids (heptanoic, 2-methylhexanoic, 5-methylhexanoic and 2,2-dimethyl-n-valeric acids) as eluents in ion-exclusion chromatography with conductimetric detection for C1-C6 aliphatic carboxylic acids (formic, acetic, propionic, isobutyric, butyric, isovaleric, valeric, isocaproic and caproic acids) was carried out using a highly sulfonated styrene-divinylbenzene co-polymer resin (TSKgel SCX) in the H+ form as a stationary phase. When using 0.05 mM sulfuric acid at pH 4.0 as the eluent, peak shapes of hydrophobic carboxylic acids (isovaleric, valeric, isocaproic and caproic acids) were tailed strongly. In contrast, when using 1 mM these C7 carboxylic acids at pH ca. 4 as the eluents, although system peaks (vacant peaks) corresponding to these C7 carboxylic acids appeared, peak shapes of these hydrophobic acids were improved drastically. Excellent simultaneous separation and relatively high sensitive conductimetric detection for these C1-C6 aliphatic carboxylic acids were achieved in 25 min on the TSKgel SCX column (150 x 6 mm I.D.) using 1 mM 5-methylhexanoic acid at pH 4.0 as the eluent.

  14. Bioprospecting of microalgae: Proper extraction followed by high performance liquid chromatographic-high resolution mass spectrometric fingerprinting as key tools for successful metabolom characterization.

    Science.gov (United States)

    Stranska-Zachariasova, Milena; Kastanek, Petr; Dzuman, Zbynek; Rubert, Josep; Godula, Michal; Hajslova, Jana

    2016-03-15

    Currently, the interest in microalgae as a source of biologically active components exploitable as supplementary ingredients to food/feed or in cosmetics continues to increase. Existing research mainly aims to focus on revealing and recovering the rare, cost competitive components of the algae metabolom. Because these components could be of very different physicochemical character, a universal approach for their isolation and characterization should be developed. This study demonstrates the systematic development of the extraction strategy that represents one of the key challenges in effective algae bioprospecting, which predefines their further industrial application. By using of Trachydiscus minutus as a model microalgae biomass, following procedures were tested and critically evaluated in order to develop the generic procedure for microalgae bioprospecting: (i) various ways of mechanical disintegration of algae cells enabling maximum extraction efficiency, (ii) the use of a wide range of extraction solvents/solvent mixtures suitable for optimal extraction yields of polar, medium-polar, and non-polar compounds, (iii) the use of consecutive extractions as a fractionation approach. Within the study, targeted screening of selected compounds representing broad range of polarities was realized by ultra-high performance liquid chromatography coupled with high resolution tandem mass spectrometric detection (UHPLC-HRMS/MS), to assess the effectiveness of undertaken isolation steps. As a result, simple and high-throughput extraction-fractionation strategy based on consecutive extraction with water-aqueous methanol-hexane/isopropanol was developed. Moreover, to demonstrate the potential of the UHPLC-HRMS/MS for the retrospective non-target screening and compounds identification, the collected mass spectra have been evaluated to characterize the pattern of extracted metabolites. Attention was focused on medium-/non-polar extracts and characterization of lipid species

  15. Total milk fat extraction and quantification of polar and neutral lipids of cow, goat, and ewe milk by using a pressurized liquid system and chromatographic techniques.

    Science.gov (United States)

    Castro-Gómez, M P; Rodriguez-Alcalá, L M; Calvo, M V; Romero, J; Mendiola, J A; Ibañez, E; Fontecha, J

    2014-11-01

    Although milk polar lipids such as phospholipids and sphingolipids located in the milk fat globule membrane constitute 0.1 to 1% of the total milk fat, those lipid fractions are gaining increasing interest because of their potential beneficial effects on human health and technological properties. In this context, the accurate quantification of the milk polar lipids is crucial for comparison of different milk species, products, or dairy treatments. Although the official International Organization for Standardization-International Dairy Federation method for milk lipid extraction gives satisfactory results for neutral lipids, it has important disadvantages in terms of polar lipid losses. Other methods using mixtures of solvents such as chloroform:methanol are highly efficient for extracting polar lipids but are also associated with low sample throughput, long time, and large solvent consumption. As an alternative, we have optimized the milk fat extraction yield by using a pressurized liquid extraction (PLE) method at different temperatures and times in comparison with those traditional lipid extraction procedures using 2:1 chloroform:methanol as a mixture of solvents. Comparison of classical extraction methods with the developed PLE procedure were carried out using raw whole milk from different species (cows, ewes, and goats) and considering fat yield, fatty acid methyl ester composition, triacylglyceride species, cholesterol content, and lipid class compositions, with special attention to polar lipids such as phospholipids and sphingolipids. The developed PLE procedure was validated for milk fat extraction and the results show that this method performs a complete or close to complete extraction of all lipid classes and in less time than the official and Folch methods. In conclusion, the PLE method optimized in this study could be an alternative to carry out milk fat extraction as a routine method.

  16. Mutagenic potentials of Amberlite XAD-2-resin extracts obtained from river and drinking waters in the Northwest district of Chiba, Japan.

    Science.gov (United States)

    Kanno, Ayako; Nishi, Iwaki; Kishi, Tomohiro; Kawakami, Tsuyoshi; Takahashi, Yasuo; Onodera, Sukeo

    2010-12-01

    Amberlite XAD-2 resin extracts of river and drinking water sampled from the Northwest district of Chiba Prefecture in each month during the period from January to December 2008 were investigated to characterize and determine their mutagenic potentials and polycyclic aromatic hydrocarbon (PAH) levels. The extracts from the river water were shown to be mutagenic in Salmonella typhimurium TA98 (a flameshift mutagen) without S9 mix, with higher mutagenic responses in summer and early fall seasons. While the drinking water extracts exhibited weak mutagenicity in both the TA98 and TA100 strains (a base-pair substitution mutagen) without S9 mix, with high mutagenic responses in fall and early winter seasons. GC/MS determinations of the water concentrates showed some seasonal scatter in PAH levels in river water. In contrast, comparatively high concentrations of PAHs were observed for drinking water samples collected during warmer seasons. Statistical studies revealed that there is a lower correlation between the levels of flameshift mutagenicity and the concentrations of PAH in the river water concentrations, but a higher correlation between them in the drinking water samples.

  17. Development of a Sustainable Procedure for the Recovery of Hydroxytyrosol from Table Olive Processing Wastewater Using Adsorption Resin Technology and Centrifugal Partition Chromatography.

    Science.gov (United States)

    Xynos, Nikos; Abatis, Dennis; Argyropoulou, Aikaterini; Polychronopoulos, Panagiotis; Aligiannis, Nektarios; Skaltsounis, Alexios-Leandros

    2015-11-01

    The present endeavor aims to establish a novel procedure, applicable to the extraction and isolation of hydroxytyrosol from table olive processing wastewater. A two-step chromatographic separation is presented using non-ionic absorbent resin for the recovery of its phenolic content, followed by purification of hydroxytyrosol with centrifugal partition chromatography. Two table olive processing wastewaters, obtained from Kalamon and Amfissis olive varieties, were used. In the extracts obtained after resin treatment, the hydroxytyrosol content was determined by high-performance liquid chromatography with diode-array detection to be 4.05% and 10.10%, respectively. The extract from Amfissis table olive processing wastewater was further processed with preparative centrifugal partition chromatography for the purification of hydroxytyrosol. High-performance liquid chromatography analysis revealed that the isolated compound was >95% purity. Georg Thieme Verlag KG Stuttgart · New York.

  18. Chromatographic fingerprint analysis of Pycnogenol dietary supplements.

    Science.gov (United States)

    Chen, Pei; Song, Fenhong; Lin, Long-Ze

    2009-01-01

    The bark of maritime pine (Pinus pinaster Aiton) has been widely used as a remedy for various degenerative diseases. A standard high-performance liquid chromatographic (HPLC) procedure for Pycnogenol analysis is a method specified in the United States Pharmacopeia (USP) monograph, which requires measurement of peak areas and identification of four components of the extract: caffeic acid, catechin, ferulic acid, and taxifolin. In this study, a fingerprint analysis using an HPLC method based on the USP monograph has been developed to provide additional qualitative information for the analysis of Pycnogenol-containing dietary supplements (PDS). Twelve commercially available PDS samples were purchased and analyzed along with a standard Pycnogenol extract. Their chromatographic fingerprints were analyzed using principal component analysis. The results showed that two of the samples were not consistent with the standard reference Pycnogenol extract. One contained other active ingredients in addition to Pycnogenol, and the other may have resulted from a quality control issue in manufacturing.

  19. Liquid Anion Exchange Chromatographic Extraction and Separation of Platinum(IV with n-Octylaniline as a Metallurgical Reagent: Analysis of Real Samples

    Directory of Open Access Journals (Sweden)

    Ashwini P. Gaikwad

    2013-01-01

    Full Text Available A simple and selective method was developed for the determination of platinum(IV with n-octylaniline in toluene. In present study, the use of n-octylaniline in toluene for the extraction of platinum(IV from ascorbate media was carried out. The effect of various parameters, such as pH, equilibrium time, extractant concentration, and organic solvent on the extraction has been discussed. The back extraction of platinum(IV has been performed. On the basis of slope analysis, the composition of the extracted species was determined as [RR′NH2+ Pt(Succinate2−](org. The interfering effects of various cations and anions were also studied, and the selectivity of the method is enhanced by using suitable masking agents. The proposed method is rapid, reproducible and successfully applied for the determination of platinum(IV in binary and synthetic mixtures. The separation of pt(IV from other associated metals has been studied. Comparison of the results with those obtained using an atomic absorption spectrophotometer also tested the validity of the method.

  20. Chromatographic Fingerprint and the Simultaneous Determination of Five Bioactive Components of Geranium carolinianum L. Water Extract by High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Li-Fang Liu

    2011-12-01

    Full Text Available A simple and sensitive HPLC method has been developed in combination with fingerprint analysis and simultaneous determination of five markers, namely gallic acid, corilagin, methyl brevifolincarboxylate, ellagic acid and rutin for evaluation and quality control of Geranium carolinianum L. water extract. Extraction methods were optimized by comparing the hydrolysis efficiency of geraniin, a major tannin of the herb, resulting in the method of extraction with water under reflux. Water extracts were analyzed by HPLC, with a mobile phase of 0.1% aqueous phosphoric acid (v/v and acetonitrile in a gradient program within 65 min. Compounds were detected at 274 nm UV wavelength. For fingerprint analysis, 17 peaks were selected as the characteristic peaks to evaluate the similarities of different samples collected from the suburb of Nanjing. The correlation coefficients of similarity were greater than 0.993. In quantitative analysis, the five selected markers showed good regression (R > 0.9991 within test ranges, and the average recoveries were between 97.2–101.7% and their RSD values were less than 4.50%. The total contents of the five markers varied from 44.28 to 71.84 mg/g. The method can be very useful for further development of G. carolinianum L. extracts and preparations.

  1. The Effect of Aloe Vera, Pomegranate Peel, Grape Seed Extract, Green Tea, and Sodium Ascorbate as Antioxidants on the Shear Bond Strength of Composite Resin to Home-bleached Enamel.

    Science.gov (United States)

    Sharafeddin, Farahnaz; Farshad, Farnaz

    2015-12-01

    Immediate application of bonding agent to home- bleached enamel leads to significant reduction in the shear bond strength of composite resin due to the residual oxygen. Different antioxidant agents may overcome this problem. This study aimed to assess the effect of different antioxidants on the shear bond strength of composite resin to home-bleached. Sixty extracted intact human incisors were embedded in cylindrical acrylic resin blocks (2.5×1.5 cm), with the coronal portion left out of the block. After bleaching the labial enamel surface with 15% carbamide peroxide, they were randomly divided into 6 groups (n=10). Before performing composite resin restoration by using a cylindrical Teflon mold (5×2 mm), each group was treated with one of the following antioxidants: 10% sodium ascorbate solution, 10% pomegranate peel solution, 10% grape seed extract, 5% green tea extract, and aloe vera leaf gel. One group was left untreated as the control. The shear bond strength of samples was tested under a universal testing machine (ZwickRoell Z020). The shear bond strength data were analyzed by one-way ANOVA and post hoc Tukey tests (pbond strength of bleached enamel. Different antioxidants used in this study had the same effect on the shear bond strength of home-bleached enamel, and none of them caused a statistically significant increase in its value.

  2. Development and validation of a reversed-phase high-performance liquid chromatographic method with solid-phase extraction for the quantification of hydrochlorothiazide in ex vivo permeation studies.

    Science.gov (United States)

    Onnainty, R; Schenfeld, E M; Longhi, M R; Quevedo, M A; Granero, G E

    2017-08-01

    Hydrochlorothiazide (HCT) is a diuretic used to treat hypertension. In order to study its intestinal permeation behavior applying an ex vivo methodology, a rapid, sensitive and selective reversed-phase liquid chromatography (RP-HPLC) method coupled with UV detection (RP-HPLC UV) was developed for the analysis of HCT in TC199 culture medium used as mucosal and serosal solutions in the everted rat intestinal sac model. Also, analytical procedures for the quantification of HCT by RP-HPLC with UV detection required a sample preparation step by solid-phase extraction. The method was validated in the concentration range of 8.05 × 10(-7) to 3.22 × 10(-5)  m for HCT. Chromatographic parameters, namely carry-over, lower limit of quantification (1.4491 × 10(-7)  m), limit of detection (3.8325 × 10(-8)  m), selectivity, inter- and intraday precision and extraction recovery, were determined and found to be adequate for the intended purposes. The validated method was successfully used for permeability assays across rat intestinal epithelium applying the ex vivo everted rat gut sac methodology to study the permeation behavior of HCT. Copyright © 2017 John Wiley & Sons, Ltd.

  3. Chromatographic and Related Reactors.

    Science.gov (United States)

    1988-01-07

    special information about effects of surface heteroge- neity in the methanation reaction. Studies of an efficient multicolumn assembly for measuring...of organic basic catalysts such as pyridine and 4-methylpicoline. It was demonstrated that the chromatographic reactor gave special information about...Programmed Reaction to obtain special information about surface heterogeneity in the methanation reaction. Advantages of stopped flow over steady state

  4. Decoloration of Raffinose Extract Solutions via Macroporous Resin Adsorption%棉籽糖提取液树脂吸附脱色

    Institute of Scientific and Technical Information of China (English)

    段舒然; 鲍宗必; 闻光东; 陈丽芬; 杨亦文

    2016-01-01

    Raffinose extract solutions contain considerable amounts of colored impurities, and those hydrophobic pigments can be removed by organic solvent extraction. However, there are still water-soluble pigments that can affect the product purity and crystallization processes. In this study, decoloration performance using several resins (HZ-801, HZ-803, HZ-806, HZ-818, D303 and D313) was compared with activated carbon, and the adsorption conditions were optimized according to raffinose decoloration ratio and loss ratio. The results show that HZ-818 is the best candidate with the highest decoloration ratio of 77.1% and loss ratio of 2.4%. The process shows the best cost-effectiveness when the dosage is 2.0 g resin per 10 mL solution under contact time of 9 h. The spent resin can be regenerated with 60% aqueous ethanol and the recycled resins are further used with decoloration ratio up to 94.0%.%棉籽糖的提取液中含有大量的有色杂质,经有机溶剂脱酚处理除去大部分疏水性色素,仍有少量水溶性色素残留,它们的存在会影响棉籽糖产品的纯度、色泽及结晶过程。研究以脱色率和棉籽糖损失率为指标,对比了HZ-801、HZ-803、HZ-806和HZ-818等四种大孔吸附树脂及D313、D303弱碱性阴离子交换树脂与活性炭的脱色性能,考察了影响静态吸附脱色的操作条件及脱色动力学,结果表明:HZ-818树脂为棉籽糖提取液的最佳脱色树脂,单次脱色率最高,达77.1%,棉籽糖损失率2.4%;树脂用量为2.0 g树脂/10 mL溶液、脱色时间为9 h时脱色过程较为经济。吸附色素的树脂可通过60%的乙醇水溶液进行再生,再生后树脂对原料液进行脱色实验,脱色率达94.0%。

  5. Sensitive determination of estrogens in environmental waters treated with polymeric ionic liquid-based stir cake sorptive extraction and liquid chromatographic analysis.

    Science.gov (United States)

    Chen, Lei; Mei, Meng; Huang, Xiaojia; Yuan, Dongxing

    2016-05-15

    A simple, sensitive and environmentally friendly method using polymeric ionic liquid-based stir cake sorptive extraction followed by high performance liquid chromatography with diode array detection (HPLC/DAD) has been developed for efficient quantification of six selected estrogens in environmental waters. To extract trace estrogens effectively, a poly (1-ally-3-vinylimidazolium chloride-co-ethylene dimethacrylate) monolithic cake was prepared and used as the sorbent of stir cake sorptive extraction (SCSE). The effects of preparation conditions of sorbent and extraction parameters of SCSE for estrogens were investigated and optimized. Under optimal conditions, the developed method showed satisfactory analytical performance for targeted analytes. Low limits of detection (S/N=3) and quantification limits (S/N=10) were achieved within the range of 0.024-0.057 µg/L and 0.08-0.19 µg/L, respectively. Good linearity of method was obtained for analytes with the correlation coefficients (R(2)) above 0.99. At the same time, satisfactory method repeatability and reproducibility was achieved in terms of intra- and inter-day precisions, respectively. Finally, the established SCSE-HPLC/DAD method was successfully applied for the determination of estrogens in different environmental water samples. Recoveries obtained for the determination of estrogens in spiked samples ranged from 71.2% to 108%, with RSDs below 10% in all cases.

  6. Métodos de extração e/ou concentração de compostos encontrados em fluidos biológicos para posterior determinação cromatográfica Methods of extraction and/or concentration of compounds found in biological fluids for subsequent chromatographic determination

    Directory of Open Access Journals (Sweden)

    Sonia C. N. Queiroz

    2001-02-01

    Full Text Available When organic compounds present in biological fluids are analysed by chromatographic methods, it is generally necessary to carry out a prior sample preparation due the high complexity of this type of sample, especially when the compounds to be determinated are found in very low concentrations. This article describes some of the principal methods for sample preparation in analyses of substances present in biological fluids. The methods include liquid-liquid extraction, solid phase extraction, supercritical fluid extraction and extraction using solid and liquid membranes. The advantages and disadvantages of these methods are discussed.

  7. Water-compatible dummy molecularly imprinted resin prepared in aqueous solution for green miniaturized solid-phase extraction of plant growth regulators.

    Science.gov (United States)

    Wang, Mingyu; Chang, Xiaochen; Wu, Xingyu; Yan, Hongyuan; Qiao, Fengxia

    2016-08-01

    A water-compatible dummy molecularly imprinted resin (MIR) was synthesized in water using melamine, urea, and formaldehyde as hydrophilic monomers of co-polycondensation. A triblock copolymer (PEO-PPO-PEO, P123) was used as porogen to dredge the network structure of MIR, and N-(1-naphthyl) ethylenediamine dihydrochloride, which has similar shape and size to the target analytes, was the dummy template of molecular imprinting. The obtained MIR was used as the adsorbent in a green miniaturized solid-phase extraction (MIR⬜mini-SPE) of plant growth regulators, and there was no organic solvent used in the entire MIR⬜mini-SPE procedure. The calibration linearity of MIR⬜mini-SPE⬜HPLC method was obtained in a range 5⬜250ngmL(↙1) for IAA, IPA, IBA, and NAA with correlation coefficient (r) Ⱕ0.9998. Recoveries at three spike levels are in the range of 87.6⬜100.0% for coconut juice with relative standard deviations Ⱔ8.1%. The MIR⬜mini-SPE method possesses the advantages of environmental friendliness, simple operation, and high efficiency, so it is potential to apply the green pretreatment strategy to extraction of trace analytes in aqueous samples.

  8. Glyoxal-Urea-Formaldehyde Molecularly Imprinted Resin as Pipette Tip Solid-Phase Extraction Adsorbent for Selective Screening of Organochlorine Pesticides in Spinach.

    Science.gov (United States)

    Yang, Chen; Lv, Tianwei; Yan, Hongyuan; Wu, Gaochan; Li, Haonan

    2015-11-01

    A new kind of glyoxal-urea-formaldehyde molecularly imprinted resin (GUF-MIR) was synthesized by a glyoxal-urea-formaldehyde (GUF) gel imprinting method with 4,4'-dichlorobenzhydrol as a dummy template. The obtained GUF-MIR was characterized by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FT-IR) and applied as a selective adsorbent of miniaturized pipet tip solid-phase extraction (PT-SPE) for the separation and extraction of three organochlorine pesticides (dicofol (DCF), dichlorodiphenyl dichloroethane (DDD), and tetradifon) in spinach samples. The proposed pretreatment procedures of spinach samples involved only 5.0 mg of GUF-MIR, 0.7 mL of MeOH-H2O (1:1, v/v) (washing solvent), and 0.6 mL of cyclohexane-ethyl acetate (9:1, v/v) (elution solvent). In comparison with other adsorbents (such as silica gel, C18, NH2-silica gel, and neutral alumina (Al2O3-N)), GUF-MIR showed higher adsorption and purification capacity for DCF, DDD, and tetradifon in aqueous solution. The average recoveries at three spiked levels ranged from 89.1% to 101.9% with relative standard deviations (RSDs) ≤ 7.1% (n = 3). The presented GUF-MIR-PT-SPE method combines the advantages of molecularly imprinted polymers (MIPs), GUF, and PT-SPE and can be used in polar solutions with high affinity and selectivity to the analytes in complex samples.

  9. Rapid determination of strontium-90 by solid phase extraction using DGA Resin® for seawater monitoring

    Science.gov (United States)

    Tazoe, H.; Obata, H.; Yamagata, T.; Karube, Z.; Yamada, M.

    2015-12-01

    Strontium-90 concentrations in seawater exceeding the background level have been observed at the accidents of nuclear facilities, such as Chernobyl and Fukushima. However, analytical procedure for strontium-90 in seawater is still quite complicated and challenging. Here we show a simple and rapid analytical technique for the determination of strontium-90 in seawater samples without time-consuming separation of strontium from calcium. The separation with DGA Resin® is used to determine the abundance of strontium-90, which selectively collects yttrium-90, progeny of strontium-90. Naturally occurring radioactive nuclides (such as potassium, lead, bismuth, uranium, and thorium) and anthropogenic radionuclides (such as cesium, barium, lanthanum, and cerium) were separated from yttrium. Through a sample separation procedure, a high chemical yield of yttrium-90 was achieved at 93.9 % for seawater. The result of IAEA 443 certified seawater analysis was in good agreement with the certified value. At 20 hrs counting a lower detection limit of 1.5 mBq L-1 was obtained from 3 L of seawater. The proposed method can finish analyzing 8 samples per day, which is a reasonably fast throughput in actual seawater monitoring. Reproducibility was found to be 3.4 % according to 10 separate analyses of natural seawater samples from the vicinity of Fukushima Daiichi Nuclear Power Plant in September 2013.

  10. An effective high-speed countercurrent chromatographic method for preparative isolation and purification of mollugin directly from the ethanol extract of the Chinese medicinal plant Rubia cordifolia.

    Science.gov (United States)

    Lu, Yanbin; Liu, Rui; Sun, Cuirong; Pan, Yuanjiang

    2007-06-01

    The medicinal plant Rubia cordifolia has been used widely in traditional Chinese medicine (TCM) for its antibacterial, antioxidant and anti-inflammatory activities. In this study, a preparative high-speed countercurrent chromatography (HSCCC) method for isolation and purification of the bioactive component mollugin directly from the ethanol extract of R. cordifolia was successfully established by using light petroleum (bp 60-90 degrees C)/ethanol/diethyl ether/water as the two-phase solvent system. The upper phase of light petroleum/ethanol/diethyl ether/water (5:4:3:1 v/v) was used as the stationary phase of HSCCC. Under the optimum conditions, 46 mg of mollugin at 98.5% purity, as determined by HPLC, could be yielded from 500 mg of the crude extract in a single HSCCC separation. The peak fraction of HSCCC was identified by 1H NMR and 13C NMR.

  11. Extraction and Chromatographic Determination of Shikimic Acid in Chinese Conifer Needles with 1-Benzyl-3-methylimidazolium Bromide Ionic Liquid Aqueous Solutions

    Directory of Open Access Journals (Sweden)

    Fengli Chen

    2014-01-01

    Full Text Available An ionic liquids-based ultrasound-assisted extraction (ILUAE method was successfully developed for extracting shikimic acid from conifer needles. Eleven 1-alkyl-3-methylimidazolium ionic liquids with different cations and anions were investigated and 1-benzyl-3-methylimidazolium bromide solution was selected as the solvent. The conditions for ILUAE, including the ionic liquid concentration, ultrasound power, ultrasound time, and liquid-solid ratio, were optimized. The proposed method had good recovery (99.37%–100.11% and reproducibility (RSD, n = 6; 3.6%. ILUAE was an efficient, rapid, and simple sample preparation technique that showed high reproducibility. Based on the results, a number of plant species, namely, Picea koraiensis, Picea meyeri, Pinus elliottii, and Pinus banksiana, were identified as among the best resources of shikimic acid.

  12. QuEChERS Method Followed by Solid Phase Extraction Method for Gas Chromatographic-Mass Spectrometric Determination of Polycyclic Aromatic Hydrocarbons in Fish

    Directory of Open Access Journals (Sweden)

    Mona Khorshid

    2015-01-01

    Full Text Available A gas chromatography equipped with mass spectrometer (GCMS method was developed and validated for determination of 16 polycyclic aromatic hydrocarbons (PAHs in fish using modified quick, easy, cheap, effective, rugged, and safe (QuEChERS method for extraction and solid phase extraction for sample cleanup to remove most of the coextract combined with GCMS for determination of low concentration of selected group of PAHs in homogenized fish samples. PAHs were separated on a GCMS with HP-5ms Ultra Inert GC Column (30 m, 0.25 mm, and 0.25 µm. Mean recovery ranged from 56 to 115%. The extraction efficiency was consistent over the entire range where indeno(1,2,3-cdpyrene and benzo(g,h,iperylene showed recovery (65, 69%, respectively, at 2 µg/kg. No significant dispersion of results was observed for the other remaining PAHs and recovery did not differ substantially, and at the lowest and the highest concentrations mean recovery and RSD% showed that most of PAHs were between 70% and 120% with RSD less than 10%. The measurement uncertainty is expressed as expanded uncertainty and in terms of relative standard deviation (at 95% confidence level is ±12%. This method is suitable for laboratories engaged daily in routine analysis of a large number of samples.

  13. Development and validation of a high-performance liquid chromatographic method for the determination of stemoninine in rat plasma after administration of Stemona tuberosa extracts.

    Science.gov (United States)

    Jiang, Dengzhao; Yang, Xue; Liu, Hongbing; Guan, Huashi

    2011-04-01

    For the first time, an HPLC method was developed and validated for the determination of stemoninine in plasma after oral and intravenous administration of the extract of the roots of Stemona tuberosa to rats. Plasma samples were analyzed on a Waters reversed-phase C(18) column using a gradient mobile-phase of eluent A (water containing 0.1% formic acid and 0.2% triethylamine, pH 3.68) and eluent B (acetonitrile-water, 50:50, v/v). The flow rate was 1.0 mL/min and the detector wavelength was 210 nm. The Waters Oasis solid-phase extraction cartridge was applied for the preparation of plasma samples with high recovery. A good linear relationship was obtained in the concentration range of 1.55-124 µg/mL (r = 0.9995). The limits of quantification and detection were 1.55 and 0.42 µg/mL, respectively. The average recoveries ranged from 91.11 to 96.43% in plasma at stemoninine concentrations of 3.10, 62.0 and 99.2 µg/mL. Intra- and inter-batch coefficient of variations were 3.27-5.37% and 2.49-3.92%, respectively. This method was successfully applied to pharmacokinetic studies after oral and intravenous administration of Stemona tuberosa extract in rats.

  14. 大孔吸附树脂纯化甘草提取物中甘草酸的研究%Macroporous Adsorption Resin Purification of Glycyrrhizic Acid in Glycyrrhiza Extract Research

    Institute of Scientific and Technical Information of China (English)

    丁利营; 李红艳

    2014-01-01

    Objective To study the best macroporous resin purification process for Glycyrrhizic acid from glycyrrhiza glabra. Methods Glycyrrhizic acid content in macroporous resin purification as the investigation index, select the best macroporous resin from 24 kinds of macroporous resins for Glycyrrhizic acid from liquorice extract, and determine the optimum process conditions for this purification. Results AB-8 macroporous adsorption resin has the best purification ef ect for glycyrrhizic acid, and the optimum process conditions:liquorice extract concentration is 0.11mg/ml, diameter/height is 1:8, liquorice extract volume is 2 times of the resin, the rates of using liquorice extract and elution both are 2bv/h, remove impurities with 30%&50%ETOH, and accumulate glycyrrhizic acid by using 80%ETOH. After purification, the purity of the product is 60.74%, the yield rate is 3.29%, the transfer rate is 76.72%. Conclusion Using AB-8 macroporous adsorption resin can purify glycyrrhizic acid very wel .%目的研究光果甘草中甘草酸的最佳大孔树脂纯化工艺。方法以大孔吸附树脂纯化物中甘草酸的含量为考察指标,从24种大孔吸附树脂中筛选出纯化甘草粗提物中甘草酸的最佳大孔吸附树脂,并确定纯化甘草酸的最佳工艺条件。结果 AB-8大孔吸附树脂纯化甘草酸效果最佳,最佳工艺条件院上柱液浓度为0.11mg/mL,径高比为1:8,上样体积为所用树脂2BV,上样速度与洗脱速度均为2BV/h,用30%、50%的乙醇除杂,用80%乙醇富集甘草酸。纯化后产品纯度为60.74%,收率为3.29%,转移率为76.33%。结论采用AB-8大孔吸附树脂可较好地纯化甘草酸。

  15. Development, modelling, optimisation and scale-up of chromatographic purification of a therapeutic protein

    DEFF Research Database (Denmark)

    Mollerup, Jørgen; Hansen, Thomas Budde; Kidal, Steffen

    2007-01-01

    Development of a chromatographic purification step proceeds through a number of stages. High-throughput screening techniques are used to identify suitable resins. This technique is also suitable for the design of a capture step and some intermediate chromatographic steps, but development and true...... by industry. The theory of residence time based scale-up is developed and applied. (c) 2007 Elsevier B.V. All rights reserved....

  16. Epoxy resins.

    Science.gov (United States)

    Bray, P G

    1999-01-01

    Epoxy resins have an extraordinarily broad range of commercial applications, especially as protective surface coatings and adhesives. Epoxy resin systems include combinations of epoxy monomers, hardeners, reactive diluents, and/or a vast array of other additives. As a result, an epoxy resin system may have a number of chemical ingredients with the potential for attendant health hazards. Most, but not all, of these health hazards arise in the occupational setting. The most frequent adverse effects are irritation or allergic mechanisms involving the dermal and respiratory systems. Sensitization usually is caused by low molecular weight or short-chain compounds. This review discusses the diagnosis, treatment, and prevention of epoxy resin-related adverse health effects.

  17. Solid phase extraction-preconcentration and high performance liquid chromatographic determination of 2-mercapto-(benzothiazole, benzoxazole and benzimidazole) using copper oxide nanoparticles.

    Science.gov (United States)

    Parham, Hooshang; Khoshnam, Farzaneh

    2013-09-30

    This study introduces a novel method of solid phase extraction (SPE), preconcentration and HPLC determination of 2-mercaptobenzimidazole (2MBI), 2-mercaptobenzoxazole (2MBO) and 2-mercaptobenzothiazole (2MBT) from an aqueous solution by a SPE cartridge loaded with copper oxide nanoparticles. Results demonstrated that copper oxide nanoparticles are quite efficient for extraction and preconcentration of trace amounts of these mercaptans at room temperature. The study also investigated the effects of parameters such as pH, buffer and its volume, electrolyte concentration, flow rate of the test solution, composition and volume of the desorbing solvent, accepted tolerable volume, amount of adsorbent, reusability of cartridges and evidence of some co-existing species on extraction and determination of the above mentioned mercaptans. The method showed good linearity for determination of these mercaptans in the range of 0.01-10 μg mL(-1) with regression coefficients better than 0.9969. The limits of detection (LODs) evaluations were 0.0021, 0.0027 and 0.0019 μg mL(-1) for 2MBT, 2MBO and 2MBI, respectively. The relative standard deviations (RSDs) for 0.2 μg mL(-1) and 5 μg mL(-1) of the measured mercaptans were below 3.04% and 4.23%, respectively. Ramin Power Plant (3000 MW, Ahvaz, Iran) cooling water containing some 2MBT (as corrosion inhibitor) was used as the real sample. Recovery tests with spiked levels of 2MBT, 2MBI and 2MBO were carried out and satisfied results were obtained.

  18. Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection.

    Science.gov (United States)

    Nakamoto, Akihiro; Nishida, Manami; Saito, Takeshi; Kishiyama, Izumi; Miyazaki, Shota; Murakami, Katsunori; Nagao, Masataka; Namura, Akira

    2010-02-19

    A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d(5) was used as an internal standard. The linear ranges were 0.01-5.0 microg mL(-1) for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 microg mL(-1) for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation > or = 0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 microg mL(-1) of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio > or = 3) in urine was 5 ng mL(-1) for MA and MDMA and 10 ng mL(-1) for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation.

  19. Comprehensive automation of the solid phase extraction gas chromatographic mass spectrometric analysis (SPE-GC/MS) of opioids, cocaine, and metabolites from serum and other matrices.

    Science.gov (United States)

    Lerch, Oliver; Temme, Oliver; Daldrup, Thomas

    2014-07-01

    The analysis of opioids, cocaine, and metabolites from blood serum is a routine task in forensic laboratories. Commonly, the employed methods include many manual or partly automated steps like protein precipitation, dilution, solid phase extraction, evaporation, and derivatization preceding a gas chromatography (GC)/mass spectrometry (MS) or liquid chromatography (LC)/MS analysis. In this study, a comprehensively automated method was developed from a validated, partly automated routine method. This was possible by replicating method parameters on the automated system. Only marginal optimization of parameters was necessary. The automation relying on an x-y-z robot after manual protein precipitation includes the solid phase extraction, evaporation of the eluate, derivatization (silylation with N-methyl-N-trimethylsilyltrifluoroacetamide, MSTFA), and injection into a GC/MS. A quantitative analysis of almost 170 authentic serum samples and more than 50 authentic samples of other matrices like urine, different tissues, and heart blood on cocaine, benzoylecgonine, methadone, morphine, codeine, 6-monoacetylmorphine, dihydrocodeine, and 7-aminoflunitrazepam was conducted with both methods proving that the analytical results are equivalent even near the limits of quantification (low ng/ml range). To our best knowledge, this application is the first one reported in the literature employing this sample preparation system.

  20. Use of ZIF-8-derived nanoporous carbon as the adsorbent for the solid phase extraction of carbamate pesticides prior to high-performance liquid chromatographic analysis.

    Science.gov (United States)

    Hao, Lin; Liu, Xingli; Wang, Juntao; Wang, Chun; Wu, Qiuhua; Wang, Zhi

    2015-09-01

    In this work, a chemically and thermally robust and highly porous zeolite-type metal-organic framework, zeolitic imidazolate framework-8 (ZIF-8), was used as both a precursor and a template and furfuryl alcohol as a second precursor to synthesize a nanoporous carbon. The prepared ZIF-8-derived nanoporous carbon was used as the solid-phase extraction adsorbent for the extraction of carbamate pesticides from cabbage and water samples. The adsorbed analytes were eluted with acetonitrile for the determination by high performance liquid chromatography-ultraviolet detection. The high surface area, high porosity, good stability and fast adsorption/desorption kinetics of the material enabled it to have a high adsorption capacity and good adsorption performance. Under optimum conditions, good linearity for the analytes in the range of 0.5-100 ng g(-1) and 0.05-20 ng mL(-1) existed for cabbage and water samples with the correlation coefficients of 0.9968-0.9980 and 0.9990-0.9995, respectively. The limits of detection (S/N=3) for the analytes were in the range of 0.25-0.1 ng g(-1) and 0.01-0.02 ng mL(-1) for the cabbage and water samples, respectively. The relative standard deviations (RSDs) for intra-day and the inter-day determinations of the analytes were below 7.0% and 12.5%, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Stability of arsenic peptides in plant extracts: off-line versus on-line parallel elemental and molecular mass spectrometric detection for liquid chromatographic separation.

    Science.gov (United States)

    Bluemlein, Katharina; Raab, Andrea; Feldmann, Jörg

    2009-01-01

    The instability of metal and metalloid complexes during analytical processes has always been an issue of an uncertainty regarding their speciation in plant extracts. Two different speciation protocols were compared regarding the analysis of arsenic phytochelatin (As(III)PC) complexes in fresh plant material. As the final step for separation/detection both methods used RP-HPLC simultaneously coupled to ICP-MS and ES-MS. However, one method was the often used off-line approach using two-dimensional separation, i.e. a pre-cleaning step using size-exclusion chromatography with subsequent fraction collection and freeze-drying prior to the analysis using RP-HPLC-ICP-MS and/or ES-MS. This approach revealed that less than 2% of the total arsenic was bound to peptides such as phytochelatins in the root extract of an arsenate exposed Thunbergia alata, whereas the direct on-line method showed that 83% of arsenic was bound to peptides, mainly as As(III)PC(3) and (GS)As(III)PC(2). Key analytical factors were identified which destabilise the As(III)PCs. The low pH of the mobile phase (0.1% formic acid) using RP-HPLC-ICP-MS/ES-MS stabilises the arsenic peptide complexes in the plant extract as well as the free peptide concentration, as shown by the kinetic disintegration study of the model compound As(III)(GS)(3) at pH 2.2 and 3.8. But only short half-lives of only a few hours were determined for the arsenic glutathione complex. Although As(III)PC(3) showed a ten times higher half-life (23 h) in a plant extract, the pre-cleaning step with subsequent fractionation in a mobile phase of pH 5.6 contributes to the destabilisation of the arsenic peptides in the off-line method. Furthermore, it was found that during a freeze-drying process more than 90% of an As(III)PC(3) complex and smaller free peptides such as PC(2) and PC(3) can be lost. Although the two-dimensional off-line method has been used successfully for other metal complexes, it is concluded here that the fractionation and

  2. Mass fragmentation study of the trimethylsilyl derivatives of arctiin, matairesinoside, arctigenin, phylligenin, matairesinol, pinoresinol and methylarctigenin: their gas and liquid chromatographic analysis in plant extracts.

    Science.gov (United States)

    Boldizsár, I; Füzfai, Zs; Tóth, F; Sedlák, E; Borsodi, L; Molnár-Perl, I

    2010-03-01

    The mass fragmentation patterns and the characteristic behavior of the trimethylsilyl (TMS) derivatives of the dibenzylbutyrolactone-type (arctiin, arctigenin, methylarctigenin, matairesinoside, matairesinol) and those of the diphenylperhydrofurotetrahydrofurane-type (phylligenin, pinoresinol) lignans, obtained by gas chromatography-mass spectrometry (GC-MS), were presented. It was shown that upon acidic hydrolysis the dibenzylbutyrolactone-type lignans are stable while the diphenylperhydrofurotetrahydrofurane-type ones decompose. As a novelty to the field we confirmed that the fragment species of the derivatized lignan glycosides, in the presence of excess hexamethyldisilazane, leaded to their in situ derivatization. Quantification of the selective fragment ions of the TMS derivatives by GC-MS, in respect of the ions found one by one, and concerning the selective fragment ions {SFI(s)} in total, provided acceptable reproducibilities, suitable for quantitation purposes: varying between 1.20% and 6.6% relative standard deviation percentages (RSD%). For characterization of the behavior of various type of lignans, analyses were performed with the untreated and with the trifluoroacetic acid hydrolyzed plant extracts, from the same sample, in parallel, both by GC-MS and by high performance liquid chromatography-mass spectrometry, working in the positive electron ionization mode (HPLC-ESPI-MS). The analysis of lignans in fruit and leaf extracts (obtained from the Arctium, Centaurea and Forsythia plants) was confirmed both by GC-MS and by HPLC-ESPI-MS. Our multicomponent system (including the identification and quantification of sugars, sugar alcohols, and several members of various homologous series of acids, anthraquinones and flavonoids) has been extended to the analysis of lignan glycosides and to the free lignans. Reproducibilities in the quantitation of lignans in plant matrices, as averages on GC and HPLC basis, varied between 0.9% and 11% (RSD). The distribution

  3. Extraction of carbamate pesticides in fruit samples by graphene reinforced hollow fibre liquid microextraction followed by high performance liquid chromatographic detection.

    Science.gov (United States)

    Ma, Xiaoxing; Wang, Juntao; Wu, Qiuhua; Wang, Chun; Wang, Zhi

    2014-08-15

    Graphene reinforced hollow fibre liquid phase microextraction combined with high performance liquid chromatography-diode array detection was developed for the determination of some carbamate pesticides (metolcarb, carbaryl, isoprocarb, and diethofencarb) in fruit samples. The main parameters that affect the extraction efficiency for the carbamates were investigated. Under the optimum conditions, a good linearity was observed in the range of 1.0-100.0 ng g(-1) for carbaryl and 3.0-100.0 ng g(-1) for the other three analytes, with the correlation coefficients (r) of 0.9965-0.9993. The limits of detection of the method ranged from 0.2 to 1.0 ng g(-1). The relative standard deviations were in the range from 6.2% to 7.8%. The results indicated that the developed method is sensitive and efficient for the determination of the carbamate pesticides in fruit samples. Copyright © 2014 Elsevier Ltd. All rights reserved.

  4. Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Nakamoto, Akihiro [Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825 (Japan); Nishida, Manami [Hiroshima University Technical Center, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan); Saito, Takeshi [Department of Emergency and Critical Care Medicine, Tokai University School of Medicine, Shimokasuya 143, Isehara, Kanagawa 259-1143 (Japan); Kishiyama, Izumi; Miyazaki, Shota [GL Sciences Inc., Sayamagahara 237-2, Iruma, Saitama 358-0032 (Japan); Murakami, Katsunori [Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825 (Japan); Nagao, Masataka [Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan); Namura, Akira, E-mail: namera@hiroshima-u.ac.jp [Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan)

    2010-02-19

    A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d{sub 5} was used as an internal standard. The linear ranges were 0.01-5.0 {mu}g mL{sup -1} for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 {mu}g mL{sup -1} for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation {>=}0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 {mu}g mL{sup -1} of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio {>=} 3) in urine was 5 ng mL{sup -1} for MA and MDMA and 10 ng mL{sup -1} for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation.

  5. Gas-chromatographic determination of aluminum in catalytic systems

    Energy Technology Data Exchange (ETDEWEB)

    Astapova, T.I.; Kutepova, A.I.; Frolova, O.D.

    1987-11-10

    The authors studied conditions for the chromatographic determination of aluminum in the form of a complex with pentane-2,4-dione in pilot plant-produced samples of GIAP-16, GIAP-16-2, SPM catalysts, talums and kaolins, aluminum oxides, and hydroxides. The influence of Zn, Mg, Ca, Na, Ni, Ti, and Mn on the extraction and the chromatographic determination of aluminum was studied.

  6. Simple liquid chromatographic method for the rapid and simultaneous determination of propoxur and its major metabolite isopropoxy phenol in rat blood and urine using solid-phase extraction.

    Science.gov (United States)

    Suma, Ramagiri; Sarin, R K; Saiprakash, P K; Ramakrishna, Sistla

    2005-10-01

    This research paper describes the development and validation of an analytical method for the simultaneous determination of propoxur and isopropoxy phenol (IPP, a major metabolite) in both blood and urine of rat using reversed-phase high-performance liquid chromatography (HPLC) employing solid-phase extraction (SPE). Sample purification was performed using a weak cation-exchange cartridge (Isolute CBA). Separation was achieved by HPLC with UV detection at 270 nm. Recoveries of propoxur and IPP from blood and urine by SPE exceeded 85%. The validated calibration range for propoxur is from 0.5 to 100 microg/L and 2 to 100 microg/L for IPP in both rat blood and urine. The limit of quantitation for propoxur in blood and urine is 0.5 and 0.8 pg/L, respectively, and 2.0 and 4.2 microg/L, respectively, for IPP. Validation results on specificity, sensitivity, linearity, precision, accuracy, and stability are shown. The applicability of the method was demonstrated by the analysis of urine and blood from rats that were orally fed propoxur at minimum dose.

  7. Non-chromatographic speciation of chromium at sub-ppb levels using cloud point extraction in the presence of unmodified silver nanoparticles.

    Science.gov (United States)

    López-García, Ignacio; Vicente-Martínez, Yesica; Hernández-Córdoba, Manuel

    2015-01-01

    The cloud point extraction (CPE) of silver nanoparticles (AgNPs) by Triton X-114 allows chromium (III) ions to be transferred to the surfactant-rich phase, where they can be measured by electrothermal atomic absorption spectrometry. Using 20 mL sample and 50 μL Triton X-114 (30% w/v), the enrichment factor was 1150, and calibration graphs were obtained in the 5-100 ng L(-1) chromium range in the presence of 5 µg L(-1) AgNPs. Speciation of trivalent and hexavalent chromium was achieved by carrying out two CPE experiments, one of them in the presence of ethylenediaminetetraacetate. While in the first experiment, in absence of the complexing agent, the concentration of total chromium was obtained, the analytical signal measured in the presence of this chemical allowed the chromium (VI) concentration to be measured, being that of chromium (III) calculated by difference. The reliability of the procedure was verified by using three standard reference materials before applying to water, beer and wine samples.

  8. Resin composites

    DEFF Research Database (Denmark)

    Benetti, Ana Raquel; Peutzfeldt, Anne; Lussi, Adrian;

    2014-01-01

    OBJECTIVE: To investigate how the modulus of elasticity of resin composites influences marginal quality in restorations submitted to thermocyclic and mechanical loading. METHODS: Charisma, Filtek Supreme XTE and Grandio were selected as they were found to possess different moduli of elasticity...... of resin composite (p=0.81) on the quality of dentine margins was observed, before or after loading. Deterioration of all margins was evident after loading (p....008). CONCLUSIONS: The resin composite with the highest modulus of elasticity resulted in the highest number of gap-free enamel margins but with an increased incidence of paramarginal enamel fractures. CLINICAL SIGNIFICANCE: The results from this study suggest that the marginal quality of restorations can...

  9. Liquid Chromatographic Determination of Alternaria Toxins in Carrots

    NARCIS (Netherlands)

    Solfrizzo, M.; Girolamo, De A.; Vitti, C.; Bulk, van den R.W.

    2004-01-01

    A liquid chromatographic (LC) method was developed for the determination of Alternaria radicina and A. alternata toxins in carrots. Toxins were extracted from carrot with an acidified mixture of water¿methanol¿acetonitrile. The filtered extract was divided in 2 parts that were purified by

  10. Report on use of XAD resins in racing chemistry.

    Science.gov (United States)

    Johnston, G. H.

    1976-01-01

    This report comprises a summary of the work done with XAD resin extraction by racing chemists and reported in the Association of Official Racing Chemists publications. It is apparent that the use of XAD resins is becoming more popular in racing laboratories as a technique for routine screening and also for the extraction of certain conjugated drugs. Most laboratories employ variations on the original Brinkmann Drug-Skreen Technique. Comparisons of the efficiency of extraction of drugs from horse urine by XAD-2 resin and by chloroform column extraction indicate that some drugs can be extracted with equal or greater efficiency by the resin technique. PMID:1000159

  11. The Effect of Aloe Vera, Pomegranate Peel, Grape Seed Extract, Green Tea, and Sodium Ascorbate as Antioxidants on the Shear Bond Strength of Composite Resin to Home-bleached Enamel

    Directory of Open Access Journals (Sweden)

    Farahnaz Sharafeddin

    2015-12-01

    Full Text Available Statement of the Problem: Immediate application of bonding agent to home- bleached enamel leads to significant reduction in the shear bond strength of composite resin due to the residual oxygen. Different antioxidant agents may overcome this problem. Purpose: This study aimed to assess the effect of different antioxidants on the shear bond strength of composite resin to home-bleached. Materials and Method: Sixty extracted intact human incisors were embedded in cylindrical acrylic resin blocks (2.5×1.5 cm, with the coronal portion left out of the block. After bleaching the labial enamel surface with 15% carbamide peroxide, they were randomly divided into 6 groups (n=10. Before performing composite resin restoration by using a cylindrical Teflon mold (5×2 mm, each group was treated with one of the following antioxidants: 10% sodium ascorbate solution, 10% pomegranate peel solution, 10% grape seed extract, 5% green tea extract, and aloe vera leaf gel. One group was left untreated as the control. The shear bond strength of samples was tested under a universal testing machine (ZwickRoell Z020. The shear bond strength data were analyzed by one-way ANOVA and post hoc Tukey tests (p< 0.05. Results: No significant difference existed between the control and experimental groups. Moreover, there was no statistically significant difference between the effects of different antioxidants on the shear bond strength of bleached enamel. Conclusion: Different antioxidants used in this study had the same effect on the shear bond strength of home-bleached enamel, and none of them caused a statistically significant increase in its value.

  12. Flavylium chromophores as species markers for dragon's blood resins from Dracaena and Daemonorops trees.

    Science.gov (United States)

    Sousa, Micaela M; Melo, Maria J; Parola, A Jorge; Seixas de Melo, J Sérgio; Catarino, Fernando; Pina, Fernando; Cook, Frances E M; Simmonds, Monique S J; Lopes, João A

    2008-10-31

    A simple and rapid liquid chromatographic method with diode-array UV-vis spectrophotometric detection has been developed for the authentication of dragon's blood resins from Dracaena and Daemonorops trees. Using this method it was discovered that the flavylium chromophores, which contribute to the red colour of these resins, differ among the species and could be used as markers to differentiate among species. A study of parameters, such as time of extraction, proportion of MeOH and pH, was undertaken to optimise the extraction of the flavyliums. This method was then used to make extracts from samples of dragon's blood resin obtained from material of known provenance. From the samples analysed 7,6-dihydroxy-5-methoxyflavylium (dracorhodin), 7,4'-dihydroxy-5-methoxyflavylium (dracoflavylium) and 7,4'-dihydroxyflavylium were selected as species markers for Daemonorops spp., Dracaena draco and Dracaena cinnabari, respectively. The chromatograms from these samples were used to build an HPLC-DAD database. The ability to discriminate among species of dragon's blood using the single marker compounds was compared with a principal components analysis of the chromatograms in the HPLC-DAD database. The results from the HPLC-DAD method based on the presence of these flavylium markers was unequivocal. The HPLC-DAD method was subsequently applied to 37 samples of dragon blood resins from the historical samples in the Economic Botany Collection, Royal Botanic Gardens, Kew. The method identified anomalies in how samples in this collection had been labelled. It is clear that the method can be used to evaluate the provenance of samples used in different areas of cultural heritage. It also could be used to monitor the trade of endangered species of dragon's blood and the species being used in complex formulations of traditional Chinese medicine.

  13. Determination of 63Ni and 59Ni in spent ion-exchange resin and activated charcoal from the IEA-R1 nuclear research reactor.

    Science.gov (United States)

    Taddei, M H T; Macacini, J F; Vicente, R; Marumo, J T; Sakata, S K; Terremoto, L A A

    2013-07-01

    A radiochemical method has been adapted to determine (59)Ni and (63)Ni in samples of radioactive wastes from the water cleanup system of the IEA-R1 nuclear research reactor. The process includes extraction chromatographic resin with dimethylglyoxime (DMG) as a functional group. Activity concentrations of (59)Ni and (63)Ni were measured, respectively, by X-ray spectrometry and liquid scintillation counting, whereas the chemical yield was determined by ICP-OES. The average ratio of measured activity concentrations of (63)Ni and (59)Ni agree well with theory. Copyright © 2013 Elsevier Ltd. All rights reserved.

  14. Scintillating 99Tc Selective Ion Exchange Resins

    Energy Technology Data Exchange (ETDEWEB)

    Mitchell Greenhalgh; Richard D. Tillotson

    2012-07-01

    Scintillating technetium (99Tc) selective ion exchange resins have been developed and evaluated for equilibrium capacities and detection efficiencies. These resins can be utilized for the in-situ concentration and detection of low levels of pertechnetate anions (99TcO4-) in natural waters. Three different polystyrene type resin support materials were impregnated with varying amounts of tricaprylmethylammonium chloride (Aliquat 336) extractant, several different scintillating fluors and wavelength shifters. The prepared resins were contacted batch-wise to equilibrium over a wide range of 99TcO4- concentrations in natural water. The measured capacities were used to develop Langmuir adsorption isotherms for each resin. 99Tc detection efficiencies were determined and up to 71.4 ± 2.6% was achieved with some resins. The results demonstrate that a low level detection limit for 99TcO4- in natural waters can be realized.

  15. Solid-Phase Extraction of Trace Amounts of Uranium(VI in Environmental Water Samples Using an Extractant-Impregnated Resin Followed by Detection with UV-Vis Spectrophotometry

    Directory of Open Access Journals (Sweden)

    Ahmad Hosseini-Bandegharaei

    2013-01-01

    Full Text Available A stable extractant-impregnated resin (EIR containing Chrome Azurol B was prepared using Amberlite XAD-2010 as a porous polymeric support. The new EIR was employed for trace separation and preconcentration of U(VI ion followed by spectrophotometric determination with the arsenazo III procedure. CAB/XAD-2010 exhibited excellent selectivity for U(VI ion over coexisting ions. Experimental parameters including pH, contact time, shaking speed, and ionic strength were investigated by batch extraction methods. Maximum sorption of U(VI ions occurred at pH 4.3–6.9. The capacity of EIR was found to be 0.632 mmol·g−1. Equilibrium was reached in 25 min and the loading half-time, t1/2, was less than 6 min. The equilibrium adsorption isotherm of U(VI was fitted with the Langmuir adsorption model. In addition, a column packed with CAB/XAD-2010 was used for column-mode separation and preconcentration of U(VI ion. For the optimization of the dynamic procedure, effects of sample volume, sample and eluent flow rate, eluent concentration, and its volume were investigated. The preconcentration factors for U(VI were found out to be 160. But, for convenience, a preconcentration factor of 150 was utilized for the column-mode preconcentration. The dynamic procedure gave a detection limit of 5.0×10-10 mol·L−1 (0.12 μg·L−1 for U(VI ion. The proposed dynamic method showed good performance in analyzing environmental water samples.

  16. Use of Modified Phenolic Thyme Extracts (Thymus vulgaris) with Reduced Polyphenol Oxidase Substrates as Anthocyanin Color and Stability Enhancing Agents.

    Science.gov (United States)

    Aguilar, Oscar; Hernández-Brenes, Carmen

    2015-12-14

    Residual enzymatic activity in certain foods, particularly of polyphenoloxidase (PPO), is responsible for the majority of anthocyanin degradation in food systems, causing also parallel losses of other relevant nutrients. The present work explored the feasibility of modifying phenolic profiles of thyme extracts, by use of chromatographic resins, to obtain phenolic extracts capable of enhancing anthocyanin colour and stability in the presence of PPO activity. Results indicated that pretreatment of thyme extracts with strong-anion exchange resins (SAE) enhanced their copigmentation abilities with strawberry juice anthocyanins. Phenolic chromatographic profiles, by HPLC-PDA, also demonstrated that thyme extracts subjected to SAE treatments had significantly lower concentrations of certain phenolic compounds, but extracts retained their colour enhancing and anthocyanin stabilization capacities though copigmentation. Additional testing also indicated that SAE modified extract had a lower ability (73% decrease) to serve as PPO substrate, when compared to the unmodified extract. Phenolic profile modification process, reported herein, could be potentially used to manufacture modified anthocyanin-copigmentation food and cosmetic additives for colour-stabilizing applications with lower secondary degradation reactions in matrixes that contain PPO activity.

  17. Use of Modified Phenolic Thyme Extracts (Thymus vulgaris with Reduced Polyphenol Oxidase Substrates as Anthocyanin Color and Stability Enhancing Agents

    Directory of Open Access Journals (Sweden)

    Oscar Aguilar

    2015-12-01

    Full Text Available Residual enzymatic activity in certain foods, particularly of polyphenoloxidase (PPO, is responsible for the majority of anthocyanin degradation in food systems, causing also parallel losses of other relevant nutrients. The present work explored the feasibility of modifying phenolic profiles of thyme extracts, by use of chromatographic resins, to obtain phenolic extracts capable of enhancing anthocyanin colour and stability in the presence of PPO activity. Results indicated that pretreatment of thyme extracts with strong-anion exchange resins (SAE enhanced their copigmentation abilities with strawberry juice anthocyanins. Phenolic chromatographic profiles, by HPLC-PDA, also demonstrated that thyme extracts subjected to SAE treatments had significantly lower concentrations of certain phenolic compounds, but extracts retained their colour enhancing and anthocyanin stabilization capacities though copigmentation. Additional testing also indicated that SAE modified extract had a lower ability (73% decrease to serve as PPO substrate, when compared to the unmodified extract. Phenolic profile modification process, reported herein, could be potentially used to manufacture modified anthocyanin-copigmentation food and cosmetic additives for colour-stabilizing applications with lower secondary degradation reactions in matrixes that contain PPO activity.

  18. Comparison of Cashew Nut Shell Liquid (CNS Resin with Polyester Resin in Composite Development

    Directory of Open Access Journals (Sweden)

    C. C. Ugoamadi

    2013-12-01

    Full Text Available Natural resins can compete effectively with the synthetic ones in composite development. In this research, cashew nuts were picked and processed for the extraction of the resin content. The resin (natural resin so obtained was mixed with cobalt amine (accelerator, methyl ethyl ketone peroxide (catalyst to develop two sets of composite specimens – specimens without fibres and specimens reinforced with glass fibres. This method of sample specimen development was repeated with polyester (synthetic resin. Compressive and tensile strength tests conducted proved that composites developed with cashew nut shell liquid (CNSL resin were comparable to those developed with polyester resin. In the results, CNSL has an ultimate compressive strength of 55MPa compared to that of polyester resin with an ultimate strength of 68MPa. The result of tensile strength proved cashew nut shell liquid resin (with ultimate strength of 44MPa to be better than polyester resin with 39MPa as ultimate tensile strength. This means that natural resins could be a better substitute for the synthetic ones when the required quantities of fibers (reinforcements and fillers are used in the fibre-reinforced plastic composite developments.

  19. First example of diglycolamide-grafted resins: synthesis, characterization, and actinide uptake studies

    NARCIS (Netherlands)

    Mohapatra, Prasanta; Ansari, Seraj A.; Iqbal, M.; Huskens, Jurriaan; Verboom, Willem

    2014-01-01

    Two diglycolamide (DGA)-functionalized chelating extraction resins were prepared for the first time by grafting onto a silica matrix and were evaluated for their actinide ion uptake behavior. The resins with one and two DGA moieties, termed as resin-I and resin-II, were quite efficient for the

  20. First example of diglycolamide-grafted resins: synthesis, characterization, and actinide uptake studies

    NARCIS (Netherlands)

    Mohapatra, Prasanta; Ansari, Seraj A.; Iqbal, M.; Huskens, Jurriaan; Verboom, Willem

    2014-01-01

    Two diglycolamide (DGA)-functionalized chelating extraction resins were prepared for the first time by grafting onto a silica matrix and were evaluated for their actinide ion uptake behavior. The resins with one and two DGA moieties, termed as resin-I and resin-II, were quite efficient for the actin

  1. 大孔树脂对桑黄多糖提取液中色素的吸附与解吸特性研究%Adsorption and desorption characteristics of macroporous resins to pigments of Phellinus linteus polysaccharide extraction

    Institute of Scientific and Technical Information of China (English)

    秦俊哲; 程伟; 杜军国

    2013-01-01

    In order to select a kind of resin which is better on purification of polysaccharide extracted from the fruiting bodies of Phellinus Igniarius. Compared the effects of DA201 and other 5 kinds of macroporous resins in the proessing of decolorization and removal effects of liquid protein. On static adsorption and desorption experiments, select the DA201 resin for static adsorption kinetics and desorption characteristics, investigated the resin saturated adsorption, decolorization rate, protein removing rate and total sugar retention rate. The results show: DA201 resin showed a good effects of deproteinization and decolorization, and total sugar retention rate was high. For the specific polysaccharide extraction, flow rate at 1. 0 mL/min, DA201 resin column to make protein and pigment adsorption reached saturation, need continuous sampling 10 multiple column volume (BV) at least, distilled water and 50% ethanol elution desorption effects was suitable. DA201 resin was suitable for the decolorization of polysaccharide,In order to make full use of DA201 resin adsorption properties, the string column method can be considered in industrial production.%为了选择对桑黄多糖提取液纯化效果较好的树脂,比较了DA201等5种大孔吸附树脂对桑黄多糖提取液的脱色和除蛋白质效果.对5种树脂进行静态吸附与解吸试验,选择DA201树脂研究静态吸附动力学曲线及其解吸特性,考察树脂的饱和吸附量、脱色率、蛋白质脱除率及总糖的保留率.DA201树脂对桑黄多糖提取液中的蛋白质和色素的吸附较多,表明其脱蛋白和脱色效果较好,且多糖的回收率较高.对于特定的多糖提取液,流速1.0 mL/min,过DA201树脂柱要使蛋白质和色素达到吸附饱和,需要连续进样10多个柱床体积(BV),蒸馏水和50%乙醇洗脱解吸效果均较好.DA201树脂较适于桑黄多糖提取液的初步纯化,为了充分发挥DA201树脂的吸附性能,工业生产上可考虑采用串柱法.

  2. 大孔吸附树脂富集枸杞子中总黄酮的工艺研究%Extraction Research of Total Flavonoids from Lycii Fructus by Macroporous Adsorption Resin

    Institute of Scientific and Technical Information of China (English)

    胡晓莲; 张华

    2013-01-01

    Objective To study the optimum extraction technology of flavonoids from Lycii fructus by macroporous adsorption resin and improve the purity of product. Methods Optimizing suitable macroporous adsorption resin and process parameters, and using colorimetric method for the determination of Lycii fructus. Results The appropriate adsorption resin was DA-201, sample loading was 10bed volume (BV), sample concentration was 15 mg/mL, the flow rate was lBV /h, pH 3; desorption experimental elution agent was 40 % ethanol, and amount of ethanol was 8 BV. The yield was 75.85 %, and the purity of flavonoids was 35.70 %. Conclusion Under the certain process condition, flavonoids can be effective extracted and purified by DA201 type resin, and the resin can be reused with a good application prospect.%  目的筛选富集纯化枸杞子中总黄酮的大孔吸附树脂并确立其工艺参数,以提高产品纯度。方法优选大孔吸附树脂,并考察其工艺参数,采用比色法测定枸杞含量。结果筛选合适的吸附树脂DA-201,得到最佳的工艺参数为:上样量10柱床体积(BV),上样液浓度15 mg/mL,上样液流速1 BV/h,上样液pH3;解吸洗脱剂乙醇浓度为40%,乙醇用量8 BV。富集纯化总黄酮得率75.85%,总黄酮纯度35.70%。结论 DA-201型树脂在所确定的工艺条件下富集纯化总黄酮效果良好,树脂可重复利用,成本低,具有很好的应用前景。

  3. Derivatization in gas chromatographic determination of phenol and aniline traces in aqueous media

    Science.gov (United States)

    Gruzdev, I. V.; Zenkevich, I. G.; Kondratenok, B. M.

    2015-06-01

    Substituted anilines and phenols are the most common hydrophilic organic environmental toxicants. The principles of gas chromatographic determination of trace amounts of these compounds in aqueous media at concentrations extractive preconcentration and selective chromatographic detection. Among the known reactions, this condition is best met by electrophilic halogenation of compounds at the aromatic moiety. The bibliography includes 177 references.

  4. Chromatographic fingerprints analysis for evaluation of Ginkgo Biloba products

    Science.gov (United States)

    The leaf extract of Ginkgo biloba has purported value for improving mental capacities in Alzheimer’s patients. The flavonoids and the terpene lactones are considered to be the two main active components that influence human health. This paper compared an LC/UV chromatographic fingerprint method wi...

  5. Chemically modified polymeric resins for separation of cations, organic acids, and small polar moleculea by high performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Morris, John B. [Iowa State Univ., Ames, IA (United States)

    1993-07-01

    This thesis is divided into 4 parts: a review, ion chromatography of metal cations on carboxylic resins, separation of hydrophilic organic acids and small polar compounds on macroporous resin columns, and use of eluent modifiers for liquid chromatographic separation of carboxylic acids using conductivity detection.

  6. Liquid chromatographic determination of furazolidone in shrimp.

    Science.gov (United States)

    Stehly, G R; Plakas, S M; el Said, K R

    1994-01-01

    A liquid chromatographic (LC) method was developed for the quantitation of furazolidone residues in shrimp muscle. The shrimp homogenate (1.0 g) is extracted with acetonitrile, and the extract is taken to dryness. The residue is dissolved in acetonitrile, and the solution is passed through alumina and C18 cleanup columns. The eluate is taken to dryness and reconstituted in a suitable solvent for reversed-phase (C18) LC with UV detection at 365 nm. Recoveries of furazolidone from shrimp homogenates spiked from 5 to 80 ng/g ranged from 74.3 to 79.7%, and relative standard deviations (RSDs) were 5.0-8.9%. RSDs for incurred furazolidone quantitated at 5.9 and 9.2 ng/g were 6.6 and 7.6%, respectively.

  7. Novel materials and methods for solid-phase extraction and liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Ambrose, Diana [Iowa State Univ., Ames, IA (United States)

    1997-06-24

    This report contains a general introduction which discusses solid-phase extraction and solid-phase micro-extraction as sample preparation techniques for high-performance liquid chromatography, which is also evaluated in the study. This report also contains the Conclusions section. Four sections have been removed and processed separately: silicalite as a sorbent for solid-phase extraction; a new, high-capacity carboxylic acid functionalized resin for solid-phase extraction; semi-micro solid-phase extraction of organic compounds from aqueous and biological samples; and the high-performance liquid chromatographic determination of drugs and metabolites in human serum and urine using direct injection and a unique molecular sieve.

  8. Gas chromatographic analysis of simmondsins and simmondsin ferulates in jojoba meal.

    Science.gov (United States)

    Van Boven, M; Holser, R; Cokelaere, M; Flo, G; Decuypere, E

    2000-09-01

    A capillary gas chromatographic method was developed for the simultaneous determination of simmondsins and simmondsin ferulates in jojoba meal, in detoxified jojoba meal, in jojoba meal extracts, and in animal food mixtures.

  9. Resin Catalyst Hybrids

    Institute of Scientific and Technical Information of China (English)

    S. Asaoka

    2005-01-01

    @@ 1Introduction: What are resin catalyst hybrids? There are typically two types of resin catalyst. One is acidic resin which representative is polystyrene sulfonic acid. The other is basic resin which is availed as metal complex support. The objective items of this study on resin catalyst are consisting of pellet hybrid, equilibrium hybrid and function hybrid of acid and base,as shown in Fig. 1[1-5].

  10. Two-step Resin Adsorption for Purification of Stevia Glycosides from Stevia Rebaudiana Aqueous Extract%两步树脂法从甜叶菊水提液中纯化甜菊糖苷

    Institute of Scientific and Technical Information of China (English)

    唐乐乐; 叶发银; 杨瑞金; 华霄; 赵伟; 张文斌

    2012-01-01

    采用两步树脂法从甜叶菊水提液中提取纯化甜菊糖苷。第一步主要是脱色,通过比较大孔树脂D293、D296、JN-1、JN-2、D890和D201处理甜叶菊水提液的脱色率、甜菊糖苷保留率和解吸性能,发现JN-1的效果最好。在优化条件下,甜叶菊水提液经JN-1处理,甜菊糖苷纯度由原来的42.65%提高到67.33%,收率达到84.87%;第二步的主要目的是提高产品纯度,通过比较大孔树脂AB-8、JNF-1、X-5、NKA-II和D101对甜菊糖苷的吸附-解吸性能和得到的纯化液的甜菊糖苷纯度,发现JNF-1的效果最好。在优化的条件下,JN-1处理后的甜菊糖苷溶液进一步采用JNF-1吸附,溶液的甜菊糖苷纯度提高至92.92%,收率91.08%。%A new method for purification of steviol glycosides from Stevia Rebaudiana crude extracts by macro- porous adsorption resin (MAR) was systematically investigated. The purification procedure consisted of two steps. In the first step, the main purpose was decolorization, and several types of macroporous resins including D293, D296, JN-1, JN-2, D890 and D201 were used in order to choose the best resin. JN-1 resin was selected according to their decolorization ratio, the retention of steviol glycosides ratio and desorption ratio. In order to increase the purity, a sec- ond step of refining was added by screening various types of macroporous resins (AB-8, JNF-1, X-5, NKA-II and D101). The results demonstrated that JNF-1 resin was the most suitable resin. The purity of steviol glycosides after the first step JN-1 was from 42.65% to 67.33% with a recovery of 84.87%. The purity of steviol glycosides in- creased to 92.92% with a recovery of 91.08% after the second step JNF-1.

  11. Preliminary Study of Performance of TTA Resin

    Institute of Scientific and Technical Information of China (English)

    HUANG; Kun; MAO; Guo-shu

    2013-01-01

    TTA(thenoyl trifluoroacetone)extraction can effectively remove large amounts of uranium in the analysis of trace neptunium in the presence of large amounts of uranium.While it is not conducive to achieve the automation of the rapid analysis of neptunium with the TTA solution,the TTA resin was prepared and its properties were studied in this work.TTA resin in this work was a kind of mixture combining styrene-divinylbenzene skeleton with TTA

  12. Fractionation of fulvic acid extracted from lake sediments using XAD resins and the metal complexing ability. Kosho taisekibutsuchu kara chushutsusareta furubosan no XAD jushi kyuchaku ni yoru bunkaku to sakka noryoku

    Energy Technology Data Exchange (ETDEWEB)

    Usui, K.; Kishino, T. (Ube Colege, Yamaguchi (Japan). laboratory of Environmental Science); Higashi, T.; Shindo, H.; Marumoto, T. (Yamaguchi University, Yamaguchi (Japan). Faculty of Agriculture)

    1993-10-10

    Fulvic acid was extracted from lake sediments, and given an adsorption treatment with Amberlite XAD-2 and XAD-8 resins. The copper complexing ability of the treated liquid was discussed using a two binding site model. As a result of deriving the condition stability constants of the treated liquid, it was learned that the fulvic acid can be divided largely into two kinds with different complexing ability by about 100 times, having log K1 = 6.33 to 7.12 and log K2 = 4.35 to 4.66. The majority was composed of fulvic acid having weak complexing ability. The resin treatment separated the fulvic acid nearly completely into an adsorption fraction and a non-adsorption fraction. The fulvic acid in the adsorption fraction showed very little complexing ability. On the other hand, the fulvic acid in the non-adsorption fraction, which is nearly colorless, exhibited a complexing ability of 33 to 45 [mu] mol/g as copper complexing capacity. Further, the amount of the non-adsorption fraction appeared to account for 52% to 69% of the total fulvic acid as judged from the TOC value. 19 refs., 1 fig., 1 tab.

  13. Determination of Some Trace Metals in Environmental Samples by Flame AAS Following Solid Phase Extraction with Amberlite XAD-2000 Resin after Complexing with 8-Hydroxyquinoline

    Institute of Scientific and Technical Information of China (English)

    DURAN Celal; SENTURK H.Basri; GUNDOGDU Ali; BULUT V.Numan; EICi Latif; SOYLAK Mustafa; TUFEKCI,Mehmet; UYGUR Yaprak

    2007-01-01

    A procedure for preconcentration of Mn(Ⅱ), Fe(Ⅱ), Co(Ⅱ), Cu(Ⅱ), Cd(Ⅱ), Zn(Ⅱ), Pb(Ⅱ) and Ni(Ⅱ) based on retention of their complexes with 8-hydroxyquinoline (HQ) on Amberlite XAD-2000 resin in a column was proposed for the analysis of environmental samples by flame AAS. Various parameters such as pH, eluent type, volume,concentration, flow rate and volume of sample solution, and matrix interference effect on the retention of the metal ions were investigated. The optimum pHs for the retention of metal complexes in question were about 6 except for Mn2+ for whose value is 8. The loading capacity of the adsorbent for these metals and their recoveries from the resin under the optimum conditions were in the range 6.82-9.26 mg·g-1 and 95%-101%, respectively. The enrichment factor was calculated as 100 and the limit of detection was in the range 0.3-2.2 μg·L 1 (n=20, blank+3s). The proposed enrichment method was applied to tap water, stream water and vegetable samples. The validation of the procedure was carried out by analysis of certified reference material and standard addition. The analytes were determined with a relative standard deviation lower than 6% in all samples.

  14. OPTIMIZED DETERMINATION OF TRACE JET FUEL VOLATILE ORGANIC COMPOUNDS IN HUMAN BLOOD USING IN-FIELD LIQUID-LIQUID EXTRACTION WITH SUBSEQUENT LABORATORY GAS CHROMATOGRAPHIC-MASS SPECTROMETRIC ANALYSIS AND ON-COLUMN LARGE VOLUME INJECTION

    Science.gov (United States)

    A practical and sensitive method to assess volatile organic compounds (VOCs) from JP-8 jet fuel in human whole blood was developed by modifying previously established liquid-liquid extraction procedures, optimizing extraction times, solvent volume, specific sample processing te...

  15. An exploration of experimental parameters in the analysis of epoxy resin by reverse phase liquid chromatography.

    Science.gov (United States)

    Twichell, J E; Walker, J Q; Maynard, J B

    1979-05-01

    Reverse phase liquid chromatographic methods have been developed for the quality control of epoxy resin formulations. The results show that different formulations require different instrumental parameters for optimun separation and detection. Operating parameters required for the analysis of complex mixtures of epoxy resins, which include curing agents and diluents, are described in this paper. Parameters found to be critical are column temperature, solvent flow rate and gradient, and detector wavelength. Microprocessor parameters required to obtain reproducible data are also discussed.

  16. Monosized macroporous resins with epoxy groups and their structure and gel chromatography properties

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    The monosized macroporous-polymer beads based on cross-linked poly(glycidyl methacrylate) have been synthesized by a new improving method--combining dispersion polymerization with swelling polymerization and polymeric solution porogens. The structure and gel chromatographic properties of the resins have been studied. The resins as matrix materials of various types of high performance liquid chromatography (HPLC) packings possess excellent separation properties

  17. Resin collection and social immunity in honey bees

    Science.gov (United States)

    We determined if the use of resins, complex plant secretions with diverse antimicrobial properties, acts as a colony-level immune defense by honey bees. Colonies were enriched with extracts of Brazilian or Minnesotan propolis (a bee mixture of resins and wax) or were left as controls. We measured ge...

  18. Guayule resin detection and influence on guayule rubber

    Science.gov (United States)

    Guayule (Parthenium argentatum) is a natural rubber (cis-1,4-polyisoprene) producing crop, native to North America. Guayule also produces organic resins, complex mixtures of terpenes, triglycerides, guayulins, triterpenoids and other components. During natural rubber extraction, guayule resins can b...

  19. Resin screening for the removal of pyridine-derivatives from waste-water by solvent impregnated resin technology

    NARCIS (Netherlands)

    Bokhove, J.; Schuur, B.; Haan, de A.B.

    2013-01-01

    The selective removal of pyridine derivatives by solvent impregnated resins has been studied. A solvent impregnated resin consists of a macro-porous particle that is impregnated with a solvent. This technology allows the use liquid–liquid extraction in fixed-bed operation, and prevents problems like

  20. 21 CFR 175.380 - Xylene-formaldehyde resins condensed with 4,4′-isopropylidenediphenol-epichlorohydrin epoxy resins.

    Science.gov (United States)

    2010-04-01

    ... required in the production of the resins or added to impart desired physical and technical properties. The optional adjuvant substances may include resins produced by the condensation of allyl ether of mono-, di... percent (by volume) ethyl alcohol in distilled water at 160 °F for 4 hours yields total extractives not...

  1. 改性脂质阴离子交换树脂脱酸工艺的优化%Optimization of Modified Lipid Deacidification with Liquid-liquid Extraction and Anion Exchange Resin

    Institute of Scientific and Technical Information of China (English)

    袁璐; 姜土; 吴炜亮; 朱文亮; 黄秋研; 郑建仙

    2012-01-01

    Deacidification of modified Chinese tallow oil has been investigated using a strategy consisted of twice liquid-liquid extraction and deacidification process of D202 polymeric anion ion exchange.The effects of material ratio,reaction time and dosage of resin were investigated by central composite response design(CCRD) to obtain the optimum process.The optimum parameters were material ratio1:4.91,reaction time 7.28h,dosage of resin 9.23g.Under these optimum process parameters,acid value of modified lipid reduced to 0.11 mgKOH/g after deacidification of D202 resin.The sequences of three factors influenced on the deacidification of modified lipid were dosage of resinextraction timematerial ratio.%以经过2次液-液萃取脱酸的乌桕脂为目标油脂,研究了D202型大孔阴离子交换树脂脱酸工艺的可行性。采用中心组合旋转响应面设计(CCRD)对树脂脱酸工艺中的物料比、反应时间、树脂用量3个工艺参数进行优化,得到阴离子交换树脂脱酸的适宜工艺条件是:改性脂质与正己烷的物料比为1∶4.91,反应时间控制在7.28 h,树脂用量为9.23 g。在此条件下脱酸后,改性脂质的酸价可降低至0.11 mgKOH/g。3个因素对树脂脱酸效果的影响次序为,树脂用量〉反应时间〉物料比。

  2. Influence of curing rate of resin composite on the bond strength to dentin

    DEFF Research Database (Denmark)

    Benetti, Ana Raquel; Asmussen, E; Peutzfeldt, A

    2007-01-01

    This study determined whether the strength with which resin composite bonds to dentin is influenced by variations in the curing rate of resin composites. Resin composites were bonded to the dentin of extracted human molars. Adhesive (AdheSE, Ivoclar Vivadent) was applied and cured (10 seconds...

  3. EXTRACT

    DEFF Research Database (Denmark)

    Pafilis, Evangelos; Buttigieg, Pier Luigi; Ferrell, Barbra

    2016-01-01

    The microbial and molecular ecology research communities have made substantial progress on developing standards for annotating samples with environment metadata. However, sample manual annotation is a highly labor intensive process and requires familiarity with the terminologies used. We have the...... and text-mining-assisted curation revealed that EXTRACT speeds up annotation by 15-25% and helps curators to detect terms that would otherwise have been missed.Database URL: https://extract.hcmr.gr/....

  4. Optimized determination of trace jet fuel volatile organic compounds in human blood using in-field liquid-liquid extraction with subsequent laboratory gas chromatographic-mass spectrometric analysis and on-column large-volume injection.

    Science.gov (United States)

    Liu, S; Pleil, J D

    2001-03-05

    A practical and sensitive method to assess volatile organic compounds (VOCs) from JP-8 jet fuel in human whole blood was developed by modifying previously established liquid-liquid extraction procedures, optimizing extraction times, solvent volume, specific sample processing techniques, and a new on-column large-volume injection method for GC-MS analysis. With the optimized methods, the extraction efficiency was improved by 4.3 to 20.1 times and the detection sensitivity increased up to 660 times over the standard method. Typical detection limits in the parts-per-trillion (ppt) level range were achieved for all monitored JP-8 constituents; this is sufficient for assessing human fuels exposures at trace environmental levels as well as occupational exposure levels. The sample extractions are performed in the field and only solvent extracts need to be shipped to the laboratory. The method is implemented with standard biological laboratory equipment and a modest bench-top GC-MS system.

  5. Extracting and purifying R-phycoerythrin from Mediterranean red algae Corallina elongata Ellis & Solander.

    Science.gov (United States)

    Rossano, R; Ungaro, N; D'Ambrosio, A; Liuzzi, G M; Riccio, P

    2003-03-20

    R-Phycoerythrin (R-PE) is a protein acting as a photosynthetic accessory pigment in red algae (Rodophyta). This protein has gained importance in many biotechnological applications in food science, immunodiagnostic, therapy, cosmetics, protein and cell labelling, and analytical processes. In this paper we report on a new, one step procedure for the extraction and purification of R-PE from a new source: the Mediterranean red algae Corallina elongata Ellis & Solander. This red algae contains mainly R-PE and is suitable for the production in culture. No other contaminating phycobiliproteins could be detected in the extracts. The method we propose for the purification is based on the use of hydroxyapatite, a chromatographic resin that can be produced in the laboratory at very low cost and can be used batch-wise with large amounts of extracts, alternative to chromatography, and therefore can be scaled up. Both the yield and the purity of R-PE are very good.

  6. Liquid chromatographic assay for dicloxacillin in plasma.

    Science.gov (United States)

    Alderete, Oscar; González-Esquivel, Dinora F; Del Rivero, L Misael; Castro Torres, Nelly

    2004-06-15

    A simple high-performance liquid chromatographic method for the determination of dicloxacillin in plasma has been developed. The method only requires 0.5 ml of plasma, phosphate buffer solution (pH = 4.7), acidification with 0.5N hydrochloride acid and liquid extraction with dichloromethane. Posterior evaporation of organic under nitrogen steam and redissolution in mobile phase is carried out. The analysis was performed on a Spherisorb C18 (5 microm) column, using methanol -0.05 M phosphate buffer, pH = 4.7 (75:25; v/v) as mobile phase, with ultraviolet detection at 220 nm. Results showed that the assay is sensitive: 0.5 microg/ml. The response is linear in the range of 0.5 - 10 microg/ml. Maximum inter-day coefficient of variation was 12.4%. Mean extraction recovery obtained was 96.95%. Stability studies showed that the loss was not higher than 10%, samples are stable at room temperature for 6 h, at -20 Celsius for 2 months, processed samples were stable at least for 24 h and also after two freeze-thaw cycles. The method has been used to perform pharmacokinetic and bioequivalence studies in humans.

  7. HPLC Characterization of Phenol-Formaldehyde Resole Resin Used in Fabrication of Shuttle Booster Nozzles

    Science.gov (United States)

    Young, Philip R.

    1999-01-01

    A reverse phase High Performance Liquid Chromatographic method was developed to rapidly fingerprint a phenol-formaldehyde resole resin similar to Durite(R) SC-1008. This resin is used in the fabrication of carbon-carbon composite materials from which Space Shuttle Solid Rocket Booster nozzles are manufactured. A knowledge of resin chemistry is essential to successful composite processing and performance. The results indicate that a high quality separation of over 35 peaks in 25 minutes were obtained using a 15 cm Phenomenex LUNA C8 bonded reverse phase column, a three-way water-acetonitrile-methanol nonlinear gradient, and LTV detection at 280 nm.

  8. Chromatographic separation of alkaline phosphatase from dental enamel

    DEFF Research Database (Denmark)

    Moe, D; Kirkeby, S; Salling, E

    1989-01-01

    Alkaline phosphatase (AP) was prepared from partly mineralized bovine enamel by extraction in phosphate buffer, centrifugation and various chromatographic techniques. Chromatofocusing showed that the enamel enzyme possessed five isoelectric points at the acid pH level ranging from pH 5.7 to pH 4.......4. Three enzyme peaks were eluted using low pressure chromatography with a Bio-gel column. With a HPLC gel filtration column the separation of the enamel extract resulted in only one peak with AP activity. The fractions of this peak were used to produce an antibody against bovine AP....

  9. Vibrational Spectroscopy of Chromatographic Interfaces

    Energy Technology Data Exchange (ETDEWEB)

    Jeanne E. Pemberton

    2011-03-10

    Chromatographic separations play a central role in DOE-supported fundamental research related to energy, biological systems, the environment, and nuclear science. The overall portfolio of research activities in the Separations and Analysis Program within the DOE Office of Basic Energy Sciences includes support for activities designed to develop a molecular-level understanding of the chemical processes that underlie separations for both large-scale and analytical-scale purposes. The research effort funded by this grant award was a continuation of DOE-supported research to develop vibrational spectroscopic methods to characterize the interfacial details of separations processes at a molecular level.

  10. Purification of total flavonoids from loquat leaves by macroporous resin and corresponding antioxidant capacity

    OpenAIRE

    Huang Suhua; Lin Biaosheng; Li Binbin; Tan Bi; Hong Yanping

    2017-01-01

    Flavonoids is one of the major active compounds in loquat leaves. In this study, the purification process of total flavonoids in loquat leaves by macroporous resin was researched and the antioxidant activity of total flavonoids was determined. The active compounds were extracted by 95% ethanol, and the total flavonoids was purified by macroporous resin. Comparing the static and dynamic adsorption and desorption characters of 6 macroporous resin, the best type of macroporous resin was determin...

  11. Occurrence of polycadinene in fossil and recent resins

    Science.gov (United States)

    Van Aarssen, B. G. K.; de Leeuw, J. W.; Collinson, M.; Boon, J. J.; Goth, K.

    1994-01-01

    Dammars produced by Dipterocarpaceae growing in Southeast Asia are partly composed of a macromolecule with a polycadinene structure. This polymer is the precursor of many specific compounds encountered in crude oils and sediment extracts from South Asia. Until recently there was no evidence for a more widespread geographical occurrence of this resinous polymer. Using different pyrolysis methods it is shown that the polymers present in a resinite from Utah, USA, and in resins contained in resin canals of Eocene fossil fruits from Germany and England are also polycadinenes. The fossil fruits were undoubtedly produced by ancient representatives of mastixioid Cornaceae, a group of plants which was widespread in the Tertiary of Europe and North America and which is not related to Dipterocarpaceae. These findings extend the known occurrence and origin of the sesquiterpenoid type resin polymer. It is to be expected that catagenetic products of these resin polymers should be present in oils, coals, and sediment extracts from areas outside Southeast Asia.

  12. [Radiopacity of composite resins].

    Science.gov (United States)

    Tamburús, J R

    1990-01-01

    The author studied the radiopacity of six composite resins, submitted to radiographic examination in standardized conditions, only with kilovoltage variations. Along with resins it was radiographed an aluminium penetrometer, to compare their optical densities. The results showed that kilovoltagem variations interfered in optical densities of the resins, being more pronounced in 50-55, 55-60 and 60-65 kilovoltages. Despite this, the relations of optical densities as compared with that of penetrometer steps kept unaltered most fo the kilovoltages used.

  13. Biocompatibility of composite resins

    OpenAIRE

    Sayed Mostafa Mousavinasab

    2011-01-01

    Dental materials that are used in dentistry should be harmless to oral tissues, so they should not contain any leachable toxic and diffusible substances that can cause some side effects. Reports about probable biologic hazards, in relation to dental resins, have increased interest to this topic in dentists. The present paper reviews the articles published about biocompatibility of resin-restorative materials specially resin composites and monomers which are mainly based on Bis-GMA and concern...

  14. Comparative study of resin sealant and resin modified glass ionomer as pit and fissure sealant

    Directory of Open Access Journals (Sweden)

    Shirin Malek

    2017-02-01

    Full Text Available The purpose of the present study was to compare the marginal integrity of resin modified glass ionomer cement with that of resin sealant, in vitro. Forty artificial pit and fissure cavities were prepared in occlusal surface of extracted premolar teeth by using ¼ round carbide bur. Cavities were condensed with artificial organic debris followed by cleaning with prophylaxis pumice brush and paste and then separated into two treatment groups. In Group A, 15 fissure cavities were sealed by resin sealant and in Group B, 15 fissure cavities were sealed by resin modified glass ionomer sealant. These specimens were subjected to thermo-cycling followed by dye penetration test. The remaining 5 cavities from each group were analyzed for debris score by the SEM. The results of the microleakage test showed that the efficacy of preventing microleakage of samples sealed by resin modified glass ionomer sealant was higher than the samples sealed by resin sealant. However, no significant differences were found. It can be concluded that use of resin modified glass ionomer sealant is a good alternative for sealing pits and fissures.

  15. RESEARCH ON IMPROVED EPOXY RESINS.

    Science.gov (United States)

    another ’million-modulus’ epoxy resin. Cast resin properties from a series of epoxy resins hardened with several aromatic diamines are reported, but these data are sufficient to advance only speculative conclusions. (Author)

  16. A validated liquid chromatographic method for the determination of polycyclic aromatic hydrocarbons in honey after homogeneous liquid-liquid extraction using hydrophilic acetonitrile and sodium chloride as mass separating agent.

    Science.gov (United States)

    Koltsakidou, Anastasia; Zacharis, Constantinos K; Fytianos, Konstantinos

    2015-01-16

    In the present report, a simple and cost-effective method for the determination of twelve US EPA priority polycyclic aromatic hydrocarbons (PAHs) in honey samples after salting-assisted liquid-liquid extraction and UHPLC with fluorescence detection is proposed. The sample treatment is based on the usage of hydrophilic acetonitrile as extraction solvent and its phase separation under high salinity conditions. Due to the high sugar content of the samples the phase separation is promoted effortlessly. Several parameters affecting the extraction efficiency and method sensitivity including the concentration of the honey samples, the type and volume of the extraction solvent, the type and quantity of the inorganic salt, extraction time and centrifugation time was systematically investigated. The method was validated in-house according to the Commission Decision 2002/657/EC guidelines. The limit of detection (LOD) of the method lay between 0.02 and 0.04ngmL(-1) (corresponding to 0.08 and 0.16ngg(-1)) which are close to the quality criteria established by European Regulation (EC) 836/2011 concerning the PAHs in foodstuffs. The mean analytical bias (expressed as relative recoveries) in all spiking levels was acceptable being in the range of 54-118% while the relative standard deviation (RSD) was lower than 19%. The proposed method has been satisfactorily applied for the analysis of the selected PAHs residues in various honey samples obtained from Greek region.

  17. 超声提取白刺中总生物碱及大孔树脂纯化的工艺研究%Ultrasound extraction total alkaloids from Nitraria sibirica Pall and process research of macroporous resin purification

    Institute of Scientific and Technical Information of China (English)

    王玉玲; 曾会明; 张建秋; 马挺军

    2013-01-01

    为优化西伯利亚白刺种籽中总生物碱的提取工艺,采用超声波提取总碱,以硫酸阿托品为对照品,酸性染料比色法测定白刺中总生物碱的含量,探讨料液比、提取温度、时间、乙醇浓度4个因素的影响,确定最佳提取参数.从7种大孔吸附树脂中筛选出对白刺生物碱有最佳分离纯化效果的一种树脂,研究其对生物碱静态、动态吸附、解析效果.研究结果表明,当料液比为1∶20,温度60℃,时间40 min,乙醇浓度70%时,总生物碱提取率(生物碱/种籽重)最高,217.372 9 μg/g D101对白刺总生物碱的吸附、解析效果最好,对其进行动态吸附,可知最佳的工艺条件为上样液pH值为5,流速为0.75 mL/min,乙醇的洗脱浓度为80%.%In order to optimize the extract condition, total alkaloids in Nitraria sibirica was extracted by ultrasound and the content of total alkaloids was determined by the acidic dye colorimetry, the effects of solid-liquid ratio, temperature, time and ethanol concentration on the optimum extraction parameters were investigated, thereby determining the optimal extraction parameters; the best one of isolation and purification from seven kinds of resin were screened out to research its effects on the alkaloids of static, dynamic adsorption. The results show that with the conditions of solid-liquid ratio of 1:20, temperature 60 ℃, time 40 minutes, ethanol concentration of 70%, the highest total alkaloid extract rate was 217.372 9 μg/g; the adsorption and resolution effects of D101 on N. sibirica's total alkaloids were the best, the dynamic adsorption tests proved that the optimum process conditions were: sample solution pH 5, flow rate 0.75mL/min, ethanol concentration 80%.

  18. Profiling and Preparation of Metabolites from Pyragrel in Human Urine by Online Solid-Phase Extraction Coupled with High Performance Liquid Chromatography Tandem Mass Spectrometry Followed by a Macroporous Resin-Based Purification Approach.

    Science.gov (United States)

    Zhao, Xin; Jiang, Jingjing; Yang, Guang; Huang, Jie; Yang, Guoping; He, Guangwei; Chu, Zhaoxing; Hang, Taijun; Fan, Guorong

    2017-03-21

    Pyragrel, a new anticoagulant drug, is derived from the molecular combination of ligustrazine and ferulic acid. Pyragrel showed significant inhibitory activity against platelet aggregation induced by adenosine diphosphate (ADP), and had been approved for a phase I clinical trial by CFDA. To characterize the metabolites of Pyragrel in human urine after intravenous administration, a reliable online solid-phase extraction couple with high performance liquid chromatography tandem mass spectrometry (online SPE-HPLC-MS(n)) method was conceived and applied. Five metabolites were detected and tentatively identified, which suggested that the major metabolic pathways of Pyragrel in human were double-bond reduction, double-bond oxidation, and then followed by glucuronide conjugation. Two main metabolites were then prepared using β-glucuronide hydrolysis and macroporous resin purification approach followed by preparative high-performance liquid chromatography (PHPLC) method, with their structures confirmed on the basis of nuclear magnetic resonance (NMR) data. This study provided information for the further study of the metabolism and excretion of Pyragrel.

  19. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of semivolatile organic compounds in bottom sediment by solvent extraction, gel permeation chromatographic fractionation, and capillary-column gas chromatography/mass spectrometry

    Science.gov (United States)

    Furlong, E.T.; Vaught, D.G.; Merten, L.M.; Foreman, W.T.; Gates, Paul M.

    1996-01-01

    A method for the determination of 79 semivolatile organic compounds (SOCs) and 4 surrogate compounds in soils and bottom sediment is described. The SOCs are extracted from bottom sediment by solvent extraction, followed by partial isolation using high-performance gel permeation chromatography (GPC). The SOCs then are qualitatively identified and quantitative concentrations determined by capillary-column gas chromatography/mass spectrometry (GC/MS). This method also is designed for an optional simultaneous isolation of polychlorinated biphenyls (PCBs) and organochlorine (OC) insecticides, including toxaphene. When OCs and PCBs are determined, an additional alumina- over-silica column chromatography step follows GPC cleanup, and quantitation is by dual capillary- column gas chromatography with electron-capture detection (GC/ECD). Bottom-sediment samples are centrifuged to remove excess water and extracted overnight with dichloromethane. The extract is concentrated, centrifuged, and then filtered through a 0.2-micrometer polytetrafluoro-ethylene syringe filter. Two aliquots of the sample extract then are quantitatively injected onto two polystyrene- divinylbenzene GPC columns connected in series. The SOCs are eluted with dichloromethane, a fraction containing the SOCs is collected, and some coextracted interferences, including elemental sulfur, are separated and discarded. The SOC-containing GPC fraction then is analyzed by GC/MS. When desired, a second aliquot from GPC is further processed for OCs and PCBs by combined alumina-over-silica column chromatography. The two fractions produced in this cleanup then are analyzed by GC/ECD. This report fully describes and is limited to the determination of SOCs by GC/MS.

  20. High Performance Liquid Chromatographic Method for Determination of Dipyridamole in Human Plasma

    Directory of Open Access Journals (Sweden)

    DAVOOD BEIGI BAND ARAB ADI

    1999-08-01

    Full Text Available A simple, rapid and specific high-performance liquid chromatographic procedure is reported for"nquantitative determination of dipyridamole in human -plasma. The assay uses a reversed-phase"nhigh-performance liquid chromatographic (HPLC and UV detection at 280nm and has a limit"nof detection of approximately 5ng/mL. The mobile phase consists of MeOH-H20 (60:40"nadjusted to pH 3.3. Dipyridamole was extracted from plasma by back-extraction procedure, with"npropranolol as the internal standard. The reproducibility of the method is satisfactory

  1. Three-dimensional graphene aerogel-supported iron oxide nanoparticles as an efficient adsorbent for magnetic solid phase extraction of organophosphorus pesticide residues in fruit juices followed by gas chromatographic determination.

    Science.gov (United States)

    Mahpishanian, Shokouh; Sereshti, Hassan

    2016-04-22

    In this research, a magnetic three dimensional-graphene nanocomposite (3D-G-Fe3O4) was prepared, characterized and used as an effective nanoadsorbent in magnetic solid-phase extraction (MSPE) of eight organophosphorus pesticides (OPPs) from juice samples prior to gas chromatography-nitrogen phosphorous detection (GC-NPD). The properties and morphology of 3D-G-Fe3O4 were characterized by scanning electron microscopy (SEM), Fourier transform-infrared spectroscopy (FT-IR) and vibrating sample magnetometry (VSM). The main experimental parameters affecting extraction recoveries including extraction time, amount of adsorbent, pH of sample solution, salt concentration and desorption conditions were carefully studied and optimized. The results showed wide linear concentration ranges with determination coefficients between 0.9973 and 0.9999. The limits of detection (S/N=3) of the method and limits of quantification (S/N=10) were from 1.2 to 5.1 ng L(-1) and 3.4-17.0 ng L(-1), respectively. The intra-day and inter-day RSDs were 2.6-5.1% and 3.5-6.9%, respectively. The method was successfully applied to the analysis of OPPs in fruit juices (apple, orange, grape, sour-cherry and apricot) with recoveries in range of 86.6-107.5%. The GC-NPD results were confirmed by gas chromatography-mass spectrometry (GC-MS). The results demonstrated that with combination of highly interconnected 3D network structure and magnetism property of adsorbent, 3D-G-Fe3O4 aerogel exhibited exceptional extraction ability towards the OPPs.

  2. Effects of the crisis in the resin sector on the demography of rural municipalities in Spain

    Energy Technology Data Exchange (ETDEWEB)

    Ortuno Perez, S.; Garcia Robredo, F.; Ayuga Tellez, E.; Fullana Belda, C.

    2013-05-01

    Aim of study: The aim of this work is to test the positive effect of a substantially developed resin sector on rural demographic evolution. This work shows how in the period between 1970 and 2010 the demographic decline in the interior regions of Spain was more pronounced in areas characterized by the importance of resin-producing forest stands compared to other nearby rural municipalities where this natural resource is not present. Area of study: The study area consists of a set of rural municipalities in Central Spain, both resin and non-resin producing, in the provinces of Segovia, Avila, Valladolid, Burgos, Soria, Cuenca and Guadalajara. Material and methods: The relationship between resin production and population in resin and non-resin producing municipalities was modeled by means of linear regression analysis. Main results: Generally speaking, between 1950 and 1970 the production of resin halted demographic decline in the regions where this activity was substantially developed. However, when the resin sector entered into crisis in the 1970s, and the economic repercussions of this activity gradually ceased to be felt, the demographic decline in the regions which had been involved in resin production was much more acute than in other non-resin-producing rural areas. Research highlights: This work shows the relationship between resin extraction activity and population evolution in rural municipalities. Sustainable resin exploitation can contribute to the maintenance and development of rural communities, and should be used as a tool for generating employment in rural areas. (Author) 37 refs.

  3. Chromatographic separation of three monoclonal antibody variants using multicolumn countercurrent solvent gradient purification (MCSGP).

    Science.gov (United States)

    Müller-Späth, Thomas; Aumann, Lars; Melter, Lena; Ströhlein, Guido; Morbidelli, Massimo

    2008-08-15

    Multicolumn countercurrent solvent gradient purification (MCSGP) is a continuous chromatographic process developed in recent years (Aumann and Morbidelli, 2007a; Aumann et al., 2007) that is particularly suited for applications in the field of bioseparations. Like batch chromatography, MCSGP is suitable for three-fraction chromatographic separations and able to perform solvent gradients but it is superior in terms of solvent consumption, yield, purity, and productivity due to the countercurrent movement of the liquid and the solid phases. In this work, the MCSGP process is applied to the separation of three monoclonal antibody variants on a conventional preparative cation exchange resin. The experimental process performance was compared to simulations based on a lumped kinetic model. Yield and purity values of the target variant of 93%, respectively were obtained experimentally. The batch reference process was clearly outperformed by the MCSGP process.

  4. Fabrication and evaluation of magnetic activated carbon as adsorbent for ultrasonic assisted magnetic solid phase dispersive extraction of bisphenol A from milk prior to high performance liquid chromatographic analysis with ultraviolet detection.

    Science.gov (United States)

    Filippou, Olga; Deliyanni, Eleni A; Samanidou, Victoria F

    2017-01-06

    In the present study, the impregnation of a micro - meso porous activated carbon with magnetite (Fe3O4) was successfully achieved by sonication and the magnetic activated carbon prepared (Bmi) was evaluated as a new adsorbent for ultrasonic assisted magnetic solid phase dispersive extraction of Bisphenol A (BPA) from cow milk and human breast milk samples, prior to the determination by HPLC with UV detection. The prepared Bmi was characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM). The effect of pH on adsorption, initial concentration, contact time and desorption were studied. The main experimental parameters influencing extraction efficiency of BPA, such as type and amount of the adsorbent, sample amount, type of desorption solvent, time of adsorption and desorption, type of precipitation solvent, were investigated and optimized. Under the optimal extraction conditions the absolute recovery of BPA was 81% and 95% in cow milk and human breast milk samples, respectively. Good linearity was observed in the investigated concentration range of 2.5μgkg(-1)-5000μgkg(-1) (R(2)=0.9997). Limit of detection (LOD) was 0.75μgL(-1), which is in accordance with the specific migration limit (SML) established by the European Union, and limit of quantification (LOQ) was 2.5μgL(-1). Within-day and between-day recoveries ranged from 91.4% to 98.6% and 89.1% to 99.4% respectively and the RSDs were less than 3.7%. Due to the excellent magnetic behavior of Bmi the proposed method was shown to be simple and rapid. Besides these, this method is sensitive, low cost, efficient and environmentally friendly. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. 协同萃取法回收地浸采铀工艺树脂中铼%Synergistic Extraction of Rhenium from In-Situ Leach Uranium Mining Technology Resin

    Institute of Scientific and Technical Information of China (English)

    彭真; 罗明标; 蒋小辉; 花榕; 廖桢葳

    2011-01-01

    Synergistic extraction of rhenium with primary amines and tributylphosphate was studied. The effects of initial pH value, composition of the extractant, and volume ratio of organic phase to aqueous phase on the extraction of rhenium were studied. The results showed that the synergistic extraction efficiency of rhenium was above 97% at pH 2-10, while dissolving loss of primary amine ( N1923) in acid condition was great. The optimum conditions were obtained with initial pH value of 9.5 with 30% N1923, 50% TBP and 20% sulphonating kerosene as extractant, 3% NaOH as stripping reagent, phase ratio of 1: 1. The extraction efficiency was above 99% , and stripping efficiency was above 97%. The distribution ratio of rhenium increased with the increase of initial concentration of rhenium, and the extraction rate of rhenium was not influenced by the uranium existed in aqueous phase, and hardly influenced by nitrate. During the progress of in-situ sulfuric acid leaching technique of uranium, U and Re in the forms of [ UO2 (SO4 )2 ]2- , [ UO2 (SO4)3]4- , ReO4- were brought into leaching solution, and simultaneously absorbed by anion exchange resin D231. Uranium was stripped by nitrate or chloride from in-situ leach uranium mining technology resin, then rhenium was stripped by 10% NH4NO3 and 8% NH40H. It was effective, for the recovery of rhenium from desorption solution by primary amines and tributylphosphate synergistic extraction that provided parameters for further industry investigation for recovery of rhenium from uranium ore.%介绍了伯胺和磷酸三丁酯协同萃取回收铼的实验研究,考察了水相初始pH值、萃取剂组成、相比(O/W)对铼萃取率的影响.结果表明:协同萃取体系在pH 2~10范围内铼的萃取率均在97%以上,但酸性条件下伯胺N1923溶解损失较大,水相初始pH9.5为最佳萃取酸度,以有机相30% N1923-50%TBP-20%磺化煤油萃取铼效果最佳,并采用3% NaOH反萃铼,

  6. Biocidal quaternary ammonium resin

    Science.gov (United States)

    Janauer, G. E.

    1983-01-01

    Activated carbon (charcoal) and polymeric resin sorbents are widely used in the filtration and treatment of drinking water, mainly to remove dissolved organic and inorganic impurities and to improve the taste. Earlier hopes that activated carbon might "disinfect' water proved to be unfounded. The feasibility of protecting against microbial infestation in charcoal and resin beds such as those to be incorporated into total water reuse systems in spacecraft was investigated. The biocidal effect of IPCD (insoluable polymeric contact disinfectants) in combination with a representative charcoal was assessed. The ion exchange resins (IPCD) were shown to adequately protect charcoal and ion exchange beds.

  7. Biocompatibility of composite resins

    Directory of Open Access Journals (Sweden)

    Sayed Mostafa Mousavinasab

    2011-01-01

    Full Text Available Dental materials that are used in dentistry should be harmless to oral tissues, so they should not contain any leachable toxic and diffusible substances that can cause some side effects. Reports about probable biologic hazards, in relation to dental resins, have increased interest to this topic in dentists. The present paper reviews the articles published about biocompatibility of resin-restorative materials specially resin composites and monomers which are mainly based on Bis-GMA and concerns about their degradation and substances which may be segregated into oral cavity.

  8. Removal of dyes from water using crosslinked aminomethane sulfonic acid based resin.

    Science.gov (United States)

    Kaner, Damla; Saraç, Ayfer; Senkal, Bahire Filiz

    2010-08-01

    A new polymeric resin with amino sulfonic acid pendant functions has been prepared for the extraction of acidic and basic dyes from water. Beaded polymer supports were prepared by suspension polymerization of vinyl benzyl chloride (0.9 mol) and ethylene glycol dimethacrylate (0.1 mol). The resulting copolymer beads were modified with amino methane sulfonic acid. The dye adsorption capacity of the resin was found as 0.16 g dye/g resin for ramazol black and 0.15 g dye/g resin for crystal violet. The pH depending measurements and dye sorption kinetics of the resin were also investigated.

  9. Resin composite repair: Quantitative microleakage evaluation of resin-resin and resin-tooth interfaces with different surface treatments

    OpenAIRE

    Celik, Cigdem; Cehreli, Sevi Burcak; Arhun, Neslihan

    2015-01-01

    Objective: The aim was to evaluate the effect of different adhesive systems and surface treatments on the integrity of resin-resin and resin-tooth interfaces after partial removal of preexisting resin composites using quantitative image analysis for microleakage testing protocol. Materials and Methods: A total of 80 human molar teeth were restored with either of the resin composites (Filtek Z250/GrandioSO) occlusally. The teeth were thermocycled (1000×). Mesial and distal 1/3 parts of the res...

  10. 固相萃取-色谱质谱技术在毒物筛查中的应用进展%Progress of Solid-phase Extraction Coupled with Chromatograph-Mass Spectrum in Toxicological Screening

    Institute of Scientific and Technical Information of China (English)

    张泽楠; 常靖; 王芳琳; 于忠山; 张云峰; 崔冠峰

    2015-01-01

    固相萃取是近年发展起来的一种样品前处理技术,主要用于样品的分离和富集,能够将生物检材中的目标待测物有效的与杂质组分分离,具有较高的回收率,其样品预处理过程简单,操作便捷。在法庭科学领域,可根据生物检材,如生物体液、组织、毛发等基质的性质,选择相应的固相萃取方法;同时亦可根据目标待测物,如目标待测物的酸碱性,选用不同的固相萃取方法。色谱法是一种分离和分析方法,它利用不同物质在不同相态的选择性分配,使混合物中的不同组分根据其性质不同而分离。质谱法在分析中可提供丰富的结构信息。固相萃取-色谱质谱联用技术集固相萃取与色谱质谱检测技术优点于一体,可实现对复杂基质中的特定毒物与非特定毒物进行高效萃取、净化与检测,具有检材消耗少、检测速度快、灵敏度高等特点,已被广泛应用于环境监测、药物分析、法庭科学领域等,成为当前毒物筛查的重要手段,具有选择性好、灵敏度高、基质效应低等特点,且易实现在线分析,特别适用于法庭毒物分析中单一毒物或多种毒物的筛查。本文综述了固相萃取-色谱质谱联用技术在法庭科学毒物毒品分析中的应用进展,以供同行参考。%Solid-phase extraction (SPE) is one of sample pretreatment technologies developed in recent years, which separates target compounds from biological complex matrixes and impurity by using the sorbent absorption. The sample pretreatment process of SPE is simple and convenient, which has been widely used in pharmaceutical analysis, food testing, environment monitoring, forensic science and other fields. Solid-phase extraction can separate target substance from complex matrix with high recovery, which makes it play an important role in the field of forensic science. As the method for separation and analysis

  11. 顶空气相色谱法测定大孔树脂提取物中的残留溶剂研究%Determination of residual solvents in macroporous resin extracts by Head-space capillary gas chromatography

    Institute of Scientific and Technical Information of China (English)

    刘冬; 杨敬芝; 杜守颖; 张东明; 赵立敏; 陈雯

    2009-01-01

    目的:建立了测定大孔树脂淫羊藿提取物、栀子提取物以及HP中乙醇、正己烷、苯、甲苯、甲基环己烷、二甲苯、苯乙烯、二乙烯苯残留有机溶剂含量的顶空气相色谱法.方法:采用顶空气相色谱法,FID检测器,以20%~50%二甲基亚砜为溶媒,顶空预热温度为90℃,预热时间为10 min,进样口温度为180℃,检测器温度为250℃,以氮气为载气,使用DB-1交联毛细管柱(60m×0.32mm,1 μm),程序升温,实现了各组分的基线分离.结果:乙醇、正己烷、苯、甲苯、甲基环己烷、二甲苯、苯乙烯、二乙烯苯在各自对应的浓度范围内,线性关系良好;乙醇、正己烷、苯、甲苯、甲基环己烷、二甲苯、苯乙烯、二乙烯苯的最小检测限分别为2.72,0.22,0.03,0.03,0.28,0.33,0.03,0.31 μg·mL~(-1);加样回收率均在75%以上,精密度较好.结论:经方法学验证,该方法灵敏、准确、可靠,可适用于大孔树脂淫羊藿提取物、栀子提取物及HP中乙醇、正己烷、苯、甲苯、甲基环己烷、二甲苯、苯乙烯、二乙烯苯等残留有机溶剂的测定.%Objective:This paper reports a Head-space GC method for determination of enthanol,hexane,benzene,toluene,methyl cyclohexane,xylene,styrene,divinyl benzene in macroporous resin extractions.Method:The analytical coluren was DB-1(60m×0.32mm,1μm).The injector temperature was 180℃ and the detector tempemture was 250℃.The column temperature was programmed raised.The carrier gas was nitrogen and the solvent was 20%-50% dimethyl sulfoxide.Results:The stand curve were linear for each solvents in the range of each consistencv.The average recoveries were all more than 75%.Conclusion:This method is simple,rapid and precise,it is suitable for measurement of residual solvents in macroporous resin extracts.

  12. Anticholinesterase activity and chemical profile of an active chromatographic fraction of ethanolic extract from Bellis perennis L. (Asteraceae) flowers; Atividade anticolinesterasica e perfil quimico de uma fracao cromatografica ativa do extrato etanolico das flores Bellis perennis L. (Asteraceae)

    Energy Technology Data Exchange (ETDEWEB)

    Marques, Thiago Henrique Costa; Santos, Pauline Sousa dos; Freitas, Rivelilson Mendes de, E-mail: rivelilson@pq.cnpq.br [Universidade Federal do Piaui (UFPI), Teresina, PI (Brazil). Centro de Ciencias da Saude. Departamento de Bioquimica e Farmacologia; Carvalho, Rusbene Bruno Fonseca de; Melo, Cassio Herbert Santos de [Universidade Federal do Piaui (UFPI), Teresina, PI (Brazil). Centro de Ciencias da Natureza. Departamento de Quimica; David, Juceni Pereira [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Faculdade de Farmacia; David, Jorge Mauricio; Lima, Luciano Silva [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Instituto de Quimica

    2013-09-01

    This work describes the isolation of an active flavonoid fraction and identification of isorhamnetin 3-O-{beta}-D-(6''-acetyl)- alactopyranoside from flowers of B. perennis, and also the evaluation of anticholinesterase (AChE) activity of ethanolic extract from flowers (EEF) and the active fraction. The chemical structure of the flavonoid was defined on the basis of spectroscopic {sup 1}H NMR, IR and UV data. EEF or flavonoid reduces AChE activity in vivo, while flavonoid also reduces AChE activity in vitro, showing a value of 1.49 {mu}M for 50% inhibitory concentration (IC{sub 50}), suggesting potential use as an insecticide or in the treatment of neurodegenerative diseases such as Alzheimer's disease. (author)

  13. Fast and simple procedure for liquid-liquid extraction of 136 analytes from different drug classes for development of a liquid chromatographic-tandem mass spectrometric quantification method in human blood plasma.

    Science.gov (United States)

    Remane, Daniela; Meyer, Markus R; Peters, Frank T; Wissenbach, Dirk K; Maurer, Hans H

    2010-07-01

    In clinical and forensic toxicology, different extraction procedures as well as analytical methods are used to monitor different drug classes of interest in biosamples. Multi-analyte procedures are preferable because they make the analytical strategy much simpler and cheaper and allow monitoring of analytes of different drug classes in one single body sample. For development of such a multi-analyte liquid chromatography-tandem mass spectrometry approach, a rapid and simple method for the extraction of 136 analytes from the following drug classes has been established: antidepressants, neuroleptics, benzodiazepines, beta-blockers, oral antidiabetics, and analytes relevant in the context of brain death diagnosis. Recovery, matrix effects, and process efficiency were tested at two concentrations using six different lots of blank plasma. The recovery results obtained using absolute peak areas were compared with those calculated using area ratios analyte/internal standard. The recoveries ranged from 8% to 84% for antidepressants, from 10% to 79% for neuroleptics, from 60% to 81% for benzodiazepines, from 1% to 71% for beta-blockers, from 10% to 73% for antidiabetics, and from 60% to 86% for analytes relevant in the context of brain death diagnosis. With the exception of 52 analytes at low concentration and 37 at high concentration, all compounds showed recoveries with acceptable variability with less than 15% and 20% coefficients of variation. Recovery results obtained by comparing peak area ratios were nearly the same, but 35 analytes at low concentration and 17 at high concentration lay above the acceptance criteria. Matrix effects with more than 25% were observed for 18 analytes. The results were acceptable for 119 analytes at high concentrations.

  14. DETERMINATION OF CHOLESTEROL IN OIL BY ULTRASONIC EXTRACTION-GAS CHROMATOGRAPHIC%超声提取-气相色谱法测定油脂中胆固醇

    Institute of Scientific and Technical Information of China (English)

    潘红红; 姜涛; 周易; 陈代伟

    2012-01-01

    建立了毛细管气相色谱法测定油脂中胆固醇含量的方法,改进了油脂皂化方法以及皂化完成后使用分液漏斗提取胆固醇过程中容易产生乳化、操作复杂且比较耗时的缺点,采用超声波提取胆固醇,优化了样品前处理条件.结果表明,该法在0.002mg/mL~0.500mg/mL范围呈线性(r=0.9997),检出限为20mg/kg,RSD=1.104%,回收率在81.3%~93.8%之间.%A method was established for the determination of cholesterol in oil by capillary gas chromatography, which improved oil saponification method and overcame the shortcomings that separatory funnel extraction of cholesterol was prone to emulsification and the operation was complex and time-consuming after saponification. Also, the use of ultrasonic extraction of cholesterol optimized the sample of pre-treatment conditions. The results showed that the method was suitable for detection, RSD= 1.104%, When cholesterol concentration was in fine linear relation ( r=0.9997) with chromatogram peak area with in the range of 0. 002~0.5 mg/mL, the detection limit of method was 20 mg/kg, the average recovery was 81. 3% - 93. 85%.The methqd of detection of cholesterol in oil was economical , sim

  15. Explorations of TALSPEAK chemistry in extraction chromatography: Comparisons of TTHA with DTPA and HDEHP with HEH[EHP

    Energy Technology Data Exchange (ETDEWEB)

    Braley, Jenifer C.; McAlister, Daniel; Horwitz, E. P.; Nash, Kenneth L.

    2013-03-01

    An advanced nuclear fuel cycle includes a reprocessing stage for the group separation of the lanthanides from the trivalent actinides. The TALSPEAK (Trivalent Actinide - Lanthanide Separation by Phosphorus reagent Extraction from Aqueous Komplexes) solvent extraction process provides the An3+/Ln3+ separation through the use of an organic lanthanide extractant (bis-2-ethyl(hexyl) phosphoric acid, HDEHP) and an aqueous actinide-selective holdback reagent (diethylenetriamine-N,N,N’,N’’,N’’-pentaacetic acid, DTPA). Organic phase interactions in TALSPEAK have proven sufficiently complex that, even with substantial research effort, a descriptive thermodynamic model has yet to be developed. If one were to consider an extraction chromatographic (EXC) version of TALSPEAK, the presence of concentrated extractant on the resin surface should augment the multifaceted organic phase chemistry. This study examines the previously unexplored impact of each aqueous phase TALSPEAK component (holdback reagent, carboxylic acid buffer, and pH) on the chemistry of the EXC system. The presence of alternative reagents, 2-ethyl(hexyl) phosphonic acid mono-2-ethyl(hexyl) ester acid (HEH[EHP]) and triethylenetetramine-N,N,N’,N’’,N’’’,N’’’-hexaacetic acid (TTHA) are also considered. Results indicate the concentrated extractant appears to enhance solid-phase reactions that most likely involve water, lactate and sodium. The presumed water, lactate and sodium partitioning consumes resin capacity sufficiently that the weaker hold-back reagent under TALSPEAK aqueous conditions (pH ~ 3.6), TTHA, provides preferential Am3+/Ln3+ separations performance. If a TALSPEAK-EXC process were to be developed, a resin with solvent diluted extractant or covalently bound functional groups may be preferential to reduce the complexity of the solid-phase chemistry.

  16. Quantification and Purification of Mulberry Anthocyanins with Macroporous Resins

    Directory of Open Access Journals (Sweden)

    Xueming Liu

    2004-01-01

    Full Text Available Total anthocyanins in different cultivars of mulberry were measured and a process for the industrial preparation of mulberry anthocyanins as a natural food colorant was studied. In 31 cultivars of mulberry, the total anthocyanins, calculated as cyanidin 3-glucoside, ranged from 147.68 to 2725.46 mg/L juice. Extracting and purifying with macroporous resins was found to be an efficient potential method for the industrial production of mulberry anthocyanins as a food colorant. Of six resins tested, X-5 demonstrated the best adsorbent capability for mulberry anthocyanins (91 mg/mL resin. The adsorption capacity of resins increased with the surface area and the pore radius. Residual mulberry fruit juice after extraction of pigment retained most of its nutrients, except for anthocyanins, and may provide a substrate for further processing.

  17. Simplified miniaturized ultrasound-assisted matrix solid phase dispersion extraction and high performance liquid chromatographic determination of seven flavonoids in citrus fruit juice and human fluid samples: hesperetin and naringenin as biomarkers.

    Science.gov (United States)

    Barfi, Behruz; Asghari, Alireza; Rajabi, Maryam; Barfi, Azadeh; Saeidi, Iman

    2013-10-11

    In the present study, for the first time, a simplified miniaturized ultrasound-assisted matrix solid-phase dispersion (SM-USA-MSPD) method with a different application for liquid matrices was developed to extract different flavonoids (hesperidin, diosmin, eriocitrin, narirutin, naringin, hesperetin and naringenin) from citrus fruit juice and human fluid samples prior to their determination using high performance liquid chromatography (HPLC). Different effective parameters were studied and under the optimum conditions (including sample volume: 150μL; solid phase: silica-based C18, 200mg; eluting solvent: methanol, 500μL; pH: 4; and sonication: 6min; at room temperature), limits of detection and limits of quantification were ranged from 23.3 to 46.8ngmL(-1) and 74.8 to 141.5ngmL(-1), respectively. Once optimized, analytical performance of the method was studied in terms of linearity (0.074-198.5μgmL(-1), r(2)>0.991), accuracy (recovery=84.6-101.5%), and precision (repeatability: intra-day precisionjuices- and the obtained results confirmed that these compounds could be used as good biomarkers of citrus fruit juice intake.

  18. Al2O3 Extraction Technologies from Fly Ash on the Properties of Modified PP Resin%粉煤灰提取Al2O3工艺对PP改性性能的影响

    Institute of Scientific and Technical Information of China (English)

    董金虎

    2012-01-01

    Extract Al2O3 was extracted from fly ash using alkali high-temperature calcinations, obtain two different structures' Al2O3 were obtained by two different technologies at the phase of Al(OH), separated out,and two different A12O3 were used to modify PP resin. The results showed that, the tensile strength of PP modified by sheet Al2O3, was better than the PP modified by flocculent Al2O3, and the elongation and impact strength of PP modified by the two different Al2O3 could have the same modification effect, and the content of sheet AlO3 litter than flocculent Al2O3 when obtained the same modification effect. And when the content of Al2O3 was about 2% , the comprehensive performance of PP modified by sheet Al2O3 was better,and the tensile strength increased about 13 % , and the elongation increased about 18 % , and the impact strength increased 15 % .%采用碱焙烧法从粉煤灰中提取Al2O3,在Al(OH)3析出过程中采用两种不同的工艺方法,可以形成两种结构的Al2O3,并分别将两种Al2O3用于改性PP树脂.结果表明:片状Al2O3改性PP的拉伸强度好于絮状Al2O3,而两种Al2O3改性PP的断裂伸长率、冲击强度可以获得相当的改性效果,且片状Al2O3的用量少于絮状Al2O3.片状Al2O3用量为2%左右时,改性PP的综合性能较好,拉伸强度提高约13%,断裂伸长率提高约18%,冲击强度提高约15%.

  19. Biocompatibility and cytotoxicity of two novel low-shrinkage dental resin matrices.

    Science.gov (United States)

    Jan, Yih-Dean; Lee, Bor-Shiunn; Lin, Chun-Pin; Tseng, Wan-Yu

    2014-06-01

    To reduce the polymerization shrinkage of dental composite resin, we used two different ratios of toluene 2,4-diisocyanate (TDI) or 1,6-hexamethylene diisocyanate (HDI) as functional side chains of bisphenol A-glycidyl methacrylate (bis-GMA) to synthesize two series of new dental resin matrices. This study evaluated the biocompatibility and cytotoxicity of these two series of new resin matrices. Two series of new dental resin matrices with the ratios of TDI or HDI functional side chain to bis-GMA (defined as B group) being 1:4, 1:2, 1:1 and 3:2 (defined as T1/4, T1/2, T1, T3/2, and H1/4, H1/2, H1, H3/2 groups, respectively) were synthesized. Each resin sample was light cured and immersed in the culture medium for 24 hours to make the extract solution. Then, human gingival fibroblasts were cultured in different extract solutions for 72 hours. The cytotoxicities of different resins were evaluated by microtitertetrazolium (MTT) assay, the levels of cell-produced reactive oxygen species (ROS) induced by different extract solutions was measured. Resins of the T1/4 and B groups revealed significantly higher cytotoxicity than resins of other groups. However, resins of the T1 and T3/2 groups exhibited less cytotoxicity. In general, resins of the TDI-modified groups showed equal or less cytotoxicity and induced equal or lower levels of ROS than the corresponding resins of the HDI-modified and B groups. Our results showed that the TDI-modified resin matrices containing more functional side chains were less cytotoxic than the corresponding HDI-modified resin matrices. When the ratio of functional side chain to bis-GMA is increased, the stereo hindrance of resin structure is increased, more toxic resin monomers are trapped in the complicated resin structure, and thus the resin matrix reveals less cytotoxicity. The TDI-modified resin matrices exhibit higher stereo hindrance of resin structure and thus show less cytotoxicity than the corresponding HDI-modified resin matrices

  20. Nanofluidic Size-Exclusion Chromatograph

    Science.gov (United States)

    Feldman, Sabrina; Svehla, Danielle; Grunthaner, Frank; Feldman, Jason; Shakkottai, P.

    2004-01-01

    Efforts are under way to develop a nanofluidic size-exclusion chromatograph (SEC), which would be a compact, robust, lightweight instrument for separating molecules of interest according to their sizes and measuring their relative abundances in small samples. About as large as a deck of playing cards, the nanofluidic SEC would serve, in effect, as a laboratory on a chip that would perform the functions of a much larger, conventional, bench-top SEC and ancillary equipment, while consuming much less power and much smaller quantities of reagent and sample materials. Its compactness and low power demand would render it attractive for field applications in which, typically, it would be used to identify and quantitate a broad range of polar and nonpolar organic compounds in soil, ice, and water samples. Size-exclusion chromatography is a special case of high-performance liquid chromatography. In a conventional SEC, a sample plug is driven by pressure along a column packed with silica or polymer beads that contain uniform nanopores. The interstices between, and the pores in, the beads collectively constitute a size-exclusion network. Molecules follow different paths through the size-exclusion network, such that characteristic elution times can be related to sizes of molecules: basically, smaller molecules reach the downstream end of the column after the larger ones do because the smaller ones enter minor pores and stay there for a while, whereas the larger ones do not enter the pores. The volume accessible to molecules gradually diminishes as their size increases. All molecules bigger than a pore size elute together. For most substances, the elution times and sizes of molecules can be correlated directly with molecular weights. Hence, by measuring the flux of molecules arriving at the downstream end as a function of time, one can obtain a liquid mass spectrum for the molecules present in a sample over a broad range of molecular weights.

  1. Fermentation and recovery of glutamic acid from palm waste hydrolysate by Ion-exchange resin column.

    Science.gov (United States)

    Das, K; Anis, M; Azemi, B M; Ismail, N

    1995-12-05

    Glutamic acid produced from palm waste hydrolysate by fermentation with Brevibacterium lactofermentum ATCC 13869 is produced with a remarkably high yield compared with that produced from pure glucose as a carbon source. The produce yield is 70 g/L with glucose, wherease, when palm waste hydrolysate is the fermentation medium in the same bioreactor under same conditions, it is 88 g/L. The higher yield may be attributed to the fact that this organism has the ability to convert sugars other than only glucose present in the hydrolysate. Bioreactor conditions most conducive for maximum production are pH 7.5, temperature of 30 degrees rmentation period of 48 h, inoculum size 6%, substrate concentration of 10 g per 100 mL, yeast extract 0.5 g per 100 mL as a suitable N source, and biotin at a concentration of 10 pg/L. Palm waste hydrolysate used in this study was prepared by enzymic saccharification of treated palm press fiber under conditions that yielded a maximum of 30 g/L total reducing sugars. Glutamic acid from fermentation broth was recovered by using a chromatographic column (5cm x 60 cm) packed with a strong ion-exchange resin. The filtered broth containing glutamic acid and other inorganic ions was fed to the fully charged column. The broth was continuously recycled at a flow rate of 50 mL/min (retention time of 55 min) until glutamic acid was fully adsorbed on the column leaving other ions in the effluent. Recovery was done by eluting with urea and sodium hydroxide for total displacement of glutamic acid from the resin. The eluent containing 88 g/L of glutamic acid was concentrated by evaporation to obtain solid crystals of the product. (c) 1995 John Wiley & Sons, Inc.

  2. Reverse-phase high pressure liquid chromatographic analysis of harpagoside, scorodioside and verbascoside from Scrophularia scorodonia: quantitative determination of harpagoside.

    Science.gov (United States)

    Díaz, A; Fernández, L; Ollivier, E; Martín, T; Villaescusa, L; Balansard, G

    1998-02-01

    A reversed-phase high performance liquid chromatographic method has been developed for the determination of the main compounds (harpagoside, scorodioside, and verbascoside) from different samples of Scrophularia scorodonia. The chromatographic method has been validated and applied for quantitative determination of harpagoside. The results show the highest levels of harpagoside in the leaf extract. The purity and identity of peaks were controlled by diode-array detection and comparison with standards.

  3. Evaluation of selectivity in homologous multimodal chromatographic systems using in silico designed antibody fragment libraries.

    Science.gov (United States)

    Karkov, Hanne Sophie; Woo, James; Krogh, Berit Olsen; Ahmadian, Haleh; Cramer, Steven M

    2015-12-24

    This study describes the in silico design, surface property analyses, production and chromatographic evaluations of a diverse set of antibody Fab fragment variants. Based on previous findings, we hypothesized that the complementarity-determining regions (CDRs) constitute important binding sites for multimodal chromatographic ligands. Given that antibodies are highly diversified molecules and in particular the CDRs, we set out to examine the generality of this result. For this purpose, four different Fab fragments with different CDRs and/or framework regions of the variable domains were identified and related variants were designed in silico. The four Fab variant libraries were subsequently generated by site-directed mutagenesis and produced by recombinant expression and affinity purification to enable examination of their chromatographic retention behavior. The effects of geometric re-arrangement of the functional moieties on the multimodal resin ligands were also investigated with respect to Fab variant retention profiles by comparing two commercially available multimodal cation-exchange ligands, Capto MMC and Nuvia cPrime, and two novel multimodal ligand prototypes. Interestingly, the chromatographic data demonstrated distinct selectivity trends between the four Fab variant libraries. For three of the Fab libraries, the CDR regions appeared as major binding sites for all multimodal ligands. In contrast, the fourth Fab library displayed a distinctly different chromatographic behavior, where Nuvia cPrime and related multimodal ligand prototypes provided markedly improved selectivity over Capto MMC. Clearly, the results illustrate that the discriminating power of multimodal ligands differs between different Fab fragments. The results are promising indications that multimodal chromatography using the appropriate multimodal ligands can be employed in downstream bioprocessing for challenging selective separation of product related variants.

  4. 白术多糖WAM-1结构的色谱分析和原子力显微镜观察%Chromatographic Analysis and Atomic Force Microscope Observation of Polysaccharide Extracted from Atractylodes macrocephala Koidz.

    Institute of Scientific and Technical Information of China (English)

    伍乐芹; 姜绍芬; 张静

    2012-01-01

    Polysaccharides extracted from the stem of Atractylodes macrocephala Koidz by hot water,were fractionated by DEAE-52 cellulose chromatography,and purified by Sephadex G-200 gel filtration chromatography to obtain a fraction, named WAM-1. HPLC and GC analysis showed that WAM-1 was a homogeneous and consisted of glucose and galactose in the molar ratio of 3. 01: 1. The molecular morphology of WAM-1 was observed under an atomic force microscope (AFM).The results showed that WAM-1 existed in different forms with different concentrations. The concentration of polysaccharide had effects on the conformation and form of chain interactions, which might be related to the interaction of intramolecular and intermolecular hydrogen bonds. At 10 μg/mL,the morphology of WAM-1 was observed clearly in rigid chains with many branches.%通过热水浸提法从草本植物白术根茎提取的水溶性粗多糖,经DEAE-52纤维素柱层析分离和Sephadex G-200凝胶过滤柱层析纯化,得到组分WAM-1.采用高效液相色谱(HPLC)检测WAM-1的纯度,气相色谱(GC)对其单糖组分进行分析,原子力显微镜(AFM)对其分子外貌进行观测.结果显示:WAM-1为均一多糖,由葡萄糖和半乳糖以3.01:1摩尔比构成;在不同浓度溶液条件下,WAM-1分子以不同形态存在,多糖溶液的浓度对WAM-1的分子链构象及链间相互作用形式产生影响,推测可能与WAM-1分子内、分子间的氢键缔合作用有关.多糖浓度为10μg/mL时,可清晰的观察到WAM-1是以刚性链状形态存在,且具有多分支结构.

  5. Chromatographic study of Euphorbia cyparissias

    Directory of Open Access Journals (Sweden)

    Cristina, T. Romeo,

    2009-12-01

    Full Text Available The ectoparasitic population control is very difficult and includes numerous chemical substances and therapeutic techniques. Although efficient at first, the repeated use of acaricidal substances leads to the appearance of resistance. The more and more reduced efficacy of the therapeutic arsenal puts serious problems for the practitionersand increases the need of newer substances on the market. Besides this appears the problem of residues in eggs and meat, which is a serious impediment. Because of this the use of plant extracts is an attractive and promising research path. The investigations tied to the parasitic biocontrol have diversified with the study of the numerous control sources (fungi, plant extracts, volatile oils etc..In this context, the plant extracts can become an alternative source for the acaricidal control knowing that they constitute a rich source of efficient bioactive compounds. Unfortunately although at hand until today, not very much data is known about what determines theacaricidal activity of some plant extracts against the argaside ticks.The present work describes an in vitro CG-MS study for identification of Euphorbia cyparissias’ chemical composition.

  6. Selenium speciation methods and application to soil saturation extracts from San Joaquin Valley, California

    Science.gov (United States)

    Fio, John L.; Fujii, Roger

    1990-01-01

    Methods to determine soluble concentrations of selenite, selenate, and organic Se were evaluated on saturation extracts of soil samples collected from three sites on the Panoche Creek alluvial fan in the western San Joaquin Valley, California. The methods were used in combination with hydride-generation atomic-absorption spectrometry for detection of Se, and included a selective chemical-digestion method and three chromatographic methods using XAD-8 resin, Sep-Pak C18 cartridge, and a combination of XAD-8 resin and activated charcoal. The chromatography methods isolate dissolved organic matter that can inhibit Se detection by hydride-generation atomic-absorption spectrometry. Isolation of hydrophobic organic matter with XAD-8 did not affect concentrations of selenite and selenate, and the isolated organic matter represents a minimal estimation of organic Se. Ninety-eight percent of the Se in the extracts was selenate and about 100% of the isolated organic Se was associated with the humic acid fraction of dissolved organic matter. The depth distribution of Se species in the soil saturation extracts support a hypothesis that the distribution of soluble Se and salinity in these soils is the result of evaporation from a shallow water table and leaching by irrigation water low in Se and salinity.

  7. Determination of Human-Health Pharmaceuticals in Filtered Water by Chemically Modified Styrene-Divinylbenzene Resin-Based Solid-Phase Extraction and High-Performance Liquid Chromatography/Mass Spectrometry

    Science.gov (United States)

    Furlong, Edward T.; Werner, Stephen L.; Anderson, Bruce D.; Cahill, Jeffery D.

    2008-01-01

    In 1999, the Methods Research and Development Program of the U.S. Geological Survey National Water Quality Laboratory began the process of developing a method designed to identify and quantify human-health pharmaceuticals in four filtered water-sample types: reagent water, ground water, surface water minimally affected by human contributions, and surface water that contains a substantial fraction of treated wastewater. Compounds derived from human pharmaceutical and personal-care product use, which enter the environment through wastewater discharge, are a newly emerging area of concern; this method was intended to fulfill the need for a highly sensitive and highly selective means to identify and quantify 14 commonly used human pharmaceuticals in filtered-water samples. The concentrations of 12 pharmaceuticals are reported without qualification; the concentrations of two pharmaceuticals are reported as estimates because long-term reagent-spike sample recoveries fall below acceptance criteria for reporting concentrations without qualification. The method uses a chemically modified styrene-divinylbenzene resin-based solid-phase extraction (SPE) cartridge for analyte isolation and concentration. For analyte detection and quantitation, an instrumental method was developed that used a high-performance liquid chromatography/mass spectrometry (HPLC/MS) system to separate the pharmaceuticals of interest from each other and coextracted material. Immediately following separation, the pharmaceuticals are ionized by electrospray ionization operated in the positive mode, and the positive ions produced are detected, identified, and quantified using a quadrupole mass spectrometer. In this method, 1-liter water samples are first filtered, either in the field or in the laboratory, using a 0.7-micrometer (um) nominal pore size glass-fiber filter to remove suspended solids. The filtered samples then are passed through cleaned and conditioned SPE cartridges at a rate of about 15

  8. Preparative Separation and Purification of the Total Flavonoids in Scorzonera austriaca with Macroporous Resins

    OpenAIRE

    Yang Xie; Qiu-Shi Guo; Guang-Shu Wang

    2016-01-01

    The use of macroporous resins for the separation and purification of total flavonoids to obtain high-purity total flavonoids from Scorzonera austriaca was studied. The optimal conditions for separation and purification of total flavonoids in S. austriaca with macroporous resins were as follows: D4020 resin columns were loaded with crude flavonoid extract solution, and after reaching adsorptive saturation, the columns were eluted successively with 5 bed volumes (BV) of water, 5 BV of 5% (v/v) ...

  9. Cementation of residue ion exchange resins at Rocky Flats

    Energy Technology Data Exchange (ETDEWEB)

    Dustin, D.F.; Beckman, T.D.; Madore, C.M.

    1998-03-03

    Ion exchange resins have been used to purify nitric acid solutions of plutonium at Rocky Flats since the 1950s. Spent ion exchange resins were retained for eventual recovery of residual plutonium, typically by incineration followed by the aqueous extraction of plutonium from the resultant ash. The elimination of incineration as a recovery process in the late 1980s and the absence of a suitable alternative process for plutonium recovery from resins led to a situation where spent ion exchange resins were simply placed into temporary storage. This report describes the method that Rocky Flats is currently using to stabilize residue ion exchange resins. The objective of the resin stabilization program is: (1) to ensure their safety during interim storage at the site, and (2) to prepare them for ultimate shipment to the Waste Isolation Pilot Plant (WIPP) in New Mexico. Included in the discussion is a description of the safety concerns associated with ion exchange resins, alternatives considered for their stabilization, the selection of the preferred treatment method, the means of implementing the preferred option, and the progress to date.

  10. Development of a composite resin disclosing agent based on the understanding of tooth staining mechanisms.

    Science.gov (United States)

    Abdallah, Mohamed-Nur; Light, Nathan; Amin, Wala M; Retrouvey, Jean-Marc; Cerruti, Marta; Tamimi, Faleh

    2014-06-01

    To characterize the surface composition of dental enamel and composite resin, assess the ability of dyes with different affinities to stain these surfaces, and use this information to develop a disclosing agent that stains composite resin more than dental enamel. One hundred and ten sound extracted teeth were collected and 60 discs of composite resin, 9 mm diameter and 3 mm thick, were prepared. X-ray photoelectron spectroscopy (XPS) was employed to determine the elemental composition on the different surfaces. A tooth shade spectrophotometer was used to assess the change in shade after staining the surfaces with different dyes. XPS analysis revealed that surfaces of both outer dental enamel and composite resin contained relatively high amounts of carbon, specifically hydrocarbons. Both dental enamel and composite surfaces were stainable with the hydrophobic dye (pcomposite resin was stained more than the dental enamel (pcomposite resin might explain their high affinity to be stained by food and beverages containing hydrophobic molecules. The composite resin is more stainable by hydrophobic dyes than dental enamel. We used this information to develop an agent for disclosing composite resins that could be used to visualize composite resins that need to be removed. Removal of composite resin can be problematic, time consuming and stressful to the dental practitioner. A composite disclosing agent would help the dental practitioner identify the composite resin and facilitate its removal without damaging the adjacent healthy tooth tissues. Copyright © 2014 Elsevier Ltd. All rights reserved.

  11. Chromatographic determination of the radiochemical purity of [[sup 131]I]MIBG [metaiodobenzylguanidine] infusion fluids: a comparison and discussion of the chromatographic characteristics using three different techniques

    Energy Technology Data Exchange (ETDEWEB)

    Wafelman, A.R.; Beijnen, J.H. (Slotervaart Hospital, Amsterdam (Netherlands). Hospital Pharmacy Nederlands Kanker Inst. ' Antoni van Leeuwenhoekhuis' , Amsterdam (Netherlands)); Hoefnagel, C.A. (Nederlands Kanker Inst. ' Antoni van Leeuwenhoekhuis' , Amsterdam (Netherlands))

    1993-05-01

    This paper proposes a reproducible and validated assay based on solid phase extraction for the determination of the level of free [[sup 131]I]iodide in [[sup 131]I]metaiodobenzylguanidine infusion fluids. The method has been compared with HPLC and TLC assays. Furthermore, a TLC system is introduced that allows the separation between metaiodobenzylguanidine, its chemical precursor metaiodobenzylamine and iodide. Attention is paid to the chromatographic characteristics of the analytes, with a discussion of the possible retention mechanisms. (Author).

  12. Gas chromatographic determination of chloramphenicol residues in shrimp: interlaboratory study.

    Science.gov (United States)

    Munns, R K; Holland, D C; Roybal, J E; Storey, J M; Long, A R; Stehly, G R; Plakas, S M

    1994-01-01

    An interlaboratory study of a gas chromatographic method for determining chloramphenicol (CAP) residues in shrimp was conducted. An internal standard (Istd), the meta isomer of CAP, was added to the shrimp, and the treated shrimp were homogenized with ethyl acetate. The ethyl acetate extract was defatted with hexane, and the CAP was partitioned into ethyl acetate from an aqueous salt solution. The ethyl acetate was evaporated, and the dried residue was treated with Sylon, a trimethylsilyl derivatizing agent, to yield the trimethylsilyl derivative of CAP. A portion of the solution containing the derivative was injected into a gas chromatograph equipped with an electron capture detector. Levels of fortified and incurred CAP were calculated from the peak area ratio of standard CAP to Istd. Recoveries of CAP from tissue directly fortified at 5 ppb were 102% (within-laboratory relative standard deviation [RSDr] = 5.6%), 104% (RSDr = 5.5%), and 108% (RSDr = 6.3%) from Laboratories 1, 2, and 3, respectively. Incurred-CAP residues at 5 and 10 ppb levels were also determined, with the following results: Laboratory 1: composite A, 4.56 ppb (RSDr = 14.0%); composite B, 8.38 ppb (RSDr = 11.6%); Laboratory 2: composite A, 4.17 ppb (RSDr = 12.5%); composite B, 8.90 ppb (RSDr = 5.60%); Laboratory 3: composite A, 4.66 ppb (RSDr = 14.9%); composite B, 11.0 ppb (RSDr = 11.8%).

  13. Solvent impregnated resins for the removal of low concentration phenol from water

    NARCIS (Netherlands)

    Burghoff, B.; Goetheer, E.L.V.; Haan, A.B. de

    2008-01-01

    The focus of this investigation is the development of a solvent impregnated resin for phenol removal from dilute aqueous solutions. Using a solvent impregnated resin (SIR) eliminates the problem of emulsification encountered in liquid-liquid extraction. Impregnated MPP particles and impregnated XAD1

  14. Agarwood-type Resin from Gyrinops walla Gaertn: A New Discovery

    Directory of Open Access Journals (Sweden)

    S.M.C.U.P. Subasinghe

    2012-10-01

    Full Text Available Agarwood is an expensive resinous product extracted from some members of Aquilaria andGyrinops species of the family Thymalaeaceae. Agarwood essential oil is a highly valued perfumeryproduct in modern cosmetics and traditional Attar. Agarwood extraction from the above species andproduct manufacturing are done in India and Southeast Asian countries. However, overharvesting, lownatural regeneration, and legal restrictions at present, have limited the supply of this product.Gyrinops walla is recorded in the wet zone of Sri Lanka, and it had been very rarely recorded inextreme Southwest India. However, recent reports of the abundance of G. walla in India are hard to find.Studies were not conducted in the past for G. walla on its ability of agarwood resin production and thequality of that resin. This study is the first to identify the agarwood resin formation and the quality of G.walla which can be used as a substitute for that of Aquilaria and other species of Gyrinops.Resinous tissues were extracted from six G. walla trees for the present study from two differentareas, i.e., Labugama and Yagirala of the wet zone of Sri Lanka. The resins were solvent extracted in thelaboratory and the resin quality was tested using gas chromatography analysis. The results indicated anextreme similarity of the compounds of G. walla resin with that of commercially available agarwoodresins. However, further studies should be conducted to identify G. walla distribution and formation ofagarwood.

  15. Chromatographic methods in the study of autism.

    Science.gov (United States)

    Żurawicz, Ewa; Kałużna-Czaplińska, Joanna; Rynkowski, Jacek

    2013-10-01

    Research into biomarkers of autism is a new means of medical intervention in this disease. Chromatographic techniques, especially coupled with mass spectrometry, are widely used in determination of biomarkers and assessment of effectiveness of autism therapy owing to their sensitivity and selectivity. Among the chromatographic techniques gas chromatography and liquid chromatography, especially high-performance liquid chromatography, have found application in clinical trials. The high-performance liquid chromatography technique allows an analysis of liquid samples with a wide range of molecules, small and large, providing an opportunity to perform advanced assays within a short time frame. Gas chromatography with the appropriate preparation of samples (gaseous and liquid) and a selection of analysis conditions enables the separation of thermally stable, volatile and non-volatile organic substances in short runtimes. The chromatographic techniques that are currently used in metabolic studies in autism are designed to identify abnormalities in three areas: the metabolism of neurotransmitters, nutritional and metabolic status and manifestations of oxidative stress. This review presents a necessary theoretical introduction and examples of applications of chromatographic studies of disorder markers in autism.

  16. 40 CFR 1065.267 - Gas chromatograph.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 32 2010-07-01 2010-07-01 false Gas chromatograph. 1065.267 Section 1065.267 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR POLLUTION CONTROLS ENGINE-TESTING PROCEDURES Measurement Instruments Hydrocarbon Measurements § 1065.267 Gas...

  17. Functional chromatographic technique for natural product isolation†

    Science.gov (United States)

    Lau, Eric C.; Mason, Damian J.; Eichhorst, Nicole; Engelder, Pearce; Mesa, Celestina; Kithsiri Wijeratne, E. M.; Gunaherath, G. M. Kamal B.; Leslie Gunatilaka, A. A.

    2015-01-01

    Natural product discovery arises through a unique interplay between chromatographic purification and biological assays. Currently, most techniques used for natural product purification deliver leads without a defined biological action. We now describe a technique, referred to herein as functional chromatography, that deploys biological affinity as the matrix for compound isolation. PMID:25588099

  18. Cyclic electrophoretic and chromatographic separation methods

    NARCIS (Netherlands)

    Eijkel, Jan C.T.; Berg, van den Albert; Manz, Andreas

    2004-01-01

    A review is given of the application of cyclic analytical methods in capillary electroseparation (CE) and liquid chromatography (LC) systems. Cyclic methods have been used since the early sixties in chromatographic systems to overcome pressure limitations to resolution. From the early nineties on th

  19. Functional chromatographic technique for natural product isolation†

    OpenAIRE

    Lau, Eric C.; Mason, Damian J.; Eichhorst, Nicole; Engelder, Pearce; Mesa, Celestina; Kithsiri Wijeratne, E. M.; Gunaherath, G. M. Kamal B.; Leslie Gunatilaka, A. A.; La Clair, James J.; Chapman, Eli

    2015-01-01

    Natural product discovery arises through a unique interplay between chromatographic purification and biological assays. Currently, most techniques used for natural product purification deliver leads without a defined biological action. We now describe a technique, referred to herein as functional chromatography, that deploys biological affinity as the matrix for compound isolation.

  20. Evaluation of ion exchange resins for iron control in copper electro-winning solutions; Evaluacion de resinas de intercambio ionico para el control de hierro en soluciones de electro-obtencion de cobre

    Energy Technology Data Exchange (ETDEWEB)

    Parada, F.; Dreisinger, D.; Wilkomirsky, I.

    2010-07-01

    Two commercial resins were evaluated for the extraction of iron from a copper electrowinning solution. Both resins efficiently extract iron. The Mono phosphonic resin has a greater charge capacity than the Diphonix resin and the Diphonix resin shows faster kinetics. Experimental results of the interrupted test and tests with different particle size of resins have demonstrated that extraction kinetics is controlled by diffusion into the particle in both resins. A good agreement with Fick's model for diffusion inside the particles confirms the proposed mechanism. Finally, temperature favors the process kinetics and its effect on the diffusion coefficient follows Arrhenius law, obtaining a value of 4,89 kcal/mol for the Mono phosphonic resin and 4,94 kcal/mol for the Diphenox resin. The aforementioned values are close to typical values for the proposed diffusional control which are 6 to 10 kcal/mol. (Author)

  1. Tadpole toxicity prediction using chromatographic systems.

    Science.gov (United States)

    Fernández-Pumarega, Alejandro; Amézqueta, Susana; Fuguet, Elisabet; Rosés, Martí

    2015-10-30

    Toxicity has been emulated in tadpole species through chromatographic systems. The parameter studied to evaluate the non-specific toxicity of a compound is the narcosis concentration (Cnar), which is defined as the concentration needed for the immobilization of the organism. Because experimental investigation with animals is lengthy, costly, technically difficult, and ethically questionable, there is a great interest in developing surrogate physicochemical systems able to emulate biological systems to obtain the same information in a faster, more economic, and easier manner. In order to see which chromatographic systems would be able to emulate tadpole narcosis, both, tadpole narcosis data and data in several chromatographic and electrophoretic systems, were fitted to a linear solvation energy relationship (LSER) model. Thus, by comparison of the models it was possible to see which of the chromatographic systems were more similar to the biological one. The physicochemical systems that best emulate tadpole narcosis were an HPLC system based on an immobilized artificial membrane (IAM) column, and two micellar electrokinetic chromatography (MEKC) systems based on sodium taurocholate (STC) and a mixture of sodium dodecylsulphate (SDS) and Brij 35 as surfactants. A system based on a RP18 HPLC column also was selected for comparison because it is a common column in most analytical laboratories. To establish the models, a set of compounds with known Cnar values were analyzed in the chromatographic, and electrophoretic selected systems and, then, the retention factor (k) was correlated to the concentration of narcosis. Statistics showed that the system based on STC micelles was the best to emulate toxicity in tadpoles. The robustness and predictive ability of the developed models were validated.

  2. 离子液体/苯并15-冠-5浸渍XAD-7树脂萃取分离锂同位素%Extraction Separation of Lithium Isotopes by Using XAD-7 Resins Impregnated With Ionic Liquid and Benzo-15-Crown-5

    Institute of Scientific and Technical Information of China (English)

    顾玲; 孙晓利; 任冬红; 邱丹; 顾志国; 李在均

    2015-01-01

    Imidazolium-type ionic liquid ([C8 mim][BF4 ],[C8 mim][PF6 ]and [C8 mim] [(SO2 CF3 )2 N])and benzo-15-crown-5 were immobilized on XAD-7 resin to obtain the im-pregnated resin for lithium isotopes separation.IR and SEM characterizations of the impreg-nated resins indicate that ionic liquids and benzo-15-crown-5 are immobilized in the resins successfully and the thermal analysis indicates that the materials are thermally stable.The optimum E was obtained in the initial solution at pH=5.55.The larger extraction percenta-ges and separation factors values were obtained from LiSCN solution and CF3 COOLi solu-tion,respectively.The maximum single-stage isotopes separation factor of 6 Li/7 Li is up to 1.045±0.002.The equilibrium time of extraction is attained in 2.5-3 h.The thermodynamic parameters of the system were presented and revealed that the extraction reaction was a spontaneous process and the temperature had slight influence on the extraction separation of lithium isotopes.The mechanism of extraction system show that 6 Li enriches in the solid phase and 7 Li concentrates in the aqueous phase.The impregnated resins can be regenerated and reused for lithium isotopes separation.%以 XAD-7树脂为支撑担体制备了含有三种不同咪唑型离子液体([C8 mim][BF4]、[C8 mim][PF6]、[C8 mim][(SO2 CF3)2 N])和萃取剂(苯并15-冠-5)的浸渍树脂,并用于锂同位素的萃取分离。浸渍树脂的红外和扫描电镜表征表明,离子液体成功负载到了树脂上;热重分析表明,该浸渍树脂具有良好的热稳定性。在水相初始 pH=5.55时,浸渍树脂具有最佳萃取率。浸渍树脂在 LiSCN 溶液中具有较高的萃取率,而在CF3 COOLi 溶液中呈现较大的单级分离因子,最大单级分离因子达到1.045±0.002。浸渍树脂的萃取平衡时间为2.5~3 h。萃取热力学研究表明,该反应为自发过程,温度对体系的影响较小。6 Li 富集于固相,7 Li 富集在水相。该系列浸渍树脂易于再生,可循环使用。

  3. Fatty acids determination in Bronte pistachios by gas chromatographic method.

    Science.gov (United States)

    Pantano, Licia; Lo Cascio, Giovanni; Alongi, Angelina; Cammilleri, Gaetano; Vella, Antonio; Macaluso, Andrea; Cicero, Nicola; Migliazzo, Aldo; Ferrantelli, Vincenzo

    2016-10-01

    A gas chromatographic with flame ionization detector (GC-MS FID) method for the identification and quantification of fatty acids based on the extraction of lipids and derivatisation of free acids to form methyl esters was developed and validated. The proposed method was evaluated to a number of standard FAs, and Bronte pistachios samples were used for that purpose and to demonstrate the applicability of the proposed method. In this regard, repeatability, mean and standard deviation of the analytical procedure were calculated. The results obtained have demonstrated oleic acid as the main component of Bronte pistachios (72.2%) followed by linoleic acid (13.4%) and showed some differences in composition with respect to Tunisian, Turkish and Iranian pistachios.

  4. Liquid Chromatographic Method for Determination of Nisoldipine from Pharmaceutical Samples

    Directory of Open Access Journals (Sweden)

    Amit Gupta

    2010-01-01

    Full Text Available A simple and specific high performance thin layer chromatographic method was developed and validated for the determination of nisoldipine from tablet dosage form. The method was carried out at 320 nm after extraction of drug in methanol. The method uses aluminum plates pre-coated with silica gel 60F-254 as stationary phase and cyclohexane-ethyl acetate-toluene (3:3:4, v/v/v as mobile phase. Linearity was established over a range of 400-2400 ng per zone. Both peak area ratio and peak height ratio showed acceptable correlation coefficient i.e. more than 0.99. However we used peak area for validation purpose. Intra-day and inter-day precision was determined and found to have less than 6.0 % RSD.

  5. Resin composite repair: Quantitative microleakage evaluation of resin-resin and resin-tooth interfaces with different surface treatments.

    Science.gov (United States)

    Celik, Cigdem; Cehreli, Sevi Burcak; Arhun, Neslihan

    2015-01-01

    The aim was to evaluate the effect of different adhesive systems and surface treatments on the integrity of resin-resin and resin-tooth interfaces after partial removal of preexisting resin composites using quantitative image analysis for microleakage testing protocol. A total of 80 human molar teeth were restored with either of the resin composites (Filtek Z250/GrandioSO) occlusally. The teeth were thermocycled (1000×). Mesial and distal 1/3 parts of the restorations were removed out leaving only middle part. One side of the cavity was finished with course diamond bur and the other was air-abraded with 50 μm Al2O3. They were randomly divided into four groups (n = 10) to receive: Group 1: Adper Single Bond 2; Group 2: All Bond 3; Group 3: ClearfilSE; Group 4: BeautiBond, before being repaired with the same resin composite (Filtek Z250). The specimens were re-thermocycled (1000×), sealed with nail varnish, stained with 0.5% basic fuchsin, sectioned mesiodistally and photographed digitally. The extent of dye penetration was measured by image analysis software (ImageJ) for both bur-finished and air-abraded surfaces at resin-tooth and resin-resin interfaces. The data were analyzed statistically. BeautiBond exhibited the most microleakage at every site. Irrespective of adhesive and initial composite type, air-abrasion showed less microleakage except for BeautiBond. The type of initial repaired restorative material did not affect the microleakage. BeautiBond adhesive may not be preferred in resin composite repair in terms of microleakage prevention. Surface treatment with air-abrasion produced the lowest microleakage scores, independent of the adhesive systems and the pre-existing resin composite type. Pre-existing composite type does not affect the microleakage issue. All-in-one adhesive resin (BeautiBond) may not be preferred in resin composite repair in terms of microleakage prevention.

  6. System for removing contaminants from plastic resin

    Science.gov (United States)

    Bohnert, George W.; Hand, Thomas E.; DeLaurentiis, Gary M.

    2010-11-23

    A resin recycling system that produces essentially contaminant-free synthetic resin material in an environmentally safe and economical manner. The system includes receiving the resin in container form. A grinder grinds the containers into resin particles. The particles are exposed to a solvent in one or more solvent wash vessels, the solvent contacting the resin particles and substantially removing contaminants on the resin particles. A separator is used to separate the resin particles and the solvent. The resin particles are then placed in solvent removing element where they are exposed to a solvent removing agent which removes any residual solvent remaining on the resin particles after separation.

  7. Stingless bees use terpenes as olfactory cues to find resin sources.

    Science.gov (United States)

    Leonhardt, S D; Zeilhofer, S; Blüthgen, N; Schmitt, Thomas

    2010-09-01

    Insects largely rely on olfactory cues when seeking and judging information on nests, partners, or resources. Bees are known to use volatile compounds-besides visual cues-to find flowers suitable for pollen and nectar collection. Tropical stingless bees additionally collect large amounts of plant resins for nest construction, nest maintenance, nest defense, and to derive chemical constituents for their cuticular profiles. We here demonstrate that stingless bees of Borneo also use olfactory cues to find tree resins. They rely on volatile mono- and sesquiterpenes to locate or recognize known resin sources. Moreover, by modifying resin extracts, we found that stingless bees do not use the entire resin bouquet but relative proportions of several terpenes. In doing so, the bees are able to learn specific tree resin profiles and distinguish between tree species and partly even tree individuals.

  8. Flame Retardant Epoxy Resins

    Science.gov (United States)

    Thompson, C. M.; Smith, J. G., Jr.; Connell, J. W.; Hergenrother, P. M.; Lyon, R. E.

    2004-01-01

    As part of a program to develop fire resistant exterior composite structures for future subsonic commercial aircraft, flame retardant epoxy resins are under investigation. Epoxies and their curing agents (aromatic diamines) containing phosphorus were synthesized and used to prepare epoxy formulations. Phosphorus was incorporated within the backbone of the epoxy resin and not used as an additive. The resulting cured epoxies were characterized by thermogravimetric analysis, propane torch test, elemental analysis and microscale combustion calorimetry. Several formulations showed excellent flame retardation with phosphorous contents as low as 1.5% by weight. The fracture toughness of plaques of several cured formulations was determined on single-edge notched bend specimens. The chemistry and properties of these new epoxy formulations are discussed.

  9. Paramagnetic epoxy resin

    Directory of Open Access Journals (Sweden)

    E. C. Vazquez Barreiro

    2017-01-01

    Full Text Available This work illustrates that macrocycles can be used as crosslinking agents for curing epoxy resins, provided that they have appropriate organic functionalities. As macrocycles can complex metal ions in their structure, this curing reaction allows for the introduction of that metal ion into the resin network. As a result, some characteristic physical properties of the metallomacrocycle could be transferred to the new material. The bisphenol A diglycidyl ether (BADGE, n = 0 and hemin (a protoporphyrin IX containing the Fe(III ion, and an additional chloride ligand have been chosen. The new material has been characterized by differential scanning calorimetry (DSC, thermogravimetric analysis (TGA, Fourier Transform Infrared (FT-IR, Nuclear Magnetic Resonance (NMR, Transmission Electron Microscopy (TEM, and magnetic susceptibility measurements. Fe(III remains in the high-spin state during the curing process and, consequently, the final material exhibits the magnetic characteristics of hemin. The loss of the chlorine atom ligand during the cure of the resin allows that Fe(III can act as Lewis acid, catalyzing the crosslinking reactions. At high BADGE n = 0/hemin ratios, the formation of ether and ester bonds occurs simultaneously during the process.

  10. Liquid chromatographic determination of benzo(a)pyrene in total particulate matter of cigarette smoke

    Energy Technology Data Exchange (ETDEWEB)

    Tomkins, B.A.; Jenkins, R.A.; Griest, W.H.; Reagan, R.R.; Holladay, S.K.

    1985-09-01

    The benzo(a)pyrene (BaP) delivery of reference and commercially available tobacco cigarettes, as well as reference and placebo marijuana cigarettes, is determined using a sequential liquid chromatographic/liquid chromatographic procedure. The total particulate matter of sample cigarette smoke is collected using a Cambridge filter pad, which is ultrasonically extracted with acetone. The resulting extract is filtered, then fractionated using semipreparative-scale normal phase liquid chromatography (LC). Quantitative determination is achieved using analytical-scale reverse phase LC equipped with a fluorescence detector. The method is precise (+/- 10-15% relative standard deviation) and yields 85% or better BaP recovery at the ng/cig. level. A single pad may be analyzed in 8 person-hours, while a more typical lot of 12 pads (6 pads each for 2 cigarette brands) may be analyzed in 10 person-days.

  11. Dry PMR-15 Resin Powders

    Science.gov (United States)

    Vannucci, Raymond D.; Roberts, Gary D.

    1988-01-01

    Shelf lives of PMR-15 polymides lengthened. Procedure involves quenching of monomer reactions by vacuum drying of PRM-15 resin solutions at 70 to 90 degree F immediately after preparation of solutions. Absence of solvent eliminates formation of higher esters and reduces formation of imides to negligible level. Provides fully-formulated dry PMR-15 resin powder readily dissolvable in solvent at room temperature immediately before use. Resins used in variety of aerospace, aeronautical, and commercial applications.

  12. Resin regeneration device for condensate desalter

    Energy Technology Data Exchange (ETDEWEB)

    Segawa, Yoshihiro [Toshiba Engineering Co. Ltd., Kawasaki, Kanagawa (Japan); Hirose, Yuki

    1998-07-28

    The present invention provides a resin regeneration device for a condensate desalter of a nuclear power plant. Namely, both anionic and cationic exchange resins are supplied in a mixed state from a forwarding water desalting tower to an anionic resin regeneration tower. In the anionic resin generation tower, the resin is once separated to an anionic exchange region layer, a mixed resin layer and an cationic exchange resin layer in this order from the upper portion by water injected from a stirring water injection tube disposed at the bottom. Then, water is injected from a developing water injection tube disposed at the lower portion of the mixed resin layer to develop the cationic exchange resin layer and the mixed resin layer to the upper portion of the cationic resin regeneration tower. Subsequently, the amount of the injection of the developing water is reduced to such a flow rate that only the anionic exchange resin is precipitated. Then, a cationic exchange resin layer is formed at the upper portion and an anion exchange resin layer is formed at the lower portion of the developing water injection tube of the cationic resin regeneration tower. The anionic exchange resin is transferred to the anionic exchange resin regeneration tower in this state. According to the present invention, the mixed resin layer can be separated to anionic and cationic exchange resins easily and reliably. (I.S.)

  13. Phytochemical screening and evaluation of the central nervous system activity of the ethanolic extract of Eugenia clarensis Britton & P.Wilson

    Directory of Open Access Journals (Sweden)

    Nghia TM. Nguyen

    2016-02-01

    Full Text Available Context: Eugenia clarensis Britton & P. Wilson is an endangered plant endemic of central region of Cuba. Aims: To perform phytochemical profile of ethanolic leaf extract of E. clarensis and evaluate its central nervous system (CNS activity. Methods: The dried powder of leaves of E. clarensis was exhaustively extracted with ethanol by maceration. This extract underwent preliminary phytochemical analysis and these results were corroborated by the thin layer chromatographic technique. CNS effects were investigated in NMRI mice at doses 200, 400 and 800 mg/kg using Irwin test, curiosity tests and traction. Results: Phytochemical screening suggested the presence of phenols, tannins, triterpenoids, sterols, flavonoids, coumarins, quinones, resins and reducing sugar. The oral administration of this extract, in Irwin test, produced slight reduction in spontaneous motor activity and muscle tone in mice at doses of 400 and 800 mg/kg, moreover, it exhibited diuretic activity. In addiction this extract at dose 800 mg/kg decreased number of times which mice introduced its head into holes in comparison with the negative control. In the traction test, the mice treated with the extract showed a non-significant failure in traction at all doses tested. Conclusions: These findings indicate that the extract in higher doses has exerts a weak sedative and non-effect about the motor coordination. The results obtained in the preliminary phytochemical testing thus suggest that the ethanolic leaf extract of E. clarensis contains some metabolites, which may be responsible of sedative action.

  14. Branched polymeric media: Perchlorate-selective resins from hyperbranched polyethyleneimine

    KAUST Repository

    Chen, Dennis P.

    2012-10-02

    Perchlorate (ClO4 -) is a persistent contaminant found in drinking groundwater sources in the United States. Ion exchange (IX) with selective and disposable resins based on cross-linked styrene divinylbenzene (STY-DVB) beads is currently the most commonly utilized process for removing low concentrations of ClO4 - (10-100 ppb) from contaminated drinking water sources. However, due to the low exchange capacity of perchlorate-selective STY-DVB resins (∼0.5-0.8 eq/L), the overall cost becomes prohibitive when treating groundwater with higher concentration of ClO4 - (e.g., 100-1000 ppb). In this article, we describe a new perchlorate-selective resin with high exchange capacity. This new resin was prepared by alkylation of branched polyethyleneimine (PEI) beads obtained from an inverse suspension polymerization process. Batch and column studies show that our new PEI resin with mixed hexyl/ethyl quaternary ammonium chloride exchange sites can selectively extract trace amounts of ClO4 - from a makeup groundwater (to below detection limit) in the presence of competing ions. In addition, this resin has a strong-base exchange capacity of 1.4 eq/L, which is 1.75-2.33 times larger than those of commercial perchlorate-selective STY-DVB resins. The overall results of our studies suggest that branched PEI beads provide versatile and promising building blocks for the preparation of perchlorate-selective resins with high exchange capacity. © 2012 American Chemical Society.

  15. [Effect of emulsion on chromatographic process].

    Science.gov (United States)

    Jiang, Yulei; Li, Xi

    2004-11-01

    The types and features of concentration wave of the chromatographic process in which the mobile phase was emulsion were studied theoretically by the method of characteristics and the concept of multi mobile phase chromatography. When the mobile phase is an emulsion, solute is partitioned between the inner and outer phases of the emulsion as well as simultaneously adsorbed on the stationary phase resulting in the great difference of concentration profiles from the case in which the mobile phase is homogenous. The various profiles and mechanisms of concentration wave of the chromatographic process in which the partition relationship between the inner and outer phases of the emulsion and the adsorption isotherm on the stationary phase were both Langmuir-like were analyzed and discussed with corresponding examples, and the comparison with the case in which the mobile phase is homogenous is also done. It is shown that the chromatographic progress with emulsion is more complicated and multiple. The existence of multi mobile phases may sharpen simple wave to be shock wave or diffuse shock wave to be simple wave.

  16. nduced hyperlipidemic rats. Methods: Column chromatographic fractionation of butanol fraction of total methanol extract of leaves of Bauhinia variegata (Linn. yields four sub-fractions (sub-fraction A-D. All sub-fractions tested for their anti-hyperlipidemic activity. Sub-fractions administered at a dose of 65 mg/kg (oral to the Triton WR-1339 induced hyperlipidemic rats and total cholesterol, triglycerides, HDL, LDL and VLDL

    Directory of Open Access Journals (Sweden)

    Deepak Kumar

    2012-10-01

    Full Text Available Objective: To investigate the effect and evaluation of Anti-hyperlipidemic activity guided subfraction isolated from total methanolic extract of Bauhinia variegata (Linn. leaves on Triton WR-1339 induced hyperlipidemic rats. Methods: Column chromatographic fractionation of butanol fraction of total methanol extract of leaves of Bauhinia variegata (Linn. yields four subfractions (sub-fraction A-D. All sub-fractions tested for their anti-hyperlipidemic activity. Subfractions administered at a dose of 65 mg/kg (oral to the Triton WR-1339 induced hyperlipidemic rats and total cholesterol, triglycerides, HDL, LDL and VLDL level in the blood were checked. Results: Sub-fraction D showed significant reduction (P<0.05 among four sub-fraction in comparison with standard drug fenofibrate. Conclusions: From the above study it could be concluded that butanol sub-fraction D of Bauhinia variegata (Linn. not only have resulted in significant reduction in cholesterol, triglyceride, LDL, VLDL level but also increases the HDL level at a reduced dose level.

  17. Solid-phase microextraction-gas chromatographic determination of volatile monoaromatic hydrocarbons in soil.

    Science.gov (United States)

    Zygmunt, B; Namiesnik, J

    2001-08-01

    Benzene, toluene, ethylbenzene, three isomers of xylene, and cumene have been isolated and enriched from soil samples by a combination of water extraction at room and elevated temperature and headspace-solid-phase microextraction before their gas chromatographic-mass spectrometric (GC-MS) determination. The conditions used for all stages of sample preparation and chromatographic analysis were optimized. Analytes sampled on a polydimethylsiloxane-coated solid-phase microextraction fiber were thermally desorbed in the split/splitless injector of a gas chromatograph (GC) coupled with a mass spectrometer (MS). The desorption temperature was optimized. The GC separation was performed in a capillary column. Detection limits were found to be of the order of ca. 1 ng g(-1). Relative recoveries of the analytes from soils were found to be highly dependent on soil organic-matter content and on compound identity; they ranged from ca 92 to 96% for sandy soil (extraction at room temperature) and from ca 27 to 55% for peaty soil (extraction at elevated temperature). A few real-world soil samples were analyzed; the individual monoaromatic hydrocarbon content ranged from below detection limits to 6.4 ng g(-1) for benzene and 8.1 for the total of p- + m-xylene.

  18. [Sample preparation methods for chromatographic analysis of organic components in atmospheric particulate matter].

    Science.gov (United States)

    Hao, Liang; Wu, Dapeng; Guan, Yafeng

    2014-09-01

    The determination of organic composition in atmospheric particulate matter (PM) is of great importance in understanding how PM affects human health, environment, climate, and ecosystem. Organic components are also the scientific basis for emission source tracking, PM regulation and risk management. Therefore, the molecular characterization of the organic fraction of PM has become one of the priority research issues in the field of environmental analysis. Due to the extreme complexity of PM samples, chromatographic methods have been the chief selection. The common procedure for the analysis of organic components in PM includes several steps: sample collection on the fiber filters, sample preparation (transform the sample into a form suitable for chromatographic analysis), analysis by chromatographic methods. Among these steps, the sample preparation methods will largely determine the throughput and the data quality. Solvent extraction methods followed by sample pretreatment (e. g. pre-separation, derivatization, pre-concentration) have long been used for PM sample analysis, and thermal desorption methods have also mainly focused on the non-polar organic component analysis in PM. In this paper, the sample preparation methods prior to chromatographic analysis of organic components in PM are reviewed comprehensively, and the corresponding merits and limitations of each method are also briefly discussed.

  19. Shear bond strength evaluation of resin composite bonded to three different liners: TheraCal LC, Biodentine, and resin-modified glass ionomer cement using universal adhesive: An in vitro study

    OpenAIRE

    Deepa, Velagala L; Bhargavi Dhamaraju; Indira Priyadharsini Bollu; Tandri S Balaji

    2016-01-01

    Aims: To compare and evaluate the bonding ability of resin composite (RC) to three different liners: TheraCal LC TM (TLC), a novel resin-modified (RM) calcium silicate cement, Biodentine TM (BD), and resin-modified glass ionomer cement (RMGIC) using an universal silane-containing adhesive and characterizing their failure modes. Materials and Methods: Thirty extracted intact human molars with occlusal cavity (6-mm diameter and 2-mm height) were mounted in acrylic blocks and divided into th...

  20. Experimental study on gold extraction by resin-in-pulp method in Dongxi gold mine and its production practice%东溪金矿树脂矿浆法提金工艺试验研究与生产实践

    Institute of Scientific and Technical Information of China (English)

    韩春国

    2013-01-01

    The paper stated that production practice of resin-in-pulp (RIP) method for the extraction of gold and demonstrated the effective performance of NK 884 resin in adsorbing gold and silver. The practice proved RIP to be better choice than the previous CIP method for Dongxi gold mine. The gold leaching rate is increased by 1. 01 % adsorption rate 0. 77 % ; technical indexes of silver are more significantly improved with leaching rate increased by 8. 34 % and adsorption rate by 28.43 % .%论述了树脂矿浆法提金工艺的生产实践过程,验证了NK884型树脂对金、银所具有的良好吸附性能.生产实践表明,对东溪金矿而言,树脂矿浆法优于其原有的炭浆法.其中,金的浸出率提高1.01%,吸附率提高0.77%;银的技术指标提高更为显著,浸出率提高8.34%,吸附率提高28.43%.

  1. Similarity analyses of chromatographic herbal fingerprints: A review

    Energy Technology Data Exchange (ETDEWEB)

    Goodarzi, Mohammad [Department of Analytical Chemistry and Pharmaceutical Technology, Center for Pharmaceutical Research, Vrije Universiteit Brussel, Laarbeeklaan 103, B-1090 Brussels (Belgium); Russell, Paul J. [Safety and Environmental Assurance Centre, Unilever, Colworth Science Park, Sharnbrook, Bedfordshire MK44 1LQ (United Kingdom); Vander Heyden, Yvan, E-mail: yvanvdh@vub.ac.be [Department of Analytical Chemistry and Pharmaceutical Technology, Center for Pharmaceutical Research, Vrije Universiteit Brussel, Laarbeeklaan 103, B-1090 Brussels (Belgium)

    2013-12-04

    Graphical abstract: -- Highlights: •Similarity analyses of herbal fingerprints are reviewed. •Different (dis)similarity approaches are discussed. •(Dis)similarity-metrics and exploratory-analysis approaches are illustrated. •Correlation and distance-based measures are overviewed. •Similarity analyses illustrated by several case studies. -- Abstract: Herbal medicines are becoming again more popular in the developed countries because being “natural” and people thus often assume that they are inherently safe. Herbs have also been used worldwide for many centuries in the traditional medicines. The concern of their safety and efficacy has grown since increasing western interest. Herbal materials and their extracts are very complex, often including hundreds of compounds. A thorough understanding of their chemical composition is essential for conducting a safety risk assessment. However, herbal material can show considerable variability. The chemical constituents and their amounts in a herb can be different, due to growing conditions, such as climate and soil, the drying process, the harvest season, etc. Among the analytical methods, chromatographic fingerprinting has been recommended as a potential and reliable methodology for the identification and quality control of herbal medicines. Identification is needed to avoid fraud and adulteration. Currently, analyzing chromatographic herbal fingerprint data sets has become one of the most applied tools in quality assessment of herbal materials. Mostly, the entire chromatographic profiles are used to identify or to evaluate the quality of the herbs investigated. Occasionally only a limited number of compounds are considered. One approach to the safety risk assessment is to determine whether the herbal material is substantially equivalent to that which is either readily consumed in the diet, has a history of application or has earlier been commercialized i.e. to what is considered as reference material. In order

  2. Sifat Fisis Dan Mekanis Basis Gigi Tiruan Resin Akrilik Polimerisasi Panas Setelah Perendaman Ekstrak Daun Salam (Syzygium Polyanthum Wight)

    OpenAIRE

    Harahap, Fitri Yuniati

    2014-01-01

    Research on the physical and mechanical properties heat cured acrylic resin denture base material immersed bay leaf extract (Syzygium polyanthum wight) has been done. This research aimed to see the effect of immersing time heat cured acrylic resin denture base in the bay leaf extracts for physical and mechanical properties. Samples were immersed in a solution of bay leaf extract with 40% concentration and soaking time 5, 10, 15, 20 and 25 minutes. From the results tests of s...

  3. [Acrylic resin removable partial dentures

    NARCIS (Netherlands)

    Baat, C. de; Witter, D.J.; Creugers, N.H.J.

    2011-01-01

    An acrylic resin removable partial denture is distinguished from other types of removable partial dentures by an all-acrylic resin base which is, in principle, solely supported by the edentulous regions of the tooth arch and in the maxilla also by the hard palate. When compared to the other types of

  4. Extraction of mercury(II) with sulfurized jojoba oil

    Energy Technology Data Exchange (ETDEWEB)

    Wisniak, J.; Schorr, G.; Zacovsky, D.; Belfer, S. (Ben-Gurion Univ. of the Negev, Beersheba (Israel). Dept. of Chemical Engineering)

    1990-09-01

    Sulfurized jojoba oil containing 12% by weight S has been tested as an extractant for Hg(II) from aqueous solutions. This paper reports on experiments performed with the extractant dissolved in a solvent (liquid--liquid extraction) or adsorbed in an appropriate resin matrix (solid--liquid extraction). The extraction characteristics of both systems have been measured and show that sulfurized jojoba oil exhibits very good possibilities as an extractant. The performance of several resins treated with sulfurized jojoba oil for adsorbing mercury(II) was studied. The morphology of the different resins was examined by using scanning electron microscopy. The sulfurized oil is attached to the resin sites through the sulfur atoms; it is estimated that there are about 2 mol of S active sites per kilogram of resin.

  5. DETERMINATION OF FLUORIDE IN HIGHLY SALINATED WATERS BY ION CHROMATOGRAPHY METHOD WITH USE OF SOLID PHASE EXTRACTION FOR SAMPLE PREPARATION

    Directory of Open Access Journals (Sweden)

    Beata Kostka

    2014-10-01

    Full Text Available Solid phase extraction (SPE is one of the most popular methods of matrix elimination in determination of anions by ion chromatography. Possibility of using cartridges containing a cation-exchange resin in the Ag+ and Na+ forms for determination of fluoride in the presence of very high concentration of chloride in mine waters was described in this paper. A Dionex ICS-2500 ion chromatograph was used for separation of anions in gradient elution using IonPac AS19 (4x250 mm separation column along with generated KOH eluent. Fluoride after separation was determined by conductivity detector with suppression. The investigations performed on mine waters (conductivity in the range 12 700 μS/cm–155 000 μS/cm and synthetic brine (38 820 mg/L Cl- and 3 408 mg/L SO4 2- confirmed usefulness of cartridges containing a cation-exchange resin for minimizing matrix influence on results of fluoride determination. The ion chromatography method accompanied by solid phase extraction for sample preparation proved to be very useful for determination of fluoride in highly salinated waters (i.e. mine waters because of low detection limit (0,02 mg/L, good precision (< 2,5 % and accuracy (recovery 91 % – 104 %.

  6. Gas chromatographic determination of yohimbine in commercial yohimbe products.

    Science.gov (United States)

    Betz, J M; White, K D; der Marderosian, A H

    1995-01-01

    The bark of Pausinystalia yohimbe [K. Schumann] Pierre (Rubiaceae), long valued as an aphrodisiac in West Africa, recently has been promoted in the United States as a dietary supplement alternative to anabolic steroids for enhancement of athletic performance. As the number of yohimbe products on the retail market increases, concerns about their safety are raised because of the reported toxicity of yohimbine (the major alkaloid of the plant). Although plant materials are usually identified microscopically, we were unable to identify them in many of the products, because as their labels indicated, the products were mixtures of various botanicals or were bark extracts and contained little or no plant material. A method for extraction and capillary gas chromatographic (GC) separation of the alkaloids of P. yohimbe was, therefore, developed and used to analyze a number of commercial yohimbe products. The method involved solvent extraction and partitioning in chloroform-water followed by separation on a methyl silicone capillary GC column (N-P detection). Comparisons of chromatograms of extracts of authentic bark with those of commercial products indicated that, although many products contained measurable quantities of the alkaloid yohimbine, they were largely devoid of the other alkaloids previously reported in this species. Concentrations of yohimbine in the commercial products ranged from < 0.1 to 489 ppm, compared with 7089 ppm in the authentic material. Authentic bark has been reported to contain up to 6% total alkaloids, 10-15% of which are yohimbine. The possible presence of undeclared diluents in the products was indicated by peaks in product chromatograms but not in those of authentic bark.

  7. 优化大孔树脂提取分离苋菜红色素的工艺%Optimization of Extraction and Separation of Red Pigment from Amaranthus Paniculatus with Macroporous Adsorption Resin

    Institute of Scientific and Technical Information of China (English)

    林海珠; 张云玲; 胥秀英; 郑一敏; 乔源; 傅善权

    2013-01-01

    AB-8 resin was selected out to purify the red pigment of Amaranthus paniculatus by orthogonal design. The best conditions for isolation of the red pigment of Amaranthus paniculatus were determined as follows: pH 3, adsorption velocity 1.2 mL/min, solution adsorbent 15% ethanol and elution velocity 0.9 mL/min. After AB-8 macroporous resin purification, greatly enhance the pigment quality.%采用正交设计实验筛选AB-8大孔树脂纯化苋菜红色素的最佳工艺条件.其最佳工艺为:上样pH值为3、吸附流速1.2mL/min、洗脱剂浓度为15%乙醇溶液、洗脱流速0.9 mL/min.经过AB-8大孔树脂提纯后,提高了苋菜红色素的品质.

  8. D370型树脂在氰化浸出提金工艺中的应用%Application of D 370 type resin in gold extraction process by cyanide leaching

    Institute of Scientific and Technical Information of China (English)

    韩春国; 高玉玺; 王静

    2012-01-01

    Contrast tests on adsorption capacity and preferential adsorption capability among D370, 201 × 4 and 201 ×7 type resins for gold and silver from cyanide pregnant solutions were carried out. And desorption test on D370 type resin followed, which showed that each technical index significantly exceeds that of 201 × 4 and 201 × 7 type res- ins.%对D 370型、201×4型和201×7型树脂从氰化贵液中吸附金、银的吸附容量以及选择性吸附能力进行了对比试验,并对载金D 370型树脂进行了解吸试验.其结果表明,D 370型树脂的各项技术指标,明显优于201×4型和201×7型树脂.

  9. Evaluation and application of anion exchange resins to measure groundwater uranium flux at a former uranium mill site.

    Science.gov (United States)

    Stucker, Valerie; Ranville, James; Newman, Mark; Peacock, Aaron; Cho, Jaehyun; Hatfield, Kirk

    2011-10-15

    Laboratory tests and a field validation experiment were performed to evaluate anion exchange resins for uranium sorption and desorption in order to develop a uranium passive flux meter (PFM). The mass of uranium sorbed to the resin and corresponding masses of alcohol tracers eluted over the duration of groundwater installation are then used to determine the groundwater and uranium contaminant fluxes. Laboratory based batch experiments were performed using Purolite A500, Dowex 21K and 21K XLT, Lewatit S6328 A resins and silver impregnated activated carbon to examine uranium sorption and extraction for each material. The Dowex resins had the highest uranium sorption, followed by Lewatit, Purolite and the activated carbon. Recoveries from all ion exchange resins were in the range of 94-99% for aqueous uranium in the environmentally relevant concentration range studied (0.01-200 ppb). Due to the lower price and well-characterized tracer capacity, Lewatit S6328 A was used for field-testing of PFMs at the DOE UMTRA site in Rifle, CO. The effect on the flux measurements of extractant (nitric acid)/resin ratio, and uranium loading were investigated. Higher cumulative uranium fluxes (as seen with concentrations>1 ug U/gram resin) yielded more homogeneous resin samples versus lower cumulative fluxes (uranium. Resin homogenization and larger volume extractions yield reproducible results for all levels of uranium fluxes. Although PFM design can be improved to measure flux and groundwater flow direction, the current methodology can be applied to uranium transport studies.

  10. Enrichment and purification of total flavonoids from Cortex Juglandis Mandshuricae extracts and their suppressive effect on carbon tetrachloride-induced hepatic injury in Mice.

    Science.gov (United States)

    Zhao, Pan; Qi, Chao; Wang, Gang; Dai, Xinpeng; Hou, Xiaohong

    2015-12-15

    In the present work, a simple and efficient chromatographic separation method was developed for preparative separation and enrichment of total flavonoids (TFs) from Cortex Juglandis Mandshuricae (CJM) extracts and then the protective effect of TFs against CCl4-induced acute liver injury in mice was investigated. Enrichment and purification of TFs from CJM extracts were studied using six macroporous resins and HPD-750 resin was selected as the best resin according to its adsorption and desorption properties. The operating parameters of resin column chromatography were optimized. Under the optimal conditions, TFs from CJM with purity larger than 50% were produced and their antioxidant activity was further evaluated in vitro. The mice were orally administrated with the purified TFs for seven days and then given CCl4 (0.3%, 10mL/kg i.p.). The results showed that TFs of CJM significantly attenuated the activities of serum aspartate transaminase (AST) and alanine transaminase (ALT) compared with model group, as well as the relative liver weight. Histopathological observation also revealed that TFs reduced the incidence of liver lesions and improved hepatocyte abnormality. Moreover, oral administration of TFs significantly enhanced antioxidant enzyme activities (superoxide dismutase (SOD) and glutathione peroxidase (GSH-Px)) and decreased the content of malondialdehyde (MDA). Histopathological and biochemical results elicited that TFs of CJM had significant hepatoprotective activity comparable to the standard silymarin. This is the first time to reveal the protective actions of the TFs from CJM against CCl4-induced liver damage in mice and this natural product should be developed as a new drug for treatment of live injury in future.

  11. Liquid chromatographic determination of beta-naphthoxyacetic acid in tomatoes.

    Science.gov (United States)

    Gökmen, V; Acar, J

    1998-03-06

    An alternative high-performance liquid chromatographic method for the determination of beta-naphthoxyacetic acid (BNOA) in tomatoes is described. BNOA was extracted from tomatoes with acetone-dichloromethane (2:1). The extract was cleaned up by Bio-Beads S-X3 gel-permeation chromatography and by partitioning. A reversed-phase C18 column was used for HPLC analysis. The mobile phase was acetonitrile-2% acetic acid in water (50:50, v/v) pumped at a flow-rate of 1.0 ml/min. Retention time of BNOA was ca. 7 min with a percentage coefficient of variation of 0.71. Resolution of BNOA was good on the column. Percentage recoveries of BNOA were 79.5 +/- 6.82, 94.8 +/- 2.70 and 86.4 +/- 16.43 for the corresponding spiking levels of 0.5, 1.0 and 2.0 micrograms per g tomato, respectively. Analysis of 10 greenhouse tomato samples from local markets in Ankara showed no BNOA residue.

  12. High-Performance Liquid Chromatographic-Tandem Mass Spectrometric Determination of Itraconazole in Human Plasma for Bioavailability and Bioequivalence Studies

    Energy Technology Data Exchange (ETDEWEB)

    Choi, Young Wook; Nam, Dae Young; Kang, Kyoung Hoon; Ha, Kyung Wook; Han, In Hee; Chang, Byung Kon; Yoon, Mi Kyeong; Lee, Jae Hwi [Chung-Ang University, Seoul (Korea, Republic of)

    2006-02-15

    A highly sensitive high-performance liquid chromatographic-tandem mass spectrometric method (HPLC-MSMS) has been developed to quantify itraconazole in human plasma for the purpose of pharmacokinetic studies. Sample preparation was carried out by liquid-liquid extraction using loratadine as an internal standard. Chromatographic separation used a YMC C{sub 18} column, giving an extremely fast total run time of 3 min. The method was validated and used for the bioequivalence study of itraconazole tablets in healthy male volunteers (n = 31). The lower limit of detection proved to be 0.2 ng /mL for itraconazole.

  13. Chromatographic, Spectroscopic and Mass Spectrometric Approaches for Exploring the Habitability of Mars in 2012 and Beyond with the Curiosity Rover

    Science.gov (United States)

    Mahaffy, Paul

    2012-01-01

    The Sample Analysis at Mars (SAM) suite of instruments on the Curiosity Rover of Mars Science Laboratory Mission is designed to provide chemical and isotopic analysis of organic and inorganic volatiles for both atmospheric and solid samples. The goals of the science investigation enabled by the gas chromatograph mass spectrometer and tunable laser spectrometer instruments of SAM are to work together with the other MSL investigations is to quantitatively assess habitability through a series of chemical and geological measurements. We describe the multi-column gas chromatograph system employed on SAM and the approach to extraction and analysis of organic compounds that might be preserved in ancient martian rocks.

  14. Affinity purification of viral protein having heterogeneous quaternary structure: modeling the impact of soluble aggregates on chromatographic performance.

    Science.gov (United States)

    Lipin, Daniel I; Raj, Abhijeet; Lua, Linda H L; Middelberg, Anton P J

    2009-07-24

    Prokaryote-expressed polyomavirus structural protein VP1 with an N-terminal glutathione-S-transferase tag (GST-VP1) self-assembles into pentamer structures that further organize into soluble aggregates of variable size (3.4 x 10(2)-1.8 x 10(4)kDa) [D.I. Lipin, L.H.L. Lua, A.P.J. Middelberg, J. Chromatogr. A 1190 (2008) 204]. The adsorption mechanism for the full range of GST-VP1 soluble aggregates was described assuming a dual-component model [T.Y. Gu, G.J. Tsai, G.T. Tsao, AICHE J. 37 (1991) 1333], with components differentiated by size, and hence pore accessibility, rather than by protein identity. GST-VP1 protein was separated into two component groups: aggregates small enough to access resin pores (LMW: 3.4 x 10(2)-1.4 x 10(3)kDa) and aggregates excluded from the resin pores (HMW: 9.0 x 10(2)-1.8 x 10(4)kDa). LMW aggregates bound to resin at a higher saturation concentration (29.7 g L(-1)) than HMW aggregates (13.3 g L(-1)), while the rate of adsorption of HMW aggregates was an order of magnitude higher than for LMW aggregates. The model was used to predict both batch and packed bed adsorption of GST-VP1 protein in solutions with known concentrations of HMW and LMW aggregates to Glutathione Sepharose HP resin. Asymmetrical flow field flow fractionation with UV absorbance was utilized in conjunction with adsorption experimentation to show that binding of HMW aggregates to the resin was strong enough to withstand model-predicted displacement by LMW aggregates. High pore concentrations of LMW aggregates were also found to significantly inhibit the diffusion rate of further protein in the resin pores. Additional downstream processing experimentation showed that enzymatic cleavage of LMW aggregates to remove GST tags yields more un-aggregated VP1 pentamers than enzymatic cleavage of HMW aggregates. This model can be used to enhance the chromatographic capture of GST-VP1, and suggests an approach for modeling chromatographic purification of proteins that have a range

  15. Selective determination of ammonium ions by high-speed ion-exclusion chromatography on a weakly basic anion-exchange resin column.

    Science.gov (United States)

    Mori, Masanobu; Tanaka, Kazuhiko; Helaleh, Murad I H; Xu, Qun; Ikedo, Mikaru; Ogura, Yutaka; Sato, Shinji; Hu, Wenzhi; Hasebe, Kiyoshi

    2003-05-16

    This paper describes an ion-exclusion chromatographic system for the rapid and selective determination of ammonium ion. The optimized ion-exclusion chromatographic system was established with a polymethacrylate-based weakly basic anion-exchange resin column (TSKgel DEAE-5PW) as the separation column, an aqueous solution containing 0.05 mM tetramethylammonium hydroxide (pH 9.10) as eluent with conductimetric detection for the analyte determination. Under the optimum chromatographic conditions, ammonium ion was determined within 2.3 min with a detection limit (S/N=3) better than 0.125 microM. Ammonium ion in rain and river waters was precisely determined using this ion-exclusion chromatographic system.

  16. Packed multi-channels for parallel chromatographic separations in microchips.

    Science.gov (United States)

    Nagy, Andrea; Gaspar, Attila

    2013-08-23

    Here we report on a simple method to fabricate microfluidic chip incorporating multi-channel systems packed by conventional chromatographic particles without the use of frits. The retaining effectivities of different bottlenecks created in the channels were studied. For the parallel multi-channel chromatographic separations several channel patterns were designed. The obtained multipackings were applied for parallel separations of dyes. The implementation of several chromatographic separation units in microscopic size makes possible faster and high throughput separations.

  17. Determination of rhodamine B in soft drink, waste water and lipstick samples after solid phase extraction.

    Science.gov (United States)

    Soylak, Mustafa; Unsal, Yunus Emre; Yilmaz, Erkan; Tuzen, Mustafa

    2011-08-01

    A new solid phase extraction method is described for sensitive and selective determination of trace levels of rhodamine B in soft drink, food and industrial waste water samples. The method is based on the adsorption of rhodamine B on the Sepabeads SP 70 resin and its elution with 5 mL of acetonitrile in a mini chromatographic column. Rhodamine B was determined by using UV visible spectrophotometry at 556 nm. The effects of different parameters such as pH, amount of rhodamine B, flow rates of sample and eluent solutions, resin amount, and sample volume were investigated. The influences of some alkali, alkali earth and transition metals on the recoveries of rhodamine B were investigated. The preconcentration factor was found 40. The detection limit based on three times the standard deviation of the reagent blank for rhodamine B was 3.14 μg L⁻¹. The relative standard deviations of the procedure were found as 5% in 1×10⁻⁵ mol L⁻¹ rhodamine B. The presented procedure was successfully applied to real samples including soft drink, food and industrial waste water and lipstick samples. Copyright © 2011 Elsevier Ltd. All rights reserved.

  18. Extraction of lactic acid from fermentation broth with anion exchange resin%阴离子交换树脂分离提取发酵液中的乳酸

    Institute of Scientific and Technical Information of China (English)

    迟国达; 王鹏; 徐伟; 黄臣勇

    2012-01-01

    The domestic anion exchange resin 315 was selected to separate lactic acid from the fermentation broth. Adsorption isotherm, kinetics, effect of dynamic adsorption and elution on lactic acid, acetic acid, pyruvic acid and citric acid were studied. Adsorption isotherm results showed that the Freundlich isotherm e- quation agreed well with the adsorption data of organic acids on anion exchange resin 315, and the characteris- tic parameter of this equation n 〉 1. It displayed that the adsorption process belonged to favorable adsorption. Besides, the adsorption kinetics of organic acids on anion exchange resin 315 was mainly controlled by liquid film diffusion, and it accorded well with the Boyd liquid film diffusion model. The optimum dynamic adsorp- tion and elution conditions were determined: adsorption flow-rate, 1.5 BV/h; pH 1.88 ; eluent, deionized water; elution flow-rate, 1 BV/h. Under these conditions, the lactic could be well separated from the fermen- tation broth to achieve the purpose of increasing the yield of lactic acid products and improving product' purity.%为提高乳酸产品收率和纯度,实验筛选得到国产315型阴离子交换树脂,用于分离提取发酵液中乳酸,并研究其对乳酸、乙酸、丙酮酸及柠檬酸的吸附等温线、吸附动力学和动态吸附及洗脱效果.吸附等温线结果表明,315型树脂对乳酸等有机酸的吸附等温线符合Freundlich方程,特征参数n〉1,属于优惠吸附.吸附动力学研究表明,液膜扩散是吸附过程的主要控制步骤,符合Boyd液膜扩散模型.动态吸附及洗脱实验结果表明,以1.5BV/h、pH1.88上柱吸附,再用1BV/h的去离子水洗脱,可实现发酵液中乳酸的良好分离.

  19. 21 CFR 177.1500 - Nylon resins.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Nylon resins. 177.1500 Section 177.1500 Food and... Repeated Use Food Contact Surfaces § 177.1500 Nylon resins. The nylon resins listed in paragraph (a) of... packaging food, subject to the provisions of this section: (a) The nylon resins are manufactured...

  20. 21 CFR 177.2440 - Polyethersulfone resins.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Polyethersulfone resins. 177.2440 Section 177.2440... Components of Articles Intended for Repeated Use § 177.2440 Polyethersulfone resins. Polyethersulfone resins... the purpose of this section, polyethersulfone resins are: (1)...

  1. 21 CFR 177.1655 - Polysulfone resins.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Polysulfone resins. 177.1655 Section 177.1655 Food... of Single and Repeated Use Food Contact Surfaces § 177.1655 Polysulfone resins. Polysulfone resins... purpose of this section, polysulfone resins are: (1)...

  2. 21 CFR 177.1585 - Polyestercarbonate resins.

    Science.gov (United States)

    2010-04-01

    .... Polyestercarbonate resins may be safely used as articles or components of articles intended for use in producing... chloride such that the finished resins are composed of 45 to 85 molepercent ester, of which up to 55 mole... the resins. (3) Residual methylene chloride levels in poly-ester-carbonate resins. Poly-ester...

  3. 21 CFR 178.3930 - Terpene resins.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Terpene resins. 178.3930 Section 178.3930 Food and... and Production Aids § 178.3930 Terpene resins. The terpene resins identified in paragraph (a) of this... the terpene resins identified in paragraph (b) of this section may be safely used as components...

  4. Determination of solute descriptors by chromatographic methods

    Energy Technology Data Exchange (ETDEWEB)

    Poole, Colin F., E-mail: cfp@chem.wayne.edu [Department of Chemistry, Wayne State University, Detroit, MI 48202 (United States); Atapattu, Sanka N.; Poole, Salwa K.; Bell, Andrea K. [Department of Chemistry, Wayne State University, Detroit, MI 48202 (United States)

    2009-10-12

    The solvation parameter model is now well established as a useful tool for obtaining quantitative structure-property relationships for chemical, biomedical and environmental processes. The model correlates a free-energy related property of a system to six free-energy derived descriptors describing molecular properties. These molecular descriptors are defined as L (gas-liquid partition coefficient on hexadecane at 298 K), V (McGowan's characteristic volume), E (excess molar refraction), S (dipolarity/polarizability), A (hydrogen-bond acidity), and B (hydrogen-bond basicity). McGowan's characteristic volume is trivially calculated from structure and the excess molar refraction can be calculated for liquids from their refractive index and easily estimated for solids. The remaining four descriptors are derived by experiment using (largely) two-phase partitioning, chromatography, and solubility measurements. In this article, the use of gas chromatography, reversed-phase liquid chromatography, micellar electrokinetic chromatography, and two-phase partitioning for determining solute descriptors is described. A large database of experimental retention factors and partition coefficients is constructed after first applying selection tools to remove unreliable experimental values and an optimized collection of varied compounds with descriptor values suitable for calibrating chromatographic systems is presented. These optimized descriptors are demonstrated to be robust and more suitable than other groups of descriptors characterizing the separation properties of chromatographic systems.

  5. High performance hand-held gas chromatograph

    Energy Technology Data Exchange (ETDEWEB)

    Yu, C.M.

    1998-04-28

    The Microtechnology Center of Lawrence Livermore National Laboratory has developed a high performance hand-held, real time detection gas chromatograph (HHGC) by Micro-Electro-Mechanical-System (MEMS) technology. The total weight of this hand-held gas chromatograph is about five lbs., with a physical size of 8{close_quotes} x 5{close_quotes} x 3{close_quotes} including carrier gas and battery. It consumes about 12 watts of electrical power with a response time on the order of one to two minutes. This HHGC has an average effective theoretical plate of about 40k. Presently, its sensitivity is limited by its thermal sensitive detector at PPM. Like a conventional G.C., this HHGC consists mainly of three major components: (1) the sample injector, (2) the column, and (3) the detector with related electronics. The present HHGC injector is a modified version of the conventional injector. Its separation column is fabricated completely on silicon wafers by means of MEMS technology. This separation column has a circular cross section with a diameter of 100 pm. The detector developed for this hand-held GC is a thermal conductivity detector fabricated on a silicon nitride window by MEMS technology. A normal Wheatstone bridge is used. The signal is fed into a PC and displayed through LabView software.

  6. Unfolding and aggregation of monoclonal antibodies on cation exchange columns: effects of resin type, load buffer, and protein stability.

    Science.gov (United States)

    Guo, Jing; Carta, Giorgio

    2015-04-03

    The chromatographic behavior of a monoclonal antibody (mAb) that exhibits a pronounced two-peak elution behavior is studied for a range of strong cation exchange resins and with varying load buffer pH and composition. Six stationary phases are considered, including two tentacle-type resins (Fractogel EMD SO3-(M) and Eshmuno S), a resin with grafted polymeric surface extenders (Nuvia S), a resin with a bimodal pore size distribution (POROS HS 50), and two macroporous resins without polymer grafts (Source 30S and UNOsphere Rapid S). The two-peak elution behavior is very pronounced for the tentacle and polymer-grafted resins and for POROS HS 50, but is essentially absent for the two macroporous resins. The extent of this behavior decreases as the buffer pH and concentration increase and, consequently, mAb binding becomes weaker. Replacing sodium with arginine as the buffer counterion, which is expected to decrease the mAb binding strength, nearly completely eliminates the two-peak behavior, while replacing sodium with tetra-n-butylammonium hydroxide, which is expected to increase the mAb binding strength, dramatically exacerbate the effect. As shown by hydrogen-deuterium exchange mass spectrometry (HX-MS), the two-peak elution behavior is related to conformational changes that occur when the mAb binds. These changes result in increased solvent exposure of specific peptides in the Fc-region for either the Fractogel or the Nuvia resin. No significant conformational changes were seen by HX-MS when the mAb was bound to the UNOsphere resin or on the Fractogel resin when arginine was used in lieu of sodium as the load buffer counterion. Experiments with two additional mAbs on the Fractogel resin show that the two-peak elution behavior is dependent on the particular antibody. Circular dichroism suggests that the propensity of different mAbs to either precipitate directly or to form stabilizing intermolecular structures upon exposure to thermal stress can be related to their

  7. Indirect resin composites

    Directory of Open Access Journals (Sweden)

    Nandini Suresh

    2010-01-01

    Full Text Available Aesthetic dentistry continues to evolve through innovations in bonding agents, restorative materials, and conservative preparation techniques. The use of direct composite restoration in posterior teeth is limited to relatively small cavities due to polymerization stresses. Indirect composites offer an esthetic alternative to ceramics for posterior teeth. This review article focuses on the material aspect of the newer generation of composites. This review was based on a PubMed database search which we limited to peer-reviewed articles in English that were published between 1990 and 2010 in dental journals. The key words used were ′indirect resin composites,′ composite inlays,′ and ′fiber-reinforced composites.′

  8. Chromatography resin support

    Science.gov (United States)

    Dobos, James G.

    2002-01-01

    An apparatus and method of using an improved chromatography resin support is disclosed. The chromatography support platform is provided by a stainless steel hollow cylinder adapted for being inserted into a chromatography column. An exterior wall of the stainless steel cylinder defines a groove for carrying therein an "O"-ring. The upper surface of the stainless steel column is covered by a fine stainless steel mesh welded to the edges of the stainless steel cylinder. When placed upon a receiving ledge defined within a chromatography column, the "O"-ring provides a fluid tight seal with the inner edge wall of the chromatography cylinder. The stainless steel mesh supports the chromatography matrix and provides a back flushable support which is economical and simple to construct.

  9. Recovery of value-added fossil resin from El-Maghara coal

    Energy Technology Data Exchange (ETDEWEB)

    Ibrahim, S.S.; Mostafa, S.I. [Central Metallurgical R and D Inst., Cairo (Egypt)

    2003-06-01

    El-Maghara coal was confirmed to contain a substantial amount of fossil resin intimately associated with its macerals. Macroscopic identification as well as physical diagnosis of solvent refined resinite material proved its particular significance and sufficient value to justify a fossil resin industry in Egypt. This resin has thermosetting properties superior to most synthetics resins available from petrochemicals. It could compete in the market as a chemical commodity in high-speed printing and high-performance adhesive applications. It could have also special values as a feedstock for high-density jet fuel after proper hydrogenation. The froth flotation technique was applied to recover this valuable material from El-Maghara ground coal. The solvent extraction method using commercial solvents was used to refine the resinite fraction collected as flotation concentrate. The variables affecting the flotation technique were studied. Characterization of refined resin was applied. (orig.)

  10. Recent advances in metal-organic frameworks and covalent organic frameworks for sample preparation and chromatographic analysis.

    Science.gov (United States)

    Wang, Xuan; Ye, Nengsheng

    2017-09-04

    In the field of analytical chemistry, sample preparation and chromatographic separation are two core procedures. The means by which to improve the sensitivity, selectivity and detection limit of a method have become a topic of great interest. Recently, porous organic frameworks, such as metal-organic frameworks (MOFs) and covalent organic frameworks (COFs), have been widely used in this research area because of their special features, and different methods have been developed. This review summarizes the applications of MOFs and COFs in sample preparation and chromatographic stationary phases. The MOF- or COF-based solid-phase extraction (SPE), solid-phase microextraction (SPME), gas chromatography (GC), high-performance liquid chromatography (HPLC) and capillary electrochromatography (CEC) methods are described. The excellent properties of MOFs and COFs have resulted in intense interest in exploring their performance and mechanisms for sample preparation and chromatographic separation. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  11. Preparation of Medium Cation Exchange Stationary Phase of Polymeric Matrix and Their Chromatographic Properties

    Institute of Scientific and Technical Information of China (English)

    CHEN,Gang; GONG,Bo-Lin; BAI,Quan; GENG,Xin-Du

    2007-01-01

    Based on the monodisperse poly(glycidyl methacrylate-co-ethylenedimethacrylate) beads (PGMA/EDMA) with macropore as a medium, a new hydrophilic medium cation exchange (MCX) stationary phase for HPLC was synthesized by a new chemically modified method. The stationary phase was evaluated with the property of ion exchange, separability, reproducibility, hydrophilicity, effect of salt concentration, salt types, column loading and pH on the separation and retention of proteins in detail. It was found that it follows ion exchange chromatographic (IEC)retention mechanism. The measured bioactivity recovery for lysozyme was (96±5)%. The dynamic protein loading capacity of the synthesized MCX packings was 21.8 mg/g. Five proteins were almost completely separated within 6.0 min at a flow rate of 4 mL/min using the synthesized MCX resin. The MCX resin was also used for the rapid separation and purification of lysozyme from egg white with only one step. The purity and specific bioactivity of the purified lysozyme was found more than 95% and 70345 U/mg, respectively.

  12. Contact allergy to epoxy resin

    DEFF Research Database (Denmark)

    Bangsgaard, Nannie; Thyssen, Jacob Pontoppidan; Menné, Torkil

    2012-01-01

    . Objectives. To evaluate the prevalence of contact allergy to epoxy resin monomer (diglycidyl ether of bisphenol A; MW 340) among patients with suspected contact dermatitis and relate this to occupation and work-related consequences. Patients/methods. The dataset comprised 20 808 consecutive dermatitis...... in an educational programme. Conclusion. The 1% prevalence of epoxy resin contact allergy is equivalent to reports from other countries. The high occurrence of epoxy resin exposure at work, and the limited use of protective measures, indicate that reinforcement of the law is required....

  13. Extraction of extracellular polymeric substances (EPS) from anaerobic granular sludges: comparison of chemical and physical extraction protocols

    NARCIS (Netherlands)

    Abzac, D' P.; Bordas, F.; Hullebusch, E.; Lens, P.N.L.; Guibaud, G.

    2010-01-01

    The characteristics of the extracellular polymeric substances (EPS) extracted with nine different extraction protocols from four different types of anaerobic granular sludge were studied. The efficiency of four physical (sonication, heating, cationic exchange resin (CER), and CER associated with son

  14. Extraction of extracellular polymeric substances (EPS) from anaerobic granular sludges: comparison of chemical and physical extraction protocols

    NARCIS (Netherlands)

    Abzac, D' P.; Bordas, F.; Hullebusch, E.; Lens, P.N.L.; Guibaud, G.

    2010-01-01

    The characteristics of the extracellular polymeric substances (EPS) extracted with nine different extraction protocols from four different types of anaerobic granular sludge were studied. The efficiency of four physical (sonication, heating, cationic exchange resin (CER), and CER associated with

  15. Chromatographic fingerprint analysis of yohimbe bark and related dietary supplements using UHPLC/UV/MS.

    Science.gov (United States)

    Sun, Jianghao; Chen, Pei

    2012-03-05

    A practical ultra high-performance liquid chromatography (UHPLC) method was developed for fingerprint analysis of and determination of yohimbine in yohimbe barks and related dietary supplements. Good separation was achieved using a Waters Acquity BEH C(18) column with gradient elution using 0.1% (v/v) aqueous ammonium hydroxide and 0.1% ammonium hydroxide in methanol as the mobile phases. The study is the first reported chromatographic method that separates corynanthine from yohimbine in yohimbe bark extract. The chromatographic fingerprint analysis was applied to the analysis of 18 yohimbe commercial dietary supplement samples. Quantitation of yohimbine, the traditional method for analysis of yohimbe barks, were also performed to evaluate the results of the fingerprint analysis. Wide variability was observed in fingerprints and yohimbine content among yohimbe dietary supplement samples. For most of the dietary supplements, the yohimbine content was not consistent with the label claims.

  16. Simultaneous liquid-chromatographic determination of urinary vanillylmandelic acid, homovanillic acid, and 5-hydroxyindoleacetic acid.

    Science.gov (United States)

    Gironi, A; Seghieri, G; Niccolai, M; Mammini, P

    1988-12-01

    We describe a liquid-chromatographic method for quantifying, simultaneously by a single procedure, vanillylmandelic acid (VMA), homovanillic acid (HVA), and 5-hydroxyindoleacetic acid (5-HIAA) in urine. After solvent extraction of acidified urine, the analytes were chromatographed on a C8 column, with use of a mobile phase of phosphate buffer (20 mmol/L, pH 4.0) and methanol with a variable gradient elution, and detected fluorometrically. We report the analytical recovery, sensitivity, precision, working linear range, and potential for interference from similar molecules or drugs. The results of such tests demonstrate that the proposed method is sensitive and reproducible. It is, furthermore, easy to perform, and thus is suitable for use in the clinical laboratory.

  17. EPOXY RESIN TOUGHENED BY THERMOPLASTICS

    Institute of Scientific and Technical Information of China (English)

    FU Zengli; SUN Yishi

    1989-01-01

    Two kinds of tough ductile heatresisting thermoplastic, namely bisphenol A polysulfone (PSF) and polyethersulfone (PES) were used to toughen thermoset epoxy resin. A systematic study on the relationship between the molecular weight and the terminal group of the thermoplastic modifier and the fracture toughness of the modified resin was carried out. The morphology of PSF modified epoxy resin was surveyed. With the same kind of PSF the structure of the epoxy resin and the toughening effect of PSF was also investigated. The fractography of PSF, particle modified epoxy was examined in detail with SEM. The contribution of every possible energy absorption process has been discussed. Crack pinning mechanism seems to be the most important toughening mechanism for tough ductile thermoplastic PSF particle modified epoxy system.

  18. Bending characteristics of resin concretes

    Directory of Open Access Journals (Sweden)

    Ribeiro Maria Cristina Santos

    2003-01-01

    Full Text Available In this research work the influence of composition and curing conditions in bending strength of polyester and epoxy concrete is analyzed. Various mixtures of resin and aggregates were considered in view of an optimal combination. The Taguchi methodology was applied in order to reduce the number of tests, and in order to evaluate the influence of various parameters in concrete properties. This methodology is very useful for the planning of experiments. Test results, analyzed by this methodology, shown that the most significant factors affecting bending strength properties of resin concretes are the type of resin, resin content and charge content. An optimal formulation leading to a maximum bending strength was achieved in terms of material parameters.

  19. Bulk-Fill Resin Composites

    DEFF Research Database (Denmark)

    Benetti, Ana Raquel; Havndrup-Pedersen, Cæcilie; Honoré, Daniel;

    2015-01-01

    the restorative procedure. The aim of this study, therefore, was to compare the depth of cure, polymerization contraction, and gap formation in bulk-fill resin composites with those of a conventional resin composite. To achieve this, the depth of cure was assessed in accordance with the International Organization...... for Standardization 4049 standard, and the polymerization contraction was determined using the bonded-disc method. The gap formation was measured at the dentin margin of Class II cavities. Five bulk-fill resin composites were investigated: two high-viscosity (Tetric EvoCeram Bulk Fill, SonicFill) and three low......-viscosity (x-tra base, Venus Bulk Fill, SDR) materials. Compared with the conventional resin composite, the high-viscosity bulk-fill materials exhibited only a small increase (but significant for Tetric EvoCeram Bulk Fill) in depth of cure and polymerization contraction, whereas the low-viscosity bulk...

  20. Epoxy hydantoins as matrix resins

    Science.gov (United States)

    Weiss, J.

    1983-01-01

    Tensile strength and fracture toughness of castings of the hydantoin resins cured with methylenedianiline are significantly higher than MY 720 control castings. Water absorption of an ethyl, amyl hydantoin formulation is 2.1 percent at equilibrium and Tg's are about 160 C, approximately 15 deg below the final cure temperature. Two series of urethane and ester-extended hydantoin epoxy resins were synthesized to determine the effect of crosslink density and functional groups on properties. Castings cured with methylenedianiline or with hexahydrophthalic anhydride were made from these compounds and evaluated. The glass transition temperatures, tensile strengths and moduli, and fracture toughness values were all much lower than that of the simple hydantoin epoxy resins. Using a methylene bishydantoin epoxy with a more rigid structure gave brittle, low-energy fractures, while a more flexible, ethoxy-extended hydantoin epoxy resin gave a very low Tg.

  1. Karakteristik Komposit Resin Berkemampuan Mengalir

    Directory of Open Access Journals (Sweden)

    Bambang Irawan

    2015-10-01

    Full Text Available The use of resin composites as posterior restoratives has markedly increased over the past decade. The patients demand for better esthetics, concerns related to possible mercury toxicity from amalgam and improvements in resin composite materials have significantly contributed the popularity of these materials. Early problems related to composites included excessive wear, less of anatomic form, post operative sensitivity, secondary caries and marginal leakage. Marginal adaptation still remains an unavoidable problem for composite restoration, especially at the gingival wall of cervical or Class II restoration. In an attempt to improve marginal sealing, many techniques and lining materials have been designed. To reduce stress generated by polymerization shrinkage, applying and curing of resin composites in layers is often recommended. Using a thick adhesive layer or low-viscosity resin may, due to its elastic properties, serve as a flexible intermediate layer and compensate for the polymerization stress created in resin composite. Flowable composites were created by retaining the same small particle size of traditional hybrid composite but reducing the filler content and allowing the increased resin to reduce the viscosity of the mixture. Flowable composites were introduced in 1996 as liners, fissure sealants and also in tunnel preparations. They have been suggested for Class I, II, III and V cavity restorations, preventive resin restorations and composite, porcelain and amalgam repairing. Their usage as a liner under high filled resins in posterior restorations has been shown to improve the adaptation of composites and effectively achieve clinically acceptable results. This article attempts to give a broad characteristics of different types of flowable composites. 

  2. Karakteristik Komposit Resin Berkemampuan Mengalir

    OpenAIRE

    Bambang Irawan

    2015-01-01

    The use of resin composites as posterior restoratives has markedly increased over the past decade. The patients demand for better esthetics, concerns related to possible mercury toxicity from amalgam and improvements in resin composite materials have significantly contributed the popularity of these materials. Early problems related to composites included excessive wear, less of anatomic form, post operative sensitivity, secondary caries and marginal leakage. Marginal adaptation still remains...

  3. New Low Cost Resin Systems

    Science.gov (United States)

    2006-05-31

    DGEBA ). 30 % of the epoxy groups of RDGE were reacted with the dihydroxyl acid and resulted 3.2 wt% phosphorous and a new epoxide equivalent weight...of 207. Adducts were also made with DGEBA and the dihydroxyl phosphorous based acid but resulted in a substantial increased viscosity and therefore...70 wt% with a standard DGEBA resin, this material accelerated the epoxy reaction too much to make a VaRTM processable resin. Due to the processing

  4. Probabilistic peak detection for first-order chromatographic data

    NARCIS (Netherlands)

    Lopatka, M.; Vivó-Truyols, G.; Sjerps, M.J.

    2014-01-01

    We present a novel algorithm for probabilistic peak detection in first-order chromatographic data. Unlike conventional methods that deliver a binary answer pertaining to the expected presence or absence of a chromatographic peak, our method calculates the probability of a point being affected by suc

  5. Separation and Purification of Two Flavone Glucuronides from Erigeron multiradiatus (Lindl. Benth with Macroporous Resins

    Directory of Open Access Journals (Sweden)

    Zhi-feng Zhang

    2009-01-01

    Full Text Available Scutellarein-7-O-β-D-glucuronide (SG and apigenin-7-O-β-D-glucuronide (AG are two major bioactive constituents with known pharmacological effects in Erigeron multiradiatus. In this study, a simple method for preparative separation of the two flavone glucuronides was established with macroporous resins. The performance and adsorption characteristics of eight macroporous resins including AB-8, HPD100, HPD450, HPD600, D100, D101, D141, and D160 have been evaluated. The results confirmed that D141 resin offered the best adsorption and desorption capacities and the highest desorption ratio for the two glucuronides among the tested resins. Sorption isotherms were constructed for D141 resin under optimal ethanol conditions and fitted well to the Freundlich and Langmuir models (R2>0.95. Dynamic adsorption and desorption tests was performed on column packed with D141 resin. After one-run treatment with D141 resin, the two-constituent content in the final product was increased from 2.14% and 1.34 % in the crude extract of Erigeron multiradiatus to 24.63% and 18.42% in the final products with the recoveries of 82.5% and 85.4%, respectively. The preparative separation of SG and AG can be easily and effectively achieved via adsorption and desorption on D141 resin, and the method developed can be referenced for large-scale separation and purification of flavone glucuronides from herbal raw materials.

  6. Fully automated high-performance liquid chromatographic assay for the analysis of free catecholamines in urine.

    Science.gov (United States)

    Said, R; Robinet, D; Barbier, C; Sartre, J; Huguet, C

    1990-08-24

    A totally automated and reliable high-performance liquid chromatographic method is described for the routine determination of free catecholamines (norepinephrine, epinephrine and dopamine) in urine. The catecholamines were isolated from urine samples using small alumina columns. A standard automated method for pH adjustment of urine before the extraction step has been developed. The extraction was performed on an ASPEC (Automatic Sample Preparation with Extraction Columns, Gilson). The eluate was collected in a separate tube and then automatically injected into the chromatographic column. The catecholamines were separated by reversed-phase ion-pair liquid chromatography and quantified by fluorescence detection. No manual intervention was required during the extraction and separation procedure. One sample may be run every 15 min, ca. 96 samples in 24 h. Analytical recoveries for all three catecholamines are 63-87%, and the detection limits are 0.01, 0.01, and 0.03 microM for norepinephrine, epinephrine and dopamine, respectively, which is highly satisfactory for urine. Day-to-day coefficients of variation were less than 10%.

  7. Effect of proanthocyanidin incorporation into dental adhesive resin on resin-dentine bond strength.

    Science.gov (United States)

    Epasinghe, D J; Yiu, C K Y; Burrow, M F; Tay, F R; King, N M

    2012-03-01

    This study evaluated the effect of proanthocyanidin (PA) incorporation into experimental dental adhesives on resin-dentine bond strength. Four experimental hydrophilic adhesives containing different PA concentrations were prepared by combining 50wt% resin comonomer mixtures with 50wt% ethanol. Proanthocyanidin was added to the ethanol-solvated resin to yield three adhesives with PA concentrations of 1.0, 2.0 and 3.0wt%, respectively. A PA-free adhesive served as the control. Flat dentine surfaces from 40 extracted third molars were etched with 32% phosphoric acid. The specimens were randomly assigned to one of the four adhesive groups. Two layers of one of the four experimental adhesives were applied to the etched dentine and light-cured for 20s. Composite build-ups were performed using Filtek Z250 (3M ESPE). After storage in distilled water at 37°C for 24h, twenty-four bonded teeth were sectioned into 0.9 mm×0.9 mm beams and stressed to failure under tension for bond strength testing. Bond strength data were evaluated by one-way ANOVA and Tukey's test (α=0.05). Interfacial nanoleakage was examined in the remaining teeth using a field-emission scanning electron microscope and analysed using the Chi-square test (α=0.05). No significant difference in bond strength was found amongst PA-free, 1% and 2% PA adhesives. However, incorporation of 3% PA into the adhesive significantly lowered bond strength as demonstrated by a greater number of adhesive failures and more extensive nanoleakage along the bonded interface. Incorporation of 2% proanthocyanidin into dental adhesives has no adverse effect on dentine bond strength. The addition of proanthocyanidin to an experimental adhesive has no adverse effect on the immediate resin-dentine bond strength when the concentration of proanthocyanidin in the adhesive is less than or equal to 2%. Copyright © 2012 Elsevier Ltd. All rights reserved.

  8. Simple gas chromatographic method for furfural analysis.

    Science.gov (United States)

    Gaspar, Elvira M S M; Lopes, João F

    2009-04-03

    A new, simple, gas chromatographic method was developed for the direct analysis of 5-hydroxymethylfurfural (5-HMF), 2-furfural (2-F) and 5-methylfurfural (5-MF) in liquid and water soluble foods, using direct immersion SPME coupled to GC-FID and/or GC-TOF-MS. The fiber (DVB/CAR/PDMS) conditions were optimized: pH effect, temperature, adsorption and desorption times. The method is simple and accurate (RSDTOF-MS: 0.3, 1.2 and 0.9 ngmL(-1) for 2-F, 5-MF and 5-HMF, respectively). It was applied to different commercial food matrices: honey, white, demerara, brown and yellow table sugars, and white and red balsamic vinegars. This one-step, sensitive and direct method for the analysis of furfurals will contribute to characterise and quantify their presence in the human diet.

  9. Functional Polymers for Chromatographic Enantiomer Separation

    Institute of Scientific and Technical Information of China (English)

    S. Allenmark; L. Thunberg

    2005-01-01

    @@ 1Introduction Today, methods to obtain pure enantiomers of organic compounds are of extreme importance, not the least due to the demands imposed on the pharmaceutical industry. Separation of the two enantiomers in a racemate is necessary in order to study possible differences in biological activity. Consequently, research on methods for direct chromatographic resolution by means of columns containing a chiral stationary phase (CSP) has been intense during the last decades and a wide variety of CSPs,many of which commercially available,exist today.Polymeric CSPs have been made from naturally occurring polymers (cellulose, amylose) via suitable derivatization, as well as either by polymerization of chiral monomers or via asymmetric catalysis to yield linear, isotactic polymers of a predominantly single-handed helicity. An excellent review of the field[1], with special emphasis on preparative applications, was published in 1994.

  10. Headspace chromatographic determination of water pollutants

    Energy Technology Data Exchange (ETDEWEB)

    Otson, R.; Williams, D.T.

    1982-05-01

    A readily constructed, automated purging assembly, on-column trapping, and simultaneous use of flame ionization and electrolytic conductivity detectors were applied to develop a dynamic headspace gas chromatographic technique which was evaluated for the determination of 42 organic polluants in water. Detection limits of <1 ..mu..g/L and linear plots of peak area against concentration in the range 0.25-16 ..mu..g/L were obtained for 32 compounds. At aqueous concentrations of 4 and 16 ..mu..g/L, peak area precision of <10% relative standard deviation (RSD) for triplicate sample analysis and purging efficiencies of >75% were generally obtained. Storage of aqueous composite standard solutions at 4 and 16 ..mu..g/L for 6 weeks at 4/sup 0/C did not usually affect analytical results by more than +/- 15%.

  11. Treatment of a Vertical Root Fracture Using Dual-Curing Resin Cement: A Case Report

    Directory of Open Access Journals (Sweden)

    Nima Moradi Majd

    2012-01-01

    Full Text Available Introduction. Vertical root fracture (VRF is one of the most frustrating complications of root canal treatment. The prognosis of the root with VRF is poor therefore tooth extraction and root amputation are usually the only treatment options. However, bonding of the fracture line with adhesive resin cement during the intentional replantation procedure was recently suggested as an alternative to tooth extraction. Methods. A vertically fractured left maxillary incisor was carefully extracted, fracture line was treated with adhesive resin cement, a retrograde cavity was produced and filled with calcium-enriched mixture (CEM cement, and tooth was replanted. Results. After 12 months the tooth was asymptomatic. The size of periapical radiolucency was noticeably reduced and there was no clinical sign of ankylosis. Conclusion. Using adhesive resin cement to bond the fracture lines extraorally in roots with VRF and intentional replantation of the reconstructed teeth could be considered as an alternative to tooth extraction, especially for anterior teeth.

  12. Gas Chromatography Analysis of Resin and Fatty Acids from Laboratory Generated Bleach Plant Effluents

    Institute of Scientific and Technical Information of China (English)

    Chhaya Sharma; S. Mohanty; S. Kumar; N.J. Rao

    2007-01-01

    Laboratory generated spent bleached liquor from the chlorination, caustic extraction stage of mixed wood kraft pulp processing has been analyzed both qualitatively and quantitatively for various resin & fatty acids by using GC. A number of resin acids,saturated and unsaturated fatty acids, chloro fatty and resin acid have been detected and their concentrations are estimated. The results are compared with results on different agriculture residue/hardwood pulps, which were reported earlier. The concentrations of various compounds detected have also been compared with their reported LC50 values.

  13. PURIFICATION OF FLAVONES OF GINKGO LEAVES BY ADSORPTION HZ-841 RESIN

    Institute of Scientific and Technical Information of China (English)

    ZENG Hui; ZHOU Xiaohua; LI Duanhua

    2004-01-01

    The purification process of total flavones of ginkgo leaves by resin HZ-841 from ethanol extract was studied. First, the total flavone was extracted from the defatted powder of ginkgo L. biloba leaves. Effects of solvents and operation conditions were examined to get a relative high yield and purity in this step. The crude extract was further purified by resin HZ-841. Both adsorption and elution process were studied to obtain an optimized conditions, i.e., pH, flow rate, concentration. A yellow powder was obtained, of which 37.3% was flavones, obviously higher than the basic international standard of 24%.

  14. Elution study of unreacted Bis-GMA, TEGDMA, UDMA, and Bis-EMA from light-cured dental resins and resin composites using HPLC.

    Science.gov (United States)

    Sideridou, Irini D; Achilias, Dimitris S

    2005-07-01

    In the present work the elution of residual monomers from light-cured dental resins and resin composites into a 75% ethanol:water solution was studied using High-Performance Liquid Chromatography (HPLC). The resins studied were made by light-curing of bisphenol A glycol dimethacrylate (Bis-GMA), triethylene glycol dimethacrylate (TEGDMA), urethane dimethacrylate (UDMA), ethoxylated bisphenol A glycol dimethacrylate [Bis-EMA(4)] and mixtures of these monomers. The resin composites were made from two commercial light-cured restorative materials (Z100 MP and Filtek Z250), the resin matrix of which is based on copolymers of these monomers. The effect of the curing time on the amount of monomers eluted was investigated. The concentration of the extractable monomers was determined at several immersion periods from 3 h to 30 days. For all the materials studied, it was observed that the chemical structure of the monomers used for the preparation of the resins, which defines the chemical and physical structure of the corresponding resin, directly affects the amount of eluted monomers, as well as the time needed for the elution of this amount. In the case of composites, it seems that the elution process it is not influenced by the presence of filler. Copyright 2005 Wiley Periodicals, Inc.

  15. 酸石榴汁红色素的树脂吸附及石榴提取物的抗氧化作用研究%Study on Absorption of Red Pigment from Pomegranate Juice with Resin and Antioxidant Activity of Pomegranate Extracts

    Institute of Scientific and Technical Information of China (English)

    朱洁; 陈旭红; 李美瑛; 丁瑞

    2011-01-01

    This article studied the absorption of red pigment from pomegranate juice with resins and antioxidant activity of pomegranate extracts. The results showed that HPD-300 was the best resin for absorption of red pigment of pomegranate juice.Compared with Vc, the DPPH · scavenging ability of the red pigment of pomegranate juice was 91. 48 % at the concentration of 2 mg/mL. The results showed that the red pigment of pomegranate juice has better antioxidant activity.%研究了7种吸附树脂对酸石榴汁红色素的吸附,及酸石榴各部分提取物对DPPH(1,1-Diphenyl-2-picrylhydrazyl;1,1-二苯基-2-苦基肼自由基)的清除作用,并且将提取出的酸石榴汁红色素添加到化妆品配方中,探讨了该配方对于延缓衰老的功效.实验结果表明:HPD-300对酸石榴汁红色素的吸附效果最好;2.0 mg/mL的酸石榴汁红色素对DPPH的清除率达91,48%,表明酸石榴汁红色素具有良好的抗氧化活性,为其在化妆品行业的应用提供依据.

  16. Repeated use of ion-exchange resin membranes in calcareous soils

    Science.gov (United States)

    Sherrod, S.K.; Belnap, J.; Miller, M.E.

    2003-01-01

    This study compared the consistency of nutrient extraction among repeated cycles of ion-exchange resin membrane use. Two sandy calcareous soils and different equilibration temperatures were tested. No single nutrient retained consistent values from cycle to cycle in all treatments, although both soil source and temperature conferred some influence. It was concluded that the most conservative use of resin membranes is single-use.

  17. Adsorption of Chromium(VI) from Aqueous Solutions by Coffee Polyphenol-Formaldehyde/Acetaldehyde Resins

    OpenAIRE

    2013-01-01

    Removal of chromium(VI) from wastewater is essential as it is toxic. Thus, removal of chromium(VI) was performed using coffee polyphenol-formaldehyde/acetaldehyde resins as adsorbents. Adsorbent resins were prepared by condensation of decaffeinated coffee powder with formaldehyde/acetaldehyde and used for the removal of Cr(VI) ions from aqueous solutions. A simple and sensitive solid phase extraction procedure was applied for the determination of chromium at trace levels by spectroscopic meth...

  18. Separation of Immunoglobulin in Conjunction with High Performance Liquid Chromatography Using Poly(vinyl ester resin) Monolith

    Institute of Scientific and Technical Information of China (English)

    YANG,Guanqun; YANG,Gengliang; LIU,Haiyan; BAI,Ligai; FENG,Xiaojuan; YANG,Xinru

    2009-01-01

    Using vinyl ester resin both as the monomer and the crosslinker,2,2-azobis(2-methylpropionitrile) (AIBN) as initiator,poly(vinyl ester resin) monolithic column was prepared to separate the immunoglobulin G (lgG) and yolk of eggs (lgY) from human plasma and egg yolk by HPLC respectively.The influence of concentration and pH of mobile phase on the chromatographic performance was investigated.Scanning electron microcopy showed that the poly(vinyl ester resin) monolithic stationary phase had a through-pore structure.Dynamic capacity of IgG on the polymeric monolithic column was investigated.The monolithic column had good flow-through properties and high resolution.The maximum adsorptive amount of IgG was 144 μg·g-1.

  19. Liquid chromatographic determination of sennosides in Cassia angustifolia leaves.

    Science.gov (United States)

    Srivastava, Alpuna; Pandey, Richa; Verma, Ram K; Gupta, Madan M

    2006-01-01

    A simple liquid chromatographic method was developed for the determination of sennosides B and A in leaves of Cassia angustifolia. These compounds were extracted from leaves with a mixture of methanol-water (70 + 30, v/v) after defatting with hexane. Analyte separation and quantitation were achieved by gradient reversed-phase liquid chromatography and UV absorbance at 270 nm using a photodiode array detector. The method involves the use of an RP-18 Lichrocart reversed-phase column (5 microm, 125 x 4.0 mm id) and a binary gradient mobile-phase profile. The various other aspects of analysis, namely, peak purity, similarity, recovery, repeatability, and robustness, were validated. Average recoveries of 98.5 and 98.6%, with a coefficient of variation of 0.8 and 0.3%, were obtained by spiking sample solution with 3 different concentration solutions of standards (60, 100, and 200 microg/mL). Detection limits were 10 microg/mL for sennoside B and 35 microg/mL for sennoside A, present in the sample solution. The quantitation limits were 28 and 100 microg/mL. The analytical method was applied to a large number of senna leaf samples. The new method provides a reliable tool for rapid screening of C. angustifolia samples in large numbers, which is needed in breeding/genetic engineering and genetic mapping experiments.

  20. Recovery of lactic acid from the pretreated fermentation broth based on a novel hyper-cross-linked meso-micropore resin: Modeling.

    Science.gov (United States)

    Song, Mingkai; Jiao, Pengfei; Qin, Taotao; Jiang, Kangkang; Zhou, Jingwei; Zhuang, Wei; Chen, Yong; Liu, Dong; Zhu, Chenjie; Chen, Xiaochun; Ying, Hanjie; Wu, Jinglan

    2017-10-01

    An innovative benign process for recovery lactic acid from its fermentation broth is proposed using a novel hyper-cross-linked meso-micropore resin and water as eluent. This work focuses on modeling the competitive adsorption behaviors of glucose, lactic acid and acetic acid ternary mixture and explosion of the adsorption mechanism. The characterization results showed the resin had a large BET surface area and specific pore structure with hydrophobic properties. By analysis of the physicochemical properties of the solutes and the resin, the mechanism of the separation is proposed as hydrophobic effect and size-exclusion. Subsequently three chromatographic models were applied to predict the competitive breakthrough curves of the ternary mixture under different operating conditions. The pore diffusion was the major limiting factor for the adsorption process, which was consistent with the BET results. The novel HD-06 resin can be a good potential adsorbent for the future SMB continuous separation process. Copyright © 2017 Elsevier Ltd. All rights reserved.

  1. Investigations into the chromatographic optimization of combined gas chromatographic/FTIR/MS

    Science.gov (United States)

    Wulff, Ditmar

    1989-12-01

    Even with the explosive growth and acceptance of GC/MS it has some analytical limitations. Several of these deficiencies can be overcome with information provided by GC/FTIR. Combining a GC/MS and a GC/FTIR into one system provides economies of sample, time, space, and money as well as a higher confidence qualitative result. The later results from the ability of the mass spectro -meter to give molecular fragment information with strength in homolog identification while the infrared spectrometer gives class specific-functional group and geometrical isomer data. Several configurations of the combined light pipe GC/FTIR/MS are evaluated looking toward ease of use, information content, and data evaluation. The combined system's sensitivity, chromatographic integrity, and gas chromatographic column choices and their operational parameters are discussed. The series arrangement with the GC column effluent passing through the FTIR light pipe and then serially to the MS is compared to the post column split of the column effluent to the FTIR and MS as well as to the configuration using two GC columns. Operational recommendations are given to maximize chromatographic resolution, detector sensitivity, and sample throughput. Examples are shown illustrating the combined systems operation. All parameters discussed apply to work done on the HP 5890A GC, the HP5965A IRD, and the HP 5970B MSD.

  2. Antimicrobial and Antioxidant Activities of Resins and Essential Oil From Pine (Pinus merkusii, Pinuso ocarpa, Pinus insularis and Agathis (Agathis loranthifolia

    Directory of Open Access Journals (Sweden)

    Mardho Tillah

    2017-04-01

    Full Text Available The most common human pathogen that colonizes in a third of healthy people around the world are Staphylococcus aureus, and one of the materials allegedly able to overcome the pathogen is resin. Resin has been used in folk medicine for thousands of years to treat diseases. The antimicrobial activity of natural resins can be associated with a variety of organic compounds contained in them such as diterpenoids and triterpenoids. This research aimed to explore the antibacterial and antioxidant activities of Pinus merkusii, P. oocarpa, P. insularis, Agathis loranthifolia resins and essential oil. Resin was separated by distillation process to get essential oil and the residue was extracted using n-hexane, ethyl acetate (EtOAc, and methanol (MeOH. Antioxidant activity was performed by DPPH (1,1diphenyl-2-picryl hydrazyl radical scavenging method. The antibacterial activity of resins and essential oil of the samples determined using the disc diffusion method against Staphylococcus aureus and Escherichia coli. The results showed that the yield of resin extract was ranging from 8.44 % to 95.56%. All extracts and essential oil could not inhibit E coli growth but inhibit the S. aureus growth. This experiment concluded that resin n-hexane extract from P.oocarpa was the most potent as antibacterial activity against S. aureus. All of the samples used had less potential antioxidant activity compared to positive control ascorbic acid. Result of this study show that pine resin from Indonesia has potential as an antibacterial agent. 

  3. Determination of trace organic impurities in water using thermal desorption from XAD resin

    Energy Technology Data Exchange (ETDEWEB)

    Ryan, J.P.; Fritz, J.S.

    1978-10-01

    A small water sample (20 to 250 ml) is passed through a small tube containing XAD-4 resin; this effectively retains the organic impurities present in the water. This tube is connected to the permanent apparatus and the sorbed organics are thermally transferred to a small Tenex pre-column while the water vapor is vented. The pre-column is closed off, preheated to 275 to 280/sup 0/C, and then a valve is opened to plug-inject the vaporized sample into a gas chromatograph. The procedure works well for a variety of model organic compounds added to water and can be used for the analysis of actual water samples.

  4. Band target entropy minimization for retrieving the information of individual components from overlapping chromatographic data.

    Science.gov (United States)

    Xia, Zhenzhen; Liu, Yan; Cai, Wensheng; Shao, Xueguang

    2015-09-11

    Band target entropy minimization (BTEM) is a self-modeling curve resolution (SMCR) approach relying on non-negative criterion and minimization of Shannon entropy. In this study, BTEM algorithm was applied to retrieving the information of individual components from overlapping gas chromatography-mass spectrometry (GC-MS) data. The algorithm starts with dividing the whole data into bands along the retention time. In each band, singular value decomposition (SVD) is used to decompose the data into scores and loadings. Because the pure chromatographic signal possesses the lowest Shannon entropy, the chromatographic signal of each component can be constructed by optimizing the combination of the loadings with minimal Shannon entropy under non-negative criterion. To show the efficiency of the algorithm, a simulated four-component overlapping GC-MS data and an experimental GC-MS data of 18 organophosphorus pesticide mixture are investigated. The results show that both the chromatographic profiles and mass spectra of the components can be successfully extracted from the overlapping signals. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Simultaneous liquid chromatographic determination of thiamine and riboflavin in selected foods.

    Science.gov (United States)

    Sims, A; Shoemaker, D

    1993-01-01

    A reliable, improved liquid chromatographic (LC) method has been developed for the measurement of thiamine and riboflavin in foods. The major improvement in the method is the chromatographic separation achieved. The method is also very reproducible and extremely sensitive. After autoclave extraction, samples are derivatized to form thiochrome (a highly fluorescent oxidation product of thiamine). Riboflavin is naturally fluorescent. Interferences are removed on a C18 cartridge and chromatographed by using a reversed-phase separation. The mobile phase used is 72% 0.005M NH4OAc (pH 5.0)-28% MeOH. Fluorescence detection using wavelength switching, 370-435 for thiamine and 370-520 for riboflavin, allows determination of each vitamin at its optimum wavelength for maximum sensitivity. Detection limits were 0.05 ng for both thiamine and riboflavin. The method can also be performed by using a fluorescence detector at a single wavelength, but with a sacrifice of sensitivity. Data comparisons between AOAC fluorometric and LC results were excellent for routine samples, as well as for American Association of Cereal Chemists (AACC) check samples. All LC results from AACC samples were within 2 standard deviations of the mean. Reproducibility was 1.9% for thiamine and 1.6% for riboflavin.

  6. Liquid chromatographic determination of benzocaine and N-acetylbenzocaine in the edible fillet tissue from rainbow trout

    Science.gov (United States)

    Meinertz, J.R.; Stehly, G.R.; Hubert, T.D.; Bernardy, J.A.

    1999-01-01

    A method was developed for determining benzocaine and N-acetylbenzocaine concentrations in fillet tissue of rainbow trout. The method involves extracting the analytes with acetonitrile, removing lipids or hydrophobic compounds from the extract with hexane, and providing additional clean-up with solid-phase extraction techniques. Analyte concentrations are determined using reversed-phase high-performance liquid chromatographic techniques with an isocratic mobile phase and UV detection. The accuracy (range, 92 to 121%), precision (R.S.D., benzocaine residues from fish exposed to benzocaine. Copyright (C) 1999.

  7. Gas chromatographic determination of xanthinol in plasma

    NARCIS (Netherlands)

    Roseboom, H.; Wiese, G.

    1979-01-01

    The determination of xanthinol in plasma is described. After extraction of the drug, together with the internal standard (papaverine hydrochloride), the extract is evaporated to dryness and the drug is derivatized with acetic anhydride for chromatography. The method is linear for 2–100μg ml-1 ; the

  8. Chromatographic analysis of olopatadine in hydrophilic interaction liquid chromatography.

    Science.gov (United States)

    Maksić, Jelena; Jovanović, Marko; Rakić, Tijana; Popović, Igor; Ivanović, Darko; Jančić-Stojanović, Biljana

    2015-01-01

    In this paper, chromatographic analysis of active substance olopatadine hydrochloride, which is used in eye drops as antihistaminic agent, and its impurity E isomer by hydrophilic interaction liquid chromatography (HILIC) and application of design of experiments (DoE) methodology are presented. In addition, benzalkonium chloride is very often used as a preservative in eye drops. Therefore, the evaluation of its chromatographic behavior in HILIC was carried out as well. In order to estimate chromatographic behavior and set optimal chromatographic conditions, DoE methodology was applied. After the selection of important chromatographic factors, Box-Behnken design was utilized, and on the basis of the obtained models factor effects were examined. Then, multi-objective robust optimization is performed aiming to obtain chromatographic conditions that comply with several quality criteria simultaneously: adequate and robust separation of critical peak pair and maximum retention of the first eluting peak. The optimal conditions are identified by using grid point search methodology. The experimental verification confirmed the adequacy of the defined optimal conditions. Finally, under optimal chromatographic conditions, the method was validated and applicability of the proposed method was confirmed.

  9. Investigation of Adsorption Behavior of Ba and Other Fission Products on the Sr·spc Chromatographic Column by Static Method

    Institute of Scientific and Technical Information of China (English)

    YANG; Lei; MA; Peng; YANG; Su-liang; LIANG; Xiao-hu

    2012-01-01

    <正>Adsorption behavior of Ba, Cs and some other fission products on the Sr·spc resin has been investigated for the purpose of extracting 141Ba from the fission product. Sr·spc resin with the main functional group of 18-crown-6 ether was purchased from US. Eichrom Company. Tracers of Ba, Cs and some other fission products were acquired from an irradiated U target.

  10. Selective flotation of fossil resin from Western coal. Final report, July 1, 1990--May 25, 1992

    Energy Technology Data Exchange (ETDEWEB)

    Jensen, G.F.; Miller, J.D.

    1992-05-25

    The proof-of-concept test program was designed to clarify a number of concerns that have been raised by coal companies who own the valuable resin resource. First, from laboratory bench-scale flotation experiments, a froth product from cleaner flotation containing more than 80% hexane-extractable resin at higher than 80% recovery can be produced. Pilot-plant testing was initiated to demonstrate the selective flotation of fossil resin and to establish a better confidence level in the new technology. Second, pilot-plant testing was designed to evaluate the effect and impact of random variation in slurry solids concentration and feed grade on this new selective fossil resin flotation technology. The flotation performance obtained under these industrial conditions is more realistic for process evaluation. Third, more accurate operating cost data was to be obtained for economic analysis. Fourth, sufficient quantities of the fossil resin concentrate were to be produced from the test program for evaluation by potential industrial users. Fifth, and finally, optimum levels for the operating variables were to be established. Such information was required for eventual scale-up and design of a fossil resin flotation plant. The pilot-plant proof-of-concept testing of selective resinate flotation has demonstrated that: (1) technically, the new flotation technologies discovered at the University of Utah and then improved upon by Advanced Processing Technologies, Inc. provide a highly efficient means to selectively recover fossil resin from coal. The proof-of-concept continuous flotation circuit (about 0.1 tph) resulted in fossil resin recovery with the same separation efficiency as was obtained from laboratory bench-scale testing (more than 80% recovery at about 80% concentrate grade); and (2) economically, the selective flotation process has been shown to be sufficiently profitable to justify the development of a fossil resin industry based on this new flotation process.

  11. Chromatographic Separations of Enantiomers and Underivatized Oligosaccharides

    Energy Technology Data Exchange (ETDEWEB)

    Ying Liu

    2004-12-19

    My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic

  12. Chromatographic Separations of Enantiomers and Underivatized Oligosaccharides

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Ying [Iowa State Univ., Ames, IA (United States)

    2004-01-01

    My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic

  13. Fourier Transform Near-infrared Spectroscopy of PE Resin used in Analysis of N-hexane Extract%傅里叶变换近红外光谱法应用于聚乙烯树脂的正己烷提取物分析

    Institute of Scientific and Technical Information of China (English)

    王豪; 张樱; 陈平; 邬蓓蕾; 林振兴

    2012-01-01

    采用偏最小二乘法(PLS),建立了傅里叶变换近红外漫反射光谱法检测聚乙烯树脂正己烷提取物的数学模型.分析过程选择了最佳光谱预处理方法、谱区范围及主因子数,并使用内部交叉验证对模型进行验证.实验结果表明,当选择最小-最大归一化的光谱预处理方法,谱区范围7 501.8 ~6 097.9 cm-1和5 025.6 ~4 597.5 cm-1,主因子数8时定量模型的准确度最好,决定系数(R2)和均方差(RMSECV)分别为0.988和0.416,近红外测定值与标准方法测定值基本一致.对297种牌号共1 251个进口聚乙烯树脂正己烷提取物项目的普查结果表明,聚乙烯树脂正己烷提取物项目的总体安全性较低,属于进口聚乙烯需重点关注的安全卫生项目.%Using partial least squares (PLS) regression to establish mathematical model of n-hexane extract in polyethylene resin by Fourier transform near-infrared spectroscopy. The best spectral pretreatment method, spectral area and main factor number were chose and used internal cross-validation to verify the model in the analysis process. It was found that the result determined by near-infrared spectroscopy coincided with that decided by standard method, when the spectrum pretreatment method was minimum-maximum normalized, spectral range were 7 501. 8 cm-1 ~6 097. 9 cm-1 and 5 025. 6 cm-1~4 597. 5 cm-1, and the main factor number was eight. The correlation coefficients (R2 ) and root-mean-square error of cross-validation were 0. 988 and 0. 416 respectively. The survey to n-hexane extract in 1 251 imports polyethylene resin of 297 kinds of grades showed that the item was lower than the overall security, and which should be focused on.

  14. Evaluation of coverage, retention patterns, and selectivity of seven liquid chromatographic methods for metabolomics.

    Science.gov (United States)

    Wernisch, Stefanie; Pennathur, Subramaniam

    2016-09-01

    Liquid chromatography-mass spectrometry-based metabolomics studies require highly selective and efficient chromatographic techniques. Typically employed reversed-phase (RP) methods fail to target polar metabolites, but the introduction of hydrophilic interaction liquid chromatography (HILIC) is slow due to perceived issues of reproducibility and ruggedness and a limited understanding of the complex retention mechanisms. In this study, we present a comparison of the chromatographic performance of a traditional RP-C18 column with zwitterionic, amide-, alkyl diol-, and aminoalkyl-based HILIC and mixed-mode columns. Our metabolite library represents one of the largest analyte sets available and consists of 764 authentic metabolite standards, including amino acids, nucleotides, sugars, and other metabolites, representing all major biological pathways and commonly observed exogenous metabolites (drugs). The coverage, retention patterns, and selectivity of the individual methods are highly diverse even between conceptually related HILIC methods. Furthermore, we show that HILIC sorbents having highly orthogonal selectivity and specificity enhance the coverage of major metabolite groups in (semi-) targeted applications compared to RP. Finally, we discuss issues encountered in the analysis of biological samples based on the results obtained with human plasma extracts. Our results demonstrate that fast and highly reproducible separations on zwitterionic columns are feasible, but knowledge of analyte properties is essential to avoid chromatographic bias and exclusion of key analytes in metabolomics studies. Graphical Abstract The chromatographic parameters of 764 authentic metabolite standards provide the basis for a comparison of coverage, selectivity and orthogonality of 7 reversed-phase (RP), mixed-mode (MM) and hydrophilic interaction liquid chromatography (HILIC) methods.

  15. Recent trends in the use of organized molecular systems combined with chromatographic techniques in environmental analysis

    Energy Technology Data Exchange (ETDEWEB)

    Santana Rodriguez, Jose J.; Sosa Ferrera, Zoraida; Vega Moreno, Daura; Torres Padron, M.E.; Mahugo Santana, Cristina [University of Las Palmas de Gran Canaria, Department of Chemistry, Faculty of Marine Sciences, Las Palmas de Gran Canaria (Spain)

    2008-06-15

    The establishment of new analytical methods which improve quality and sensitivity in the determination of environmental pollutants in liquid and solid samples is demanded. The use of micellar systems have become an advantageous tool for the extraction of pollutant compounds, due to their easy handling, biodegradability, and the one-step procedure, and they are compatible with the hydroalcoholic mobile phases used in HPLC. The focus of this review is to present recently developed methods and the main trends in the use of micellar media combined with solid-phase microextraction and solid-phase extraction in the chromatographic analysis of organic compounds in different types of environmental matrix, including water, sediments, and biological samples. Selected samples illustrate the benefits of these systems in the whole of analytical process. The advantages of micellar media over conventional extractants are reduction of solvent usage, low cost, easy handling, and non-toxic procedure. (orig.)

  16. Rocket-powered high-performance liquid chromatographic analysis of plant ascorbate and glutathione.

    Science.gov (United States)

    Davey, M W; Dekempeneer, E; Keulemans, J

    2003-05-01

    We describe a robust procedure for the extraction and high-performance liquid chromatographic analysis of L-ascorbate (vitamin C), glutathione (gamma-glutamyl cysteinylglycine), and their respective oxidized forms from various plant tissues. Parameters such as the choice of extraction buffer, tissue disruption technique, sample stability, and separation conditions have all been optimized. In particular we found that the inclusion of the reducing agent dithiothreitol as a "stabilizer" in extracts with high phenolic content actually promoted oxidation of these antioxidants. Further, by using commercially available short "Rocket" HPLC columns in combination with high mobile-phase flow rates, analysis times were reduced to only 6min, making the method suitable for the high-resolution screening of large numbers of samples.

  17. Gas-liquid chromatographic determination of adipate content of acetylated di-starch adipate.

    Science.gov (United States)

    Mitchell, G A; Vanderbist, M J; Meert, F F

    1982-03-01

    A gas-liquid chromatographic method is described for rapid, quantitative determination of adipate content of acetylated di-starch adipate. The adipate group is very labile and, under mild alkaline conditions at ambient temperature, is easily hydrolyzed from the starch. Free adipic acid is formed by acidification of the solution with HCl, and then extracted with ethyl acetate. Ethyl acetate is removed under vacuum distillation, and a silyl derivative of the adipic acid is formed. Glutaric acid internal standard is introduced into the original starch sample before hydrolysis. An aliquot of the silylated solution is injected into a gas chromatograph fitted with a column having silicone oil as the active phase. A flame ionization detector is also incorporated. Results correlate well the amount of adipylating reagent used. No adipic acid is detectable when a hydrolyzed, extracted sample of acetylated di-starch adipate is subjected to a second extraction. Recovery levels of adipic acid, from starches fortified with 100-500 ppm, are in the range of 97-102.5%.

  18. Gas chromatographic determination of propionates as paranitrobenzyl ester in bakery products.

    Science.gov (United States)

    Takatsuki, K; Sakai, K

    1982-07-01

    A procedure was developed to determine propionates used as mold inhibitors and preservatives in bakery products. Propionates were extracted from the sample with water alkalinized by potassium carbonate. Water was evaporated, and the residue was reacted with paranitrobenzyl bromide in dimethyl-formamide-water (90 + 10) at room temperature to convert propionates to paranitrobenzyl ester, which was determined with a gas chromatograph equipped with a flame ionization detector. Bakery products, such as bread, sponge cake, cookies, and biscuits, were analyzed by this procedure. Recoveries from samples fortified with propionates ranged from 94 to 101%, with a standard deviation of 3.32. The concentrations determined were 50 to 2500 micrograms/g sample.

  19. Capillary gas chromatographic determination of dimethachlon residues in fresh tobacco leaves and cut-tobacco

    Institute of Scientific and Technical Information of China (English)

    LIU Hong-cheng; LI Qi-wan; TANG Li-bin

    2007-01-01

    Simple procedures for extraction and chromatographic determination of dimethachlon residues in fresh tobacco leaves and cut-tobacco are described. The determination was carried out by capillary gas chromatography (GC) with electron capture detection (ECD) and confirmed by GC-MS. The mean recoveries and relative standard deviation (RSD) were 93.2%~112.9% and 3.5%~6.7%, respectively at levels ranging from 0.01 to 0.1 mg/kg. The limit of determination was 0.001 mg/kg. Tobacco samples in routine check were successfully analyzed using the proposed method.

  20. A new method for high-performance liquid chromatographic determination of drotaverine in plasma.

    Science.gov (United States)

    Mezei, J; Küttel, S; Szentmiklósi, P; Marton, S; Rácz, I

    1984-10-01

    A sensitive, specific high-performance liquid chromatographic procedure was developed for the determination of plasma drotaverine levels. Basic plasma samples were adjusted to pH 1.5 and extracted with chloroform. HPLC [n-heptane-dichloromethane-diethylamine (50:25:2)] on a microporous silica column, with a variable-wavelength UV detector set at 302 nm allowed the measurement of drotaverine at the 50-ng/mL level. The utility of this method for determination of drotaverine in dog and rat plasma was demonstrated.

  1. Seasonal Variation and Resin Composition in the Andean Tree Austrocedrus chilensis

    Directory of Open Access Journals (Sweden)

    Verónica Rachel Olate

    2014-05-01

    Full Text Available Little is known about the changes in resin composition in South American gymnosperms associated with the different seasons of the year. The diterpene composition of 44 resin samples from seven Austrocedrus chilensis (Cupressaceae trees, including male and female individuals, was investigated in three different seasons of the year (February, June and November. Twelve main diterpenes were isolated by chromatographic means and identified by gas chromatography-mass spectrometry and nuclear magnetic resonance (NMR. The diterpene composition was submitted to multivariate analysis to find possible associations between chemical composition and season of the year. The principal component analysis showed a clear relation between diterpene composition and season. The most characteristic compounds in resins collected in summer were Z-communic acid (9 and 12-oxo-labda-8(17,13E-dien-19 oic acid methyl ester (10 for male trees and 8(17,12,14-labdatriene (7 for female trees. For the winter samples, a clear correlation of female trees with torulosic acid (6 was observed. In spring, E-communic acid (8 and Z-communic acid (9 were correlated with female trees and 18-hydroxy isopimar-15-ene (1 with male tree resin. A comparison between percent diterpene composition and collection time showed p < 0.05 for isopimara-8(9,15-diene (2, sandaracopimaric acid (4, compound (7 and ferruginol (11.

  2. Seasonal variation and resin composition in the Andean tree Austrocedrus chilensis.

    Science.gov (United States)

    Olate, Verónica Rachel; Soto, Alex; Schmeda-Hirschmann, Guillermo

    2014-05-21

    Little is known about the changes in resin composition in South American gymnosperms associated with the different seasons of the year. The diterpene composition of 44 resin samples from seven Austrocedrus chilensis (Cupressaceae) trees, including male and female individuals, was investigated in three different seasons of the year (February, June and November). Twelve main diterpenes were isolated by chromatographic means and identified by gas chromatography-mass spectrometry and nuclear magnetic resonance (NMR). The diterpene composition was submitted to multivariate analysis to find possible associations between chemical composition and season of the year. The principal component analysis showed a clear relation between diterpene composition and season. The most characteristic compounds in resins collected in summer were Z-communic acid (9) and 12-oxo-labda-8(17),13E-dien-19 oic acid methyl ester (10) for male trees and 8(17),12,14-labdatriene (7) for female trees. For the winter samples, a clear correlation of female trees with torulosic acid (6) was observed. In spring, E-communic acid (8) and Z-communic acid (9) were correlated with female trees and 18-hydroxy isopimar-15-ene (1) with male tree resin. A comparison between percent diterpene composition and collection time showed p < 0.05 for isopimara-8(9),15-diene (2), sandaracopimaric acid (4), compound (7) and ferruginol (11).

  3. Resin-infiltrated-dentine--a FE-ESEM microscopy investigation.

    Science.gov (United States)

    Eick, J D; Dusevich, V M; de Wet, F A; van der Vyver, P J

    2004-09-01

    The formation of a hybrid layer is essential for bonding of dental composites to dentine. The objective of this study was to examine the effects of various etchants/conditioners and dentine bonding systems on dentine surfaces utilising a Field Emission Environmental SEM (FE-ESEM). Twenty one, freshly extracted human molar teeth were utilised. Dentine without resin application was initially observed both wet and dried in the following conditions: (1) fractured surface, (2) smear layer, and (3) smear layer removed with 37% phosphoric acid. Resin infiltration into dentine was then studied after applying Scotchbond 1, Optibond Solo, Prime & Bond NT, or Prompt L-Pop systems. Scotchbond 1, Optibond Solo, and Prime & Bond NT resins penetrated the dentine tubules and created hybrid layers; although, in some cases Prime & Bond NT only created a partially filled hybrid layer. No polymerised resin or hybrid layer was observed for Prompt L-Pop. The FE-ESEM permitted observation of specimens at near in-vivo wet conditions.

  4. HIGH PERFORMANCE THIN LAYER CHROMATOGRAPHIC DETERMINATION OF CAFFEIC ACID AND ROSMARINIC ACID FROM THE LEAVES OF Orthosiphon stamineus

    Directory of Open Access Journals (Sweden)

    M. Amzad Hossain

    2010-06-01

    Full Text Available This paper presents the studies performed on extraction of Orthosiphon stamineus, Benth by using different solvent for the identification and quantification of the caffeic acid derivatives such as caffeic acid  and rosmarinic acid which confers to the leaves of this plant with remarkable pharmaceutical properties. High performance thin-layer chromatographic (HPTLC allows the identification and the quantification of more than 20 samples in the same chromatographic run. The analysis of the samples requires 15-30 min compared with more than 2 h using a typical HPLC method. Using the techniques of the HPTLC and the UV-VIS spectra we have found that the extraction of this herb plant contain, the caffeic acid and rosmarinic acid ranging between 0.029% up to 0.506% and up to 0.24% to 2.24% respectively.     Keywords: Caffice acid derivatives, quantification, Malaysian Orthosiphon stamineus, HPTLC

  5. Hydrophilic interaction chromatographic analysis of anthocyanins.

    Science.gov (United States)

    Willemse, Chandré M; Stander, Maria A; de Villiers, André

    2013-12-06

    Hydrophilic interaction chromatography (HILIC) provides an alternative separation mode for the analysis of phenolic compounds, in which aqueous-organic mobile phases with polar stationary phases are used. This paper reports the evaluation of HILIC for the analysis of the natural pigments anthocyanins, which are of importance because of their chromophoric properties and a range of health benefits associated with their consumption. Several HILIC stationary phases (silica, diol, amine, cyanopropyl and amide) and mobile phase combinations were evaluated, with the latter proving particularly important due to the distinctive chromatographic behaviour of anthocyanins. Diode array detection was used for selective detection of anthocyanins, while high resolution quadrupole-time-of-flight mass spectrometry (Q-TOF-MS) was used for compound identification. The potential of HILIC separation is demonstrated for a range of anthocyanins varying in glycosylation and acylation patterns found in blueberries, grape skins, black beans, red cabbage and red radish. HILIC is shown to be a complementary separation method to reversed phase liquid chromatography (RP-LC) due to the alternative retention mechanism.

  6. Chromatographic Separation of Vitamin E Enantiomers

    Directory of Open Access Journals (Sweden)

    Ju-Yen Fu

    2017-02-01

    Full Text Available Vitamin E is recognized as an essential vitamin since its discovery in 1922. Most vegetable oils contain a mixture of tocopherols and tocotrienols in the vitamin E composition. Structurally, tocopherols and tocotrienols share a similar chromanol ring and a side chain at the C-2 position. Owing to the three chiral centers in tocopherols, they can appear as eight different stereoisomers. Plant sources of tocopherol are naturally occurring in the form of RRR while synthetic tocopherols are usually in the form of all-racemic mixture. Similarly, with only one chiral center, natural tocotrienols occur as the R-isoform. In this review, we aim to discuss a few chromatographic methods that had been used to separate the stereoisomers of tocopherols and tocotrienols. These methods include high performance liquid chromatography, gas chromatography and combination of both. The review will focus on method development including selection of chiral columns, detection method and choice of elution solvent in the context of separation efficiency, resolution and chiral purity. The applications for separation of enantiomers in vitamin E will also be discussed especially in terms of the distinctive biological potency among the stereoisoforms.

  7. THE SYNTHESIS OF MODIFIED DIPHENYL OXIDE RESIN

    Institute of Scientific and Technical Information of China (English)

    MAOMingfei; LIUZhifang; 等

    2002-01-01

    Modified diphenyl oxide resin was synthesized by co-polymerization of unsaturated acid and diphenyl oxide derivants.And then modified bismaleimide resin and expoxide linear phenolic resin were added into modified diphenyl oxide resin to co-polymerized and modify once more.The system was applied in composites.Their properties wrer investigated and found that they met the requirements as a heat-resisting adhesive.

  8. chromatographic analysis of crude oils and petroleum

    African Journals Online (AJOL)

    methods to industrial process operations have been discussed, ... petroleum by distillation, crystallization, and solvent extraction, as well as the analysis of the ...... Bland, F.W.; Davidson, R.L. Petroleum Processing Handbook, 4th ed., William ...

  9. The effect of flowable and dual-cure resin composite liners on gingival microleakage of posterior resin composites

    Directory of Open Access Journals (Sweden)

    Shirani F.

    2008-11-01

    Full Text Available "nBackground and Aim: Microleakage has been always a major concern in restorative dentistry. The curing contraction of composites still presents a problem with controlling microleakage and postoperative sensitivity. The aim of this study was to investigate the effect of flowable and dual-cure resin composite liners on gingival microleakage of packable resin composite restorations. "nMaterials and Methods: Sixty Class II cavities with cervical margins 1 mm below the CEJ were prepared in 30 extracted human molars. The teeth were randomly divided into five groups of 12 each. In control group, each tooth was restored incrementally with Tetric Ceram composite without applying any liner. In the second and forth groups, flowable materials- Tetric Flow and dual-cure composite resin cement Relay X ARC were placed respectively as a 1-mm thick gingival increment and cured before the resin composite restoration, whereas, in the third and fifth groups liners were cured with the first increment of packable composite.The restored teeth were stored for one week in distilled water at 370C, and thermocycled between 50C and 550C, sealed with nail varnish except the tooth - composite interface in cervical restoration margins and immersed in 2% basic fuchsin for 24 hours. Dye penetration was evaluated using a stereomicroscope with 28x magnification. The data were analyzed by Kruskal-Wallis and Mann-Whitney U-tests with p<0.05 as the level of significance. "nResults: The results of this study indicated that there were significant statistical differences between control - cured flowable liner, control-flowable liner without separately curing, control-cured dual cure composite resin cement groups.However there were no significant differences between dual-cure composite resin cement without separately curing-control,cured flowable liner-cured dual cure composite resin cement, flowable liner without separately curing-dual cure composite resin cement without separately

  10. 21 CFR 872.3140 - Resin applicator.

    Science.gov (United States)

    2010-04-01

    ... DEVICES DENTAL DEVICES Prosthetic Devices § 872.3140 Resin applicator. (a) Identification. A resin applicator is a brushlike device intended for use in spreading dental resin on a tooth during application of tooth shade material. (b) Classification. Class I (general controls). The device is exempt from...

  11. Method of removing contaminants from plastic resins

    Science.gov (United States)

    Bohnert,George W.; Hand,Thomas E.; Delaurentiis,Gary M.

    2007-08-07

    A method for removing contaminants from synthetic resin material containers using a first organic solvent system and a second carbon dioxide system. The organic solvent is utilized for removing the contaminants from the synthetic resin material and the carbon dioxide is used to separate any residual organic solvent from the synthetic resin material.

  12. Method for removing contaminants from plastic resin

    Science.gov (United States)

    Bohnert, George W.; Hand, Thomas E.; DeLaurentiis, Gary M.

    2008-12-30

    A method for removing contaminants from synthetic resin material containers using a first organic solvent system and a second carbon dioxide system. The organic solvent is utilized for removing the contaminants from the synthetic resin material and the carbon dioxide is used to separate any residual organic solvent from the synthetic resin material.

  13. 21 CFR 177.1595 - Polyetherimide resin.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Polyetherimide resin. 177.1595 Section 177.1595... Components of Single and Repeated Use Food Contact Surfaces § 177.1595 Polyetherimide resin. The polyetherimide resin identified in this section may be safely used as an article or component of an...

  14. 21 CFR 177.1556 - Polyaryletherketone resins.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Polyaryletherketone resins. 177.1556 Section 177... Components of Single and Repeated Use Food Contact Surfaces § 177.1556 Polyaryletherketone resins. The poly...) resins (CAS Reg. No. 55088-54-5 and CAS Reg. No. 60015-05-6 and commonly referred to...

  15. 21 CFR 177.1555 - Polyarylate resins.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Polyarylate resins. 177.1555 Section 177.1555 Food... of Single and Repeated Use Food Contact Surfaces § 177.1555 Polyarylate resins. Polyarylate resins... contact with food in accordance with the following prescribed conditions: (a) Identity. Polyarylate...

  16. 21 CFR 177.1560 - Polyarylsulfone resins.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Polyarylsulfone resins. 177.1560 Section 177.1560... Components of Single and Repeated Use Food Contact Surfaces § 177.1560 Polyarylsulfone resins. Polyarylsulfone resins (CAS Reg. No. 79293-56-4) may be safely used as articles or components of articles...

  17. 40 CFR 721.9495 - Acrylosilane resins.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Acrylosilane resins. 721.9495 Section... Substances § 721.9495 Acrylosilane resins. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substances identified as acrylosilane resins (PMNs P-95-1024/1040) are...

  18. 21 CFR 172.280 - Terpene resin.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Terpene resin. 172.280 Section 172.280 Food and..., Films and Related Substances § 172.280 Terpene resin. The food additive terpene resin may be safely used... polymer obtained by polymerizing terpene hydrocarbons derived from wood. It has a softening point of...

  19. 21 CFR 177.1680 - Polyurethane resins.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Polyurethane resins. 177.1680 Section 177.1680 Food... of Single and Repeated Use Food Contact Surfaces § 177.1680 Polyurethane resins. The polyurethane...) For the purpose of this section, polyurethane resins are those produced when one or more of...

  20. Multiple chromatographic peaks of phenylalanyl-tRNA associated with spontaneous hydrolysis of Y base during isolation.

    Science.gov (United States)

    Mushinski, J F; Marini, M

    1977-06-17

    In contrast to the single phenylalanyl-tRNA found in normal cells, some tumours are known to have more than one phenylalanine isoacceptor. However, during certain steps in tRNA isolation from normal or tumour tissue, additional chromatographic peaks can be artificially produced which may be confused with the tumour-specific Phe-tRNA. Such procedures as extraction with unbuffered phenol and unbuffered gel filtration chromatography appear to produce adventitious isoacceptors by hydrolysis of Y base.

  1. Comparison of Shear Bond Strength of RMGI and Composite Resin for Orthodontic Bracket Bonding.

    Science.gov (United States)

    Yassaei, Soghra; Davari, Abdolrahim; Goldani Moghadam, Mahjobeh; Kamaei, Ahmad

    2014-05-01

    The aim of this study was to compare the shear bond strength (SBS) of resin modified glass ionomer (RMGI) and composite resin for bonding metal and ceramic brackets. Eighty-eight human premolars extracted for orthodontic purposes were divided into 4 groups (n=22). In groups 1 and 2, 22 metal and ceramic brackets were bonded using composite resin (Transbond XT), respectively. Twenty-two metal and ceramic brackets in groups 3 and 4, respectively were bonded using RMGI (Fuji Ortho LC, Japan). After photo polymerization, the teeth were stored in water and thermocycled (500 cycles between 5° and 55°). The SBS value of each sample was determined using a Universal Testing Machine. The amount of residual adhesive remaining on each tooth was evaluated under a stereomicroscope. Statistical analyses were done using two-way ANOVA. RMGI bonded brackets had significantly lower SBS value compared to composite resin bonded groups. No statistically significant difference was observed between metal and ceramic brackets bonded with either the RMGI or composite resin. The comparison of the adhesive remnant index (ARI) scores between the groups indicated that the bracket failure mode was significantly different among groups (Pcomposite resin. RMGIs have significantly lower SBS compared to composite resin for orthodontic bonding purposes; however the provided SBS is still within the clinically acceptable range.

  2. Production of renewable phenolic resins by thermochemical conversion of biomass: A review

    Energy Technology Data Exchange (ETDEWEB)

    Effendi, A.; Gerhauser, H.; Bridgwater, A.V. [Bio-Energy Research Group, Aston University, Birmingham B4 7ET (United Kingdom)

    2008-10-15

    This review covers the production and utilisation of liquids from the thermal processing of biomass and related materials to substitute for synthetic phenol and formaldehyde in phenol formaldehyde resins. These resins are primarily employed in the manufacture of wood panels such as plywood, MDF, particle-board and OSB. The most important thermal conversion methods for this purpose are fast pyrolysis and vacuum pyrolysis, pressure liquefaction and phenolysis. Many feedstocks have been tested for their suitability as sources of phenolics including hard and softwoods, bark and residual lignins. Resins have been prepared utilising either the whole liquid product, or a phenolics enriched fraction obtained after fractional condensation or further processing, such as solvent extraction. None of the phenolics production and fractionation techniques covered in this review are believed to allow substitution of 100% of the phenol content of the resin without impacting its effectiveness compared to commercial formulations based on petroleum derived phenol. This survey shows that considerable progress has been made towards reaching the goal of a price competitive renewable resin, but that further research is required to meet the twin challenges of low renewable resin cost and satisfactory quality requirements. Particular areas of concern are wood panel press times, variability of renewable resin properties, odour, lack of reactive sites compared to phenol and potential for increased emissions of volatile organic compounds. (author)

  3. Gas chromatographic separation of hydrogen isotopes using metal hydrides

    Energy Technology Data Exchange (ETDEWEB)

    Aldridge, F.T.

    1984-05-09

    A study was made of the properties of metal hydrides which may be suitable for use in chromatographic separation of hydrogen isotopes. Sixty-five alloys were measured, with the best having a hydrogen-deuterium separation factor of 1.35 at 60/sup 0/C. Chromatographic columns using these alloys produced deuterium enrichments of up to 3.6 in a single pass, using natural abundance hydrogen as starting material. 25 references, 16 figures, 4 tables.

  4. Biological activity of some naturally occurring resins, gums and pigments against in vitro LDL oxidation.

    Science.gov (United States)

    Andrikopoulos, Nikolaos K; Kaliora, Andriana C; Assimopoulou, Andreana N; Papapeorgiou, Vassilios P

    2003-05-01

    Naturally occurring gums and resins with beneficial pharmaceutical and nutraceutical properties were tested for their possible protective effect against copper-induced LDL oxidation in vitro. Chiosmastic gum (CMG) (Pistacia lentiscus var. Chia resin) was the most effective in protecting human LDL from oxidation. The minimum and maximum doses for the saturation phenomena of inhibition of LDL oxidation were 2.5 mg and 50 mg CMG (75.3% and 99.9%, respectively). The methanol/water extract of CMG was the most effective compared with other solvent combinations. CMG when fractionated in order to determine a structure-activity relationship showed that the total mastic essential oil, collofonium-like residue and acidic fractions of CMG exhibited a high protective activity ranging from 65.0% to 77.8%. The other natural gums and resins (CMG resin 'liquid collection', P. terebinthus var. Chia resin, dammar resin, acacia gum, tragacanth gum, storax gum) also tested as above, showed 27.0%-78.8% of the maximum LDL protection. The other naturally occurring substances, i.e. triterpenes (amyrin, oleanolic acid, ursolic acid, lupeol, 18-a-glycyrrhetinic acid) and hydroxynaphthoquinones (naphthazarin, shikonin and alkannin) showed 53.5%-78.8% and 27.0%-64.1% LDL protective activity, respectively. The combination effects (68.7%-76.2% LDL protection) of ursolic-, oleanolic- and ursodeoxycholic- acids were almost equal to the effect (75.3%) of the CMG extract in comparable doses.

  5. Use of rhodamine WT with XAD-7 resin for determining groundwater flow paths

    Science.gov (United States)

    Close, Murray E.; Stanton, Greg J.; Pang, Liping

    2002-06-01

    A passive sampling system for use with rhodamine WT (RWT) in groundwater tracing experiments was developed to assist in the characterisation of groundwater flow paths. Amberlite XAD-7 resin was found to be suitable for adsorption of RWT, which can then be extracted using an ethanol/water mix and analysed fluorometrically. Batch and column experiments showed that XAD-7 resin has a high RWT capacity. The adsorption was slightly dependent on pH, but was always above 75% under batch conditions. The resin had a high percentage mass recovery at flow velocities around 1.5 m/day, but this decreased with increasing flow velocities. Desorption of RWT off the resin in water is dependent on the flow velocity of water and the time after the peak RWT has passed. The mass of RWT extracted from the resin bags correlated very well with both the RWT mass flux in the water and the peak concentrations observed in the monitoring wells in a field experiment. The results of resin bags were reproducible in the field with a mean coefficient of variation equal to 16%. This method has been successfully applied to two field situations with different flow velocities to indicate groundwater flow paths.

  6. Quantifying process tradeoffs in the operation of chromatographic sequences.

    Science.gov (United States)

    Ngiam, Sheau-Huey; Bracewell, Daniel G; Zhou, Yuhong; Titchener-Hooker, Nigel J

    2003-01-01

    A method for the rapid representation of key process tradeoffs that need to be made during the analysis of chromatographic sequences has been proposed. It involves the construction of fractionation and maximum purification factor versus yield diagrams, which can be completed easily on the basis of chromatographic data. The output of the framework developed reflects the degree of tradeoff between levels of yield and purity and provides a fast and precise prediction of the sample fraction collection strategy needed to meet a desired process specification. The usefulness of this approach for the purposes of product purification and contaminant removal in a single chromatographic step has been successfully demonstrated in an earlier paper and it is now extended by application to a chromatographic sequence: the separation of a hypothetical three-component protein system by hydrophobic interaction chromatography (HIC) followed by size exclusion chromatography (SEC). The HIC operation has a strong impact upon the subsequent SEC step. The studies show how the analysis of performance in such a chromatographic sequence can be carried out easily and in a straightforward fashion using the fractionation diagram approach. The methodology proposed serves as a useful tool for identifying the process tradeoffs that must be made during operation of a sequence of chromatographic steps and indicates the impact on further processing of the cut-point decisions that are made.

  7. Chromatographic Enantioseparations in Achiral Environments: Myth or Truth?

    Science.gov (United States)

    Martens, Jürgen; Bhushan, Ravi; Sajewicz, Mieczyslaw; Kowalska, Teresa

    2017-08-01

    Direct chromatographic enantioseparations are among the most important practical tasks of chromatography. The accepted rules and concepts of stereochemistry anticipated one type of chromatographic systems applicable only to such enantioseparations consisting either of chiral stationary phase, or chiral selector present in mobile phase. In such a model of chromatographic system, both racemic and non-racemic mixtures could be enantioseparated. Over the years, however, reports on successful chiral enantioseparations in non-chiral chromatographic systems have cumulated as well. To adapt the initial model to novel experimental evidence, an assumption had to be added stating that these were only non-racemic mixtures (and not racemic ones), which could be enantioseparated in achiral chromatographic systems, by granting them an inevitable chirality from the enantiomeric excess of a more abundant enantiomer. There still exists an overlooked portion of experimental evidence for successful enantioseparations of racemic mixtures in the non-chiral chromatographic systems, which cannot be explained by the accepted model. Facing this incompatibility between the model and practical results, we reflect on how to reconcile these two by questioning the possibility of pinpointing a true racemate with the help of our imperfect analytical tools. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  8. Sorption of Uranium Ions from Their Aqueous Solution by Resins Containing Nanomagnetite Particles

    Directory of Open Access Journals (Sweden)

    Mahmoud O. Abd El-Magied

    2016-01-01

    Full Text Available Magnetic amine resins composed of nanomagnetite (Fe3O4 core and glycidyl methacrylate (GMA/N,N′-methylenebisacrylamide (MBA shell were prepared by suspension polymerization of glycidyl methacrylate with N,N′-methylenebisacrylamide in the presence of nanomagnetite particles and immobilized with different amine ligands. These resins showed good magnetic properties and could be easily retrieved from their suspensions using an external magnetic field. Adsorption behaviors of uranium ions on the prepared resins were studied. Maximum sorption capacities of uranium ions on R-1 and R-2 were found to be 92 and 158 mg/g. Uranium was extracted successfully from three granite samples collected from Gabal Gattar pluton, North Eastern Desert, Egypt. The studied resins showed good durability and regeneration using HNO3.

  9. Occupational exposure to epoxy resins

    NARCIS (Netherlands)

    Terwoert, J.; Kersting, K.

    2014-01-01

    Products based on epoxy resins as a binder have become popular in various settings, among which the construction industry and in windmill blade production, as a result of their excellent technical properties. However, due to the same properties epoxy products are a notorious cause of allergic skin d

  10. Stochastic resin transfer molding process

    CERN Document Server

    Park, M

    2016-01-01

    We consider one-dimensional and two-dimensional models of stochastic resin transfer molding process, which are formulated as random moving boundary problems. We study their properties, analytically in the one-dimensional case and numerically in the two-dimensional case. We show how variability of time to fill depends on correlation lengths and smoothness of a random permeability field.

  11. Occupational exposure to epoxy resins

    NARCIS (Netherlands)

    Terwoert, J.; Kersting, K.

    2014-01-01

    Products based on epoxy resins as a binder have become popular in various settings, among which the construction industry and in windmill blade production, as a result of their excellent technical properties. However, due to the same properties epoxy products are a notorious cause of allergic skin

  12. [Epoxy resin systems and contact dermatitis].

    Science.gov (United States)

    Pietranek, Jolanta Eliza

    2007-01-01

    Contact dermatitis is the major chronic skin disease that represents a global health problem. Its prevalence has been significant increasing in the latest decades. Contact dermatitis substantially alters the social life of patients and affects their work productivity. Epoxy resin systems are a frequent cause of occupational allergic contact dermatitis. Epoxy resins have an extremely wide range of commercial applications. Epoxy resin systems include combinations of epoxy monomers, hardeners, reactive diluents, and/or a vast array of other additives. In occupational settings, sensitization occurs not only to resins, but also to hardeners and reactive diluents. In this article adverse effects of epoxy resin systems are discussed.

  13. Antioxidant phenolic extracts obtained from secondary Tunisian date varieties (Phoenix dactylifera L.) by hydrothermal treatments.

    Science.gov (United States)

    Mrabet, Abdessalem; Jiménez-Araujo, Ana; Fernández-Bolaños, Juan; Rubio-Senent, Fátima; Lama-Muñoz, Antonio; Sindic, Marianne; Rodríguez-Gutiérrez, Guillermo

    2016-04-01

    Three common non-commercial Tunisian date varieties were treated by two thermal systems, obtaining a liquid fraction which was characterized and its antioxidant capacity determined. The concentration of total phenols in the three varieties (Smeti, Garen Gazel, and Eguwa) was increased by steam explosion treatment up to 5311, 4680, and 3832 mg/kg of fresh dates, and their antioxidant activity up to 62.5, 46.5 and 43.1 mmol Trolox/kg of fresh date, respectively. Both thermal treatments increased the content of phenolic acids. Additionally, a long scale study was carried out in a pilot plant, with steam treatment at 140 °C and 160 °C for 30 min. The liquid phase was extracted and fractionated chromatographically using adsorbent or ionic resins. The phenolic profiles were determined for each fraction, yielding fractions with interesting antioxidant activities with EC50 values of up to 0.08 mg/L or values of TEAC of 0.67 mmol Trolox/g of extract.

  14. [Dimensional accuracy of microwave-cured denture base resin].

    Science.gov (United States)

    Uchida, K; Okamoto, F; Ogata, K; Sato, T

    1989-02-01

    Recently, microwave-cured denture base resin was developed, and the resin solved the problem of internal porosity which had been generated by curing the conventional denture base resins with microwave irradiation. In this study, the dimensional accuracy of microwave-cured denture base resin was compared with that of other denture base resins, such as pour-type resin, heat-cured resin and heat-shock resin. From the experiment, the following results were obtained. 1. Dimensional accuracy of microwave-cured denture base resin was better than that of heat-cured resin and heat-shock resin, and was similar to that of pour-type resin. 2. Dimensional accuracy of microwave-cured denture base resin by slow cooling method and rapid cooling method was almost the same. Those findings suggest that microwave-cured denture base resin is valuable in clinic.

  15. Regional bond strengths of adhesive resins to pulp chamber dentin.

    Science.gov (United States)

    Belli, S; Zhang, Y; Pereira, P N; Ozer, F; Pashley, D H

    2001-08-01

    Microleakage of oral microorganisms, which can occur due to the lack of sealing ability of permanent restorative materials, may cause failure of root canal treatments. Although a great deal of research has been done on sealing enamel and coronal dentin with resins, little research has been done on the adhesion of resins to the walls of pulp chambers. The purpose of this study was to evaluate regional bond strengths of two adhesive systems to the walls of pulp chambers. A section was made horizontally through the middle of the pulp chamber of extracted human third molars to divide the chamber into upper and lower halves. The pulp tissue was removed and the tooth segments were then divided into treatment subgroups. The pulp chambers were bonded with C&B Metabond (Parkell) or One-Step (Bisco), with or without 5% NaOCI pretreatment. The microtensile bond strengths of these resins to four different pulp chamber regions (bottom, wall, roof, and pulp horn areas) were then measured using an Instron machine. The data were expressed in MPa and were analyzed by a three-way ANOVA. Statistically significant differences were found among the test groups (p < 0.001). One-Step produced higher bond strengths to all pulp chamber regions except the floor, compared with C&B Metabond. The results indicated that high bond strengths can be achieved between adhesive resins and the various regions of the pulp chamber. This should permit the use of a thick layer of unfilled resin along the floor of the pulp chamber and over the canal orifices as a secondary protective seal after finishing root canal therapy.

  16. STUDIES ON INOSINE EXTRACTION BY ION EXCHANGE METHOD

    Institute of Scientific and Technical Information of China (English)

    HuangXiwen; ShiFang; 等

    1998-01-01

    The adsorption characteristics of inosine from fermentation solution on anion exchange resin under the condition of different pH,resin type are investigated.Besides,the desorption conditions are studied under different temperature.The adsorption and desorption mechanism are described to obtain the optimum technological condition of inosine extraction.

  17. Photoacoustic analysis of dental resin polymerization

    Science.gov (United States)

    Coloiano, E. C. R.; Rocha, R.; Martin, A. A.; da Silva, M. D.; Acosta-Avalos, D.; Barja, P. R.

    2005-06-01

    In this work, we use the photoacoustic technique to monitor the curing process of diverse dental materials, as the resins chemically activated (RCA). The results obtained reveal that the composition of a determined RCA significantly alters its activation kinetics. Photoacoustic data also show that temperature is a significant parameter in the activation kinetics of resins. The photoacoustic technique was also applied to evaluate the polymerization kinetics of photoactivated resins. Such resins are photoactivated by incidence of continuous light from a photodiode. This leads to the polymerization of the resin, modifying its thermal properties and, consequently, the level of the photoacoustic signal. Measurements show that the polymerization of the resin changes the photoacoustic signal amplitude, indicating that photoacoustic measurements can be utilized to monitor the polymerization kinetic and the degree of polymerization of photoactivated dental resins.

  18. Bond strength of self-adhesive resin cements to different treated indirect composites.

    Science.gov (United States)

    Fuentes, M Victoria; Ceballos, Laura; González-López, Santiago

    2013-04-01

    The objective of this study was to determine microtensile bond strength (μTBS) to dentin of three self-adhesive and a total-etch resin cements used for luting different treated indirect composites. Composite overlays (Filtek Z250) were prepared. Their intaglio surfaces were ground with 600-grit SiC papers and randomly assigned to three different surface treatments: no treatment, silane application (RelyX Ceramic Primer), and silane agent followed by a bonding agent (Adper Scotchbond 1 XT). The composite overlays were luted to flat dentin surfaces of extracted human third molars using the following self-adhesive resin cements: RelyX Unicem, Maxcem Elite and G-Cem, and a total-etch resin cement, RelyX ARC. The bonded assemblies were stored in water (24 h, 37 °C) and subsequently prepared for μTBS testing. Beams of approximately 1 mm(2) were tested in tension at 1 mm/min in a universal tester (Instron 3345). Data were analyzed by two-way ANOVA and Student-Newman-Keuls tests (α = 0.05). A significant influence of the resin cement used was detected. Composite surface treatment and the interaction between the resin cement applied and surface treatment did not affect μTBS. Surface treatment of indirect resin composite did not improve the μTBS results of dentin/composite overlay complex. Self-adhesive resin cements tested obtained lower μTBS than the total-etch resin cement RelyX ARC. Specimens luted with Maxcem Elite exhibited the highest percentage of pretesting failures. Surface treatment of indirect resin composite with silane or silane followed by a bonding agent did not affect bond strength to dentin.

  19. Effect of laser preparation on bond strength of a self-adhesive flowable resin.

    Science.gov (United States)

    Yazici, A Rüya; Agarwal, Ishita; Campillo-Funollet, Marc; Munoz-Viveros, Carlos; Antonson, Sibel A; Antonson, Donald E; Mang, Thomas

    2013-01-01

    The aim of this in vitro study was to evaluate the effect of laser treatment on shear bond strength of a self-adhesive flowable resin composite to human dentin. Eighty extracted sound human molar teeth were used for the study. The teeth were sectioned mesiodistally and embedded in acrylic blocks. The dentin surfaces were ground wet with 600-grit silicon carbide (SiC) paper. They were randomly divided into two preparation groups: laser (Er:YAG laser, with 12 Hz, 350 mJ energy) and control (SiC). Each group was then divided into two subgroups according to the flowable resin composite type (n = 20). A self-adhesive flowable (Vertise Flow) and a conventional flowable resin (Premise Flow) were used. Flowable resin composites were applied according to the manufacturer's recommendations using the Ultradent shear bond Teflon mold system. The bonded specimens were stored in water at 37 °C for 24 h. Shear bond strength was tested at 1 mm/min. The data were logarithmically transformed and analyzed using two-way analysis of variance and Student-Newman-Keul's test at a significance level of 0.05. The self-adhesive flowable resin showed significantly higher bond strength values to laser-prepared surfaces than to SiC-prepared surfaces (p flowable resin did not show such differences (p = 0.224). While there was a significant difference between the two flowable resin composites in SiC-prepared surfaces (p flowable resin composite differs according to the type of dentin surface preparation. Laser treatment increased the dentin bonding values of the self-adhesive flowable resin.

  20. Multivariate analysis of variance of designed chromatographic data. A case study involving fermentation of rooibos tea.

    Science.gov (United States)

    Marini, Federico; de Beer, Dalene; Walters, Nico A; de Villiers, André; Joubert, Elizabeth; Walczak, Beata

    2017-03-17

    An ultimate goal of investigations of rooibos plant material subjected to different stages of fermentation is to identify the chemical changes taking place in the phenolic composition, using an untargeted approach and chromatographic fingerprints. Realization of this goal requires, among others, identification of the main components of the plant material involved in chemical reactions during the fermentation process. Quantitative chromatographic data for the compounds for extracts of green, semi-fermented and fermented rooibos form the basis of preliminary study following a targeted approach. The aim is to estimate whether treatment has a significant effect based on all quantified compounds and to identify the compounds, which contribute significantly to it. Analysis of variance is performed using modern multivariate methods such as ANOVA-Simultaneous Component Analysis, ANOVA - Target Projection and regularized MANOVA. This study is the first one in which all three approaches are compared and evaluated. For the data studied, all tree methods reveal the same significance of the fermentation effect on the extract compositions, but they lead to its different interpretation.