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Sample records for chromatography hplc coupled

  1. Determination of organic and inorganic mercury species in Sungai Kinta, Perak by reversed-phase high performance liquid chromatography (HPLC) on-line coupled with ICP-MS

    International Nuclear Information System (INIS)

    This paper describes a simple method for mercury speciation in river water samples of Sungai Kinta, Perak. Separation and measurement were done by high-performance liquid chromatography on-line with inductively coupled plasma mass spectrometry (HPLC/ ICP-MS). Separation of mercury species was accomplished within 6 minutes on an AQ C18 4.6 mm i.d x 150 mm, 5 μm reversed phase column with 0.1 % (w/ v) L-cysteine as mobile phase. Under the optimum instrumental conditions, recoveries of 101-104 % for MeHg+ and 96 - 104 % for Hg2+ were obtained with experimental detection limits of 1ngL-1 for inorganic mercury and 1.5 μgL-1 for organic mercury. (author)

  2. Characterization of chemical constituents in Rhodiola Crenulate by high-performance liquid chromatography coupled with Fourier-transform ion cyclotron resonance mass spectrometer (HPLC-FT-ICR MS).

    Science.gov (United States)

    Han, Fei; Li, Yanting; Mao, Xinjuan; Xu, Rui; Yin, Ran

    2016-05-01

    In this work, an approach using high-performance liquid chromatography coupled with diode-array detection and Fourier-transform ion cyclotron resonance mass spectrometer (HPLC-FT-ICR MS) for the identification and profiling of chemical constituents in Rhodiola crenulata was developed for the first time. The chromatographic separation was achieved on an Inertsil ODS-3 column (150 mm × 4.6 mm,3 µm) using a gradient elution program, and the detection was performed on a Bruker Solarix 7.0 T mass spectrometer equipped with electrospray ionization source in both positive and negative modes. Under the optimized conditions, a total of 48 chemical compounds, including 26 alcohols and their glycosides, 12 flavonoids and their glycosides, 5 flavanols and gallic acid derivatives, 4 organic acids and 1 cyanogenic glycoside were identified or tentatively characterized. The results indicated that the developed HPLC-FT-ICR MS method with ultra-high sensitivity and resolution is suitable for identifying and characterizing the chemical constituents in R. crenulata. And it provides a helpful chemical basis for further research on R. crenulata. Copyright © 2016 John Wiley & Sons, Ltd. PMID:27194521

  3. Measurement of isotopic composition of lanthanides in reprocessing process solutions by high-performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC/ICP-MS)

    International Nuclear Information System (INIS)

    Isotopic compositions of fission products in process solutions and wastes in a reprocessing plant are valuable to proceed safety study of the solutions and research/development concerning treatment/disposal of the wastes. The amount of neodymium-148 is a reliable indication to evaluate irradiation history. The isotopic compositions of samarium and gadolinium in high radioactive wastes are referred to as essential data to evaluate environmental impact in geological repositories. However, pretreatment of analysis must be done with complicated chemical separation such as solvent extraction and ion exchange. The actual measurement data of isotopic compositions of lanthanides comparable to the one of actinides in spent fuel reprocessing process has not been obtained enough. Rapid and high sensitive analytical technique based on high-performance liquid chromatography (HPLC) with an inductively coupled plasma mass spectrometry (ICP-MS) has been developed for the measurement of isotopic compositions of lanthanides in spent fuel reprocessing solutions. HPLC/ICP-MS measurement system was customized for a glove-box to be applied to the radioactive solutions. The cation exchange chromatographic columns (Shim-pack IC-C1) and injection valve (20μL) were located inside of the glove-box except the chromatographic pump. The elements of lanthanide group were separated by a gradient program of HPLC with α-hydroxyisobutyric acid. Isotopic compositions of lanthanides in eluate was sequentially analyzed by a quadruple ICP-MS. Optimization of parameter of HPLC and ICP-MS measurement system was examined with standard solutions containing 14 lanthanide elements. The elements of lanthanides were separated by HPLC and detected by ICP-MS within 25 minutes. The detection limits of Nd-146, Sm-147 and Gd-157 were 0.37 μg L-1, 0.69 μg L-1 and 0.47 μg L-1, respectively. The analytical precision of the above three isotopes was better than 10% for standard solutions of 100 μg L-1 with five

  4. Application of high performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC-ICP-MS) for determination of chromium compounds in the air at the workplace.

    Science.gov (United States)

    Stanislawska, Magdalena; Janasik, Beata; Wasowicz, Wojciech

    2013-12-15

    The toxicity and bioavailability of chromium species are highly dependable on the form or species, therefore determination of total chromium is insufficient for a complete toxicological evaluation and risk assessment. An analytical method for determination of soluble and insoluble Cr (III) and Cr (VI) compounds in welding fume at workplace air has been developed. The total chromium (Cr) was determined by using quadruple inductively coupled plasma mass spectrometry (ICP-MS) equipped with a dynamic reaction cell (DRC(®)). Soluble trivalent and hexavalent chromium compounds were determined by high performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC-ICP-MS). A high-speed, reversed-phase CR C8 column (PerkinElmer, Inc., Shelton, CT, USA) was used for the speciation of soluble Cr (III) and soluble Cr (VI). The separation was accomplished by interaction of the chromium species with the different components of the mobile phase. Cr (III) formed a complex with EDTA, i.e. retained on the column, while Cr (VI) existed in the solutions as dichromate. Alkaline extraction (2% KOH and 3% Na2CO3) and anion exchange column (PRP-X100, PEEK, Hamilton) were used for the separation of the total Cr (VI). The results of the determination of Cr (VI) were confirmed by the analysis of the certified reference material BCR CRM 545 (Cr (VI) in welding dust). The results obtained for the certified material (40.2±0.6 g kg(-1)) and the values recorded in the examined samples (40.7±0.6 g kg(-1)) were highly consistent. This analytical method was applied for the determination of chromium in the samples in the workplace air collected onto glass (Whatman, Ø 37 mm) and membrane filters (Sartorius, 0.8 μm, Ø 37 mm). High performance liquid chromatography with inductively coupled plasma mass spectrometry is a remarkably powerful and versatile technique for determination of chromium species in welding fume at workplace air. PMID:24209303

  5. Determination of trace amounts of rare-earth elements in highly pure neodymium oxide by sector field inductively coupled plasma mass spectrometry (ICP-SFMS) and high-performance liquid chromatography (HPLC) techniques

    International Nuclear Information System (INIS)

    Recently rare-earth elements (REE) have received much attention in fields of geochemistry and industry. Rapid and accurate determinations of them are increasingly required as industrial demands expand. Sector field inductively coupled plasma mass spectrometry (ICP-SFMS) with high-performance liquid chromatography (HPLC) has been applied to the determination of REE. HR ICP-MS was used as an element-selective detector for HPLC in highly pure materials. The separation of REE with HPLC helped to avoid erroneous analytical results due to spectral interferences. Sixteen elements (Sc, Y and 14 lanthanides) were determined selectively with the HPLC/ICP-SFMS system using a concentration gradient methods. The detection limits with the HPLC/ICP-SFMS system were about 0.5-10 pg mL-1. The percentage recovery ranged from 90% to 100% for different REE. The %RSD of the methods varying between 2.5% and 4.5% for a set of five (n=5) replicates was found for the IPEN's material and for the certificate reference sample. Determination of trace REEs in two highly pure neodymium oxides samples (IPEN and Johnson Matthey Company) were performed. In short, the IPEN's materials which are highly pure (>99.9%) were successfully analyzed without spectral interferences

  6. Determination of trace elements in high pure rare earth oxide by double focusing inductively coupled plasma mass spectrometry (HR ICP-MS) and high performance liquid chromatography (HPLC) techniques

    International Nuclear Information System (INIS)

    Rare earth oxides are used in several technological fields whose applications can be observed in several areas of modern technology, among which are included: lasers, semiconductors semi, high purity materials and metallic alloys. The field of applications of the rare earth elements is quite wide. Several important industrial applications are ceramics, catalysts and metallurgical as well as research areas and high technology sectors. Such applications have been presenting an accentuated growth in the last years. Chemical characterization of rare earth oxides of high purity has been constituting one of the major challenges of analytical chemistry. Several analytical techniques were used for chemical characterization of high purity rare earth the oxides. Even so, those techniques present limitations when one needs to characterize materials of a high level of purity, as in the case of rare earth oxides. Some of those limitations are associated, for example, to spectral interference. Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is a powerful analytical tool for quantitative analysis of metal impurities in high purity materials. The Instituto de Pesquisas Energeticas e Nucleares (IPEN) has an unit of production and purification of rare earth oxides, with above 99,9% level of purity. In this work, the rare earth impurities were characterized in samples (La2O3; CeO2; Pr6O11; Nd2O3; Sm2O3; Gd2O3; Y2O3) produced at the IPEN and certified standard materials produced by Johnson Matthey Chemical (JMC). The technique of high performance liquid chromatography (HPLC) was used in the separation of the impurities. Quantification of metallic impurities was carried out as inductively coupled plasma mass spectrometer (HR-ICP MS). In this work it is presented a new analytical methodology in the chemical characterization of metallic impurities in rare earth oxides of high purity (> 99,9%) with and without separation of the matrix. Analyses of standard certified materials and

  7. Characterisation of steroids in wooden crates of veal calves by accelerated solvent extraction (ASE) and ultra-high performance liquid chromatography coupled to triple quadrupole mass spectrometry (U-HPLC-QqQ-MS-MS).

    Science.gov (United States)

    Verheyden, K; Noppe, H; Vanden Bussche, J; Wille, K; Bekaert, K; De Boever, L; Van Acker, J; Janssen, C R; De Brabander, H F; Vanhaecke, L

    2010-05-01

    Illegal steroid administration to enhance growth performance in veal calves has long been, and still is, a serious issue facing regulatory agencies. Over the last years, stating undisputable markers of illegal treatment has become complex because of the endogenous origin of several anabolic steroids. Knowledge on the origin of an analyte is therefore of paramount importance. The present study shows the presence of steroid analytes in wooden crates used for housing veal calves. For this purpose, an analytical procedure using accelerated solvent extraction (ASE(R)), solid-phase extraction (SPE) and ultra-high performance liquid chromatography coupled to triple quadrupole mass spectrometry (U-HPLC-MS-MS) is developed for the characterisation of androstadienedione (ADD), boldenone (bBol), androstenedione (AED), beta-testosterone (bT), alpha-testosterone (aT), progesterone (P) and 17alpha-hydroxy-progesterone (OH-P) in wood samples. In samples of wooden crates used for housing veal calves, ADD, AED, aT and P could be identified. Using the standard addition approach concentrations of these analytes were determined ranging from 20 +/- 4 ppb to 32 +/- 4 ppb for ADD, from 19 +/- 5 ppb to 44 +/- 17 ppb for AED, from 11 +/- 6 ppb to 30 +/- 2 ppb for aT and from 14 +/- 1 ppb to 42 +/- 27 ppb for P, depending on the sample type. As exposure of veal calves to steroid hormones in their housing facilities might complicate decision-making on illegal hormone administration, inequitable slaughter of animals remains possible. Therefore, complete prohibition of wooden calf accommodation should be considered. PMID:20186540

  8. Speciation analysis by small-bore HPLC coupled to ICP-MS

    OpenAIRE

    Grotti, Marco; Terol Pardo, Amanda; Todolí Torró, José Luis

    2014-01-01

    Although high-performance liquid chromatography with inductively-coupled mass spectrometry (HPLC-ICP-MS) has established itself as the analytical technique of choice for elemental speciation analysis, there are remaining limitations, mainly concerning post-column dispersion effects and degradation of the ICP stability and ionization efficiency due to organic or saline mobile phases. The application of small-bore columns in conjunction with low dead-volume interfaces has proved very useful for...

  9. Analysis of alcohol dehydrogenase inhibitors from Desmodium styracifolium using centrifugal ultrafiltration coupled with HPLC-MS

    OpenAIRE

    Liu Liangliang; Chen Miao; Chen Xiaoqing

    2015-01-01

    Alcohol dehydrogenase (ADH) inhibitors play an important role in the treatment of human methanol or ethylene glycol poisoning and the suppression of acetaldehyde accumulation in alcoholics. In this study, centrifugal ultrafiltration coupled with high performance liquid chromatography-mass spectrometry (HPLC-MS) was utilized to screen and identify ADH inhibitors from ethyl acetate extract of Desmosium styracifolium (Osb.) Merr. The experiment conditions of c...

  10. Detection of Adulteration of Notoginseng Root Extract with Other Panax Species by Quantitative HPLC Coupled with PCA

    OpenAIRE

    Wang, Chong-Zhi; Ni, Ming; Sun, Shi; Li, Xiao-Li; He, Hui; Mehendale, Sangeeta R; Yuan, Chun-Su

    2009-01-01

    To distinguish the extract of notoginseng root from that of other species in the genus Panax, we used reverse phase high performance liquid chromatography (HPLC) coupled with a principal component analysis (PCA) method. The content of 12 saponins in notoginseng root extracts from different sources was evaluated. Herbal extracts from different plant parts of notoginseng, Asian ginseng, and American ginseng were also evaluated. With an HPLC assay, however, it is difficult to determine whether n...

  11. A hybrid FIA/HPLC system incorporating monolithic column chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Adcock, Jacqui L. [School of Life and Environmental Sciences, Deakin University, Geelong, Victoria 3217 (Australia); Francis, Paul S. [School of Life and Environmental Sciences, Deakin University, Geelong, Victoria 3217 (Australia)], E-mail: psf@deakin.edu.au; Agg, Kent M. [School of Life and Environmental Sciences, Deakin University, Geelong, Victoria 3217 (Australia); Marshall, Graham D. [GlobalFIA, Fox Island, WA 98333 (United States); Barnett, Neil W. [School of Life and Environmental Sciences, Deakin University, Geelong, Victoria 3217 (Australia)

    2007-09-26

    We have combined the generation of solvent gradients using milliGAT pumps, chromatographic separations with monolithic columns and chemiluminescence detection in an instrument manifold that approaches the automation and separation efficiency of HPLC, whilst maintaining the positive attributes of flow injection analysis (FIA), such as manifold versatility, speed of analysis and portability. As preliminary demonstrations of this hybrid FIA/HPLC system, we have determined six opiate alkaloids (morphine, pseudomorphine, codeine, oripavine, ethylmorphine and thebaine) and four biogenic amines (vanilmandelic acid, serotonin, 5-hydroxyindole-3-acetic acid and homovanillic acid) in human urine, using tris(2,2'-bipyridyl)ruthenium(III) and acidic potassium permanganate chemiluminescence detection.

  12. A hybrid FIA/HPLC system incorporating monolithic column chromatography

    International Nuclear Information System (INIS)

    We have combined the generation of solvent gradients using milliGAT pumps, chromatographic separations with monolithic columns and chemiluminescence detection in an instrument manifold that approaches the automation and separation efficiency of HPLC, whilst maintaining the positive attributes of flow injection analysis (FIA), such as manifold versatility, speed of analysis and portability. As preliminary demonstrations of this hybrid FIA/HPLC system, we have determined six opiate alkaloids (morphine, pseudomorphine, codeine, oripavine, ethylmorphine and thebaine) and four biogenic amines (vanilmandelic acid, serotonin, 5-hydroxyindole-3-acetic acid and homovanillic acid) in human urine, using tris(2,2'-bipyridyl)ruthenium(III) and acidic potassium permanganate chemiluminescence detection

  13. High performance liquid chromatography (HPLC) fingerprints and primary structure identification of corn peptides by HPLC-diode array detection and HPLC-electrospray ionization tandem mass spectrometry

    OpenAIRE

    Chi Wang; Hui He; Jiu-liang Zhang; Xing Li; Zhi-li Ma

    2016-01-01

    Corn peptides (CPs) are reported to have many biological functions, such as facilitating alcohol metabolism, antioxidation, antitumor, antihypertension, and hepatoprotection. To develop a method for quality control, the high-performance liquid chromatography (HPLC) system was applied. Twenty-eight common peaks were found in all the CPs of corn samples from Enshi, China, based on which, a fingerprinting chromatogram was established for use in quality control in future research. Subsequently, t...

  14. Quantification of 3α-hydroxytibolone in human plasma by high performance liquid chromatography coupled to electrospray ionization tandem mass spectrometry (HPLC-ESI-MS/MS: Application in a bioequivalence study in healthy postmenopausal volunteers

    Directory of Open Access Journals (Sweden)

    Lucas Azevedo Portela

    2016-06-01

    Full Text Available A sensitive, specific and fast method to quantify 3α-hydroxytibolone in human plasma using deuterated 3α-hydroxytibolone (d5 as internal standard is described. The analyte and the internal standard were extracted from plasma (900 μL by liquid-liquid extraction using ethyl ether/hexane (50/50, v/v and ammonium hydroxide (50%. The extracts were analyzed by high performance liquid chromatography coupled to electrospray ionization tandem mass spectrometry without derivatization. Chromatography was performed isocratically on a Gemini-NX™ C18 5 μm (150 × 4.6 mm i. d. column. The method had a chromatographic run time of 3.75 min and a linear calibration curve over the range 1–100 ng/mL. The limit of quantification validated was 1 ng/mL. This method was used to assess the bioequivalence between two different tibolone oral formulations: Livolon (1.25 mg tablet provided by Biolab Sanus Farmacêutica (Brazil, as the test formulation, and Libiam™ (1.25 mg tablet produced by Libbs Farmacêutica (Brazil, as the reference formulation. A single 3.75 mg dose of each formulation was administered to 46 postmenopausal female healthy volunteers. The study was conducted in an open, randomized, two-period crossover balanced design with a 2 week washout interval between the doses. The 90% confidence interval for Cmax, AUC(0-last and AUC(0-inf individual test/reference ratios were 97.48–111.51, 95.35–103.20 and 96.42–103.86, respectively. It is concluded that Livolon (1.25 mg tablet is bioequivalent to Libiam™ (1.25 mg tablet, with regards to both rate and extent of absorption.

  15. Separation of mAbs molecular variants by analytical hydrophobic interaction chromatography HPLC: overview and applications

    OpenAIRE

    Haverick, Mark; Mengisen, Selina; Shameem, Mohammed; Ambrogelly, Alexandre

    2014-01-01

    Hydrophobic interaction chromatography-high performance liquid chromatography (HIC-HPLC) is a powerful analytical method used for the separation of molecular variants of therapeutic proteins. The method has been employed for monitoring various post-translational modifications, including proteolytic fragments and domain misfolding in etanercept (Enbrel®); tryptophan oxidation, aspartic acid isomerization, the formation of cyclic imide, and α amidated carboxy terminus in recombinant therapeutic...

  16. Extraction and Purification of Glucoraphanin by Preparative High-Performance Liquid Chromatography (HPLC)

    Science.gov (United States)

    Lee, Iris; Boyce, Mary C.

    2011-01-01

    A student activity that focuses on the isolation of glucoraphanin from broccoli using preparative high-performance liquid chromatography (HPLC) is presented here. Glucoraphanin is a glucosinolate, whose byproducts are known to possess anticancer properties. It is present naturally at high levels in broccoli and other "Brassica" vegetables. This…

  17. Determination of methylmercury and estimation of total mercury in seafood using high performance liquid chromatography (HPLC) and inductively coupled plasma-mass spectrometry (ICP-MS): Method development and validation

    International Nuclear Information System (INIS)

    A method was developed for determination of methylmercury and estimation of total mercury in seafood. Mercury (Hg) compounds were extracted from 0.5 g edible seafood or 0.2 g lyophilized reference material by adding 50 ml aqueous 1% w/v L-cysteine.HCl.H2O and heating 120 min at 60 deg. C in glass vials. Hg compounds in 50 μl of filtered extract were separated by reversed-phase high performance liquid chromatography using a C-18 column and aqueous 0.1% w/v L-cysteine.HCl.H2O + 0.1% w/v L-cysteine mobile phase at room temperature and were detected by inductively coupled plasma-mass spectrometry at mass-to-charge ratio 202. Total Hg was calculated as the mathematical sum of methyl and inorganic Hg determined in extracts. For seafoods containing 0.055-2.78 mg kg-1 methylmercury and 0.014-0.137 mg kg-1 inorganic Hg, precision of analyses was ≤5% relative standard deviation (R.S.D.) for methylmercury and ≤9% R.S.D. for inorganic Hg. Recovery of added analyte was 94% for methylmercury and 98% for inorganic Hg. Methyl and total Hg results for reference materials agreed with certified values. Limits of quantitation were 0.007 mg kg-1 methylmercury and 0.005 mg kg-1 inorganic Hg in edible seafood and 0.017 mg kg-1 methylmercury and 0.012 mg kg-1 inorganic Hg in lyophilized reference materials. Evaluation of analyte stability demonstrated that L-cysteine both stabilized and de-alkylated methylmercury, depending on holding time and cysteine concentration. Polypropylene adversely affected methylmercury stability. Total Hg results determined by this method were equivalent to results determined independently by cold vapour-atomic absorption spectrometry. Methylmercury was the predominant form of Hg in finfish. Ratios of methylmercury/total Hg determined by this method were 93-98% for finfish and 38-48% for mollusks

  18. Characterisation of spent nuclear fuels by an on-line coupled HPLC-ICP-MS system

    Energy Technology Data Exchange (ETDEWEB)

    Guenther-Leopold, I.; Gabler, F.; Wernli, B.; Kopajtic, Z

    2000-07-01

    The determination of burn-up is one of the essential components of post-irradiation examination of nuclear fuel samples. In the framework of the ARIANE programme (Actinides Research in a Nuclear Element), at PSI the analysis of the isotopic vectors of uranium, plutonium, neodymium and some other fission and spallation products was carried out for the first time in the Hot Lab using high-performance liquid chromatography (HPLC), coupled on-line with an inductively coupled plasma mass spectrometer (ICP-MS). The results of these investigations, a comparison with the classical technique for burn-up determination, the advantages and limitations of the new method, the accuracy and precision of these types of analyses, the applicability of the technique to other samples and separation problems, and conclusions for further analyses of nuclear fuel samples, are here presented. (authors)

  19. Characterisation of spent nuclear fuels by an on-line coupled HPLC-ICP-MS system

    International Nuclear Information System (INIS)

    The determination of burn-up is one of the essential components of post-irradiation examination of nuclear fuel samples. In the framework of the ARIANE programme (Actinides Research in a Nuclear Element), at PSI the analysis of the isotopic vectors of uranium, plutonium, neodymium and some other fission and spallation products was carried out for the first time in the Hot Lab using high-performance liquid chromatography (HPLC), coupled on-line with an inductively coupled plasma mass spectrometer (ICP-MS). The results of these investigations, a comparison with the classical technique for burn-up determination, the advantages and limitations of the new method, the accuracy and precision of these types of analyses, the applicability of the technique to other samples and separation problems, and conclusions for further analyses of nuclear fuel samples, are here presented. (authors)

  20. Application of directly coupled HPLC MMR to separation and characterization of lipoproteins from human serum

    DEFF Research Database (Denmark)

    Daykin, C. A.; Corcoran, O.; Hansen, S. H.;

    2001-01-01

    plasma proteins such as albumin occurred, and this clearly limits quantitation of that species by HPLC peak integration. We also show, for the first time, the application of directly coupled HPLC H-1 NMR spectroscopy to confirm the identification of the three major lipoproteins, The full chromatographic...... by the HPLC separation and that their gross supramolecular organization was intact....

  1. Specific determination of selenoaminoacids in whole milk by 2D size-exclusion-ion-paring reversed phase high-performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP MS)

    International Nuclear Information System (INIS)

    A procedure was developed for the quantitative recovery of selenomethionine (SeMet) and selenocysteine (SeCys) from whole milk. It was based on the protein unfolding, carbamidomethylation of the aminoacid residues using iodoacetamide and proteolysis using Protease XIV. The selenoaminoacids were specifically determined by ion-paring reversed phase HPLC-ICP MS after their isolation from the post-reaction mixture by size-exclusion LC. Se(IV) present in the sample was derivatized as well and was determined along with the selenoaminoacids. The origin and identity of species were identified by the co-elution with the Se(IV), isotopically labelled selenomethionine, and with the synthetic standard of carbamidomethylated selenocysteine. The method development for SeCys was assisted by using glutathione peroxidise as the SeCys standard. SeMet, SeCys and Se(IV) were quantified by the method of standard additions. The mass balance provided a measure of the method validation. The method was applied to monitoring selenium speciation during supplementation of cows (dose-effect study) with Se-rich yeast containing feed and during milk processing

  2. Specific determination of selenoaminoacids in whole milk by 2D size-exclusion-ion-paring reversed phase high-performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP MS)

    Energy Technology Data Exchange (ETDEWEB)

    Bierla, Katarzyna [Laboratoire de Chimie Analytique Bio-Inorganique et Environnement, CNRS UMR5254, Helioparc, 2, av. Pr. Angot, 64053 Pau (France)], E-mail: katarzyabierla@wp.pl; Szpunar, Joanna [Laboratoire de Chimie Analytique Bio-Inorganique et Environnement, CNRS UMR5254, Helioparc, 2, av. Pr. Angot, 64053 Pau (France); Lobinski, Ryszard [Laboratoire de Chimie Analytique Bio-Inorganique et Environnement, CNRS UMR5254, Helioparc, 2, av. Pr. Angot, 64053 Pau (France); Warsaw Technical University, Department of Analytical Chemistry, Noakowskiego 3, 00-664 Warsaw (Poland)

    2008-08-29

    A procedure was developed for the quantitative recovery of selenomethionine (SeMet) and selenocysteine (SeCys) from whole milk. It was based on the protein unfolding, carbamidomethylation of the aminoacid residues using iodoacetamide and proteolysis using Protease XIV. The selenoaminoacids were specifically determined by ion-paring reversed phase HPLC-ICP MS after their isolation from the post-reaction mixture by size-exclusion LC. Se(IV) present in the sample was derivatized as well and was determined along with the selenoaminoacids. The origin and identity of species were identified by the co-elution with the Se(IV), isotopically labelled selenomethionine, and with the synthetic standard of carbamidomethylated selenocysteine. The method development for SeCys was assisted by using glutathione peroxidise as the SeCys standard. SeMet, SeCys and Se(IV) were quantified by the method of standard additions. The mass balance provided a measure of the method validation. The method was applied to monitoring selenium speciation during supplementation of cows (dose-effect study) with Se-rich yeast containing feed and during milk processing.

  3. Study of HPLC/ICP-MS coupling for the As speciation

    International Nuclear Information System (INIS)

    Trace metals in the environment may provide benefit or risk to humans, other life forms, and the environment. More robust and information-rich trace and ultra-trace analyses are needed to all adequate risk/benefit assessments. Further, it is no longer adequate to consider only the total trace metal or metalloid, because the impact of elements on ecological systems or biological organisms is not necessarily given by total element concentrations alone. It is necessary to determine the chemical form (species) of the element, primarily the oxidation state or the organometallic nature, because different species of the same metal can range from essential to innocuous to toxic. The actual toxicity levels from different arsenic compounds vary greatly. Inorganic arsenic is considered the most acutely toxic form; arsenite (AsIII) is more toxic than arsenate (AsV). The chronic toxicity of arsenic compounds is currently not well understood and is actively being researched. In this study, the viability of the ICP-MS detector coupled with High Performance Liquid Chromatography (HPLC) was tested in 21 water samples from the Das Velhas River, Minas Gerais state, in Brazil. The results showed that the low detection limits and the ease coupling HPLC system - which offers a rugged and versatile separation technique - makes ICP-MS a successful detection method for arsenic speciation analysis. (author)

  4. Preparation and Characterization of a Polymeric Monolithic Column for Use in High-Performance Liquid Chromatography (HPLC)

    Science.gov (United States)

    Bindis, Michael P.; Bretz, Stacey Lowery; Danielson, Neil D.

    2011-01-01

    The high-performance liquid chromatography (HPLC) experiment, most often done in the undergraduate analytical instrumentation laboratory course, generally illustrates reversed-phase chromatography using a commercial C[subscript]18 silica column. To avoid the expense of periodic column replacement and introduce a choice of columns with different…

  5. Gas and liquid chromatography with inductively coupled plasma mass spectrometry detection for environmental speciation analysis — advances and limitations

    Science.gov (United States)

    Szpunar, Joanna; McSheehy, Shona; Połeć, Kasia; Vacchina, Véronique; Mounicou, Sandra; Rodriguez, Isaac; Łobiński, Ryszard

    2000-07-01

    Recent advances in the coupling of gas chromatography (GC) and high performance liquid chromatography (HPLC) with inductively coupled plasma mass spectrometry (ICP MS) and their role in trace element speciation analysis of environmental materials are presented. The discussion is illustrated with three research examples concerning the following topics: (i) development and coupling of multicapillary microcolumn GC with ICP MS for speciation of organotin in sediment and biological tissue samples; (ii) speciation of arsenic in marine algae by size-exclusion-anion-exchange HPLC-ICP MS; and (iii) speciation of cadmium in plant cell cultures by size-exclusion HPLC-ICP MS. Particular attention is paid to the problem of signal identification in ICP MS chromatograms; the potential of electrospray MS/MS for this purpose is highlighted.

  6. Discrimination of Black Ball-point Pen Inks by High Performance Liquid Chromatography (HPLC)

    International Nuclear Information System (INIS)

    In this study, thirteen types of black ball-point pen inks of three major brands were analyzed using high performance liquid chromatography (HPLC). Separation of the ink components was achieved using Bondapak C-18 column with gradient elution using water, ethanol and ethyl acetate. The chromatographic data obtained at wavelength 254.8 nm was analyzed using agglomerative hierarchical clustering (AHC) and principle component analysis (PCA). AHC was able to group the inks into three clusters. This result was supported by PCA, whereby distinct separation of the three different brands was achieved. Therefore, HPLC in combination with chemometric methods may be a valuable tool for the analysis of black ball-point pen inks for forensic purposes. (author)

  7. Determination of alpha-Tocopherol (vitamin E) in irradiated garlic by high performance liquid chromatography (HPLC)

    International Nuclear Information System (INIS)

    The effects of 60Co ionizing radiations in doses of 0, 75, 100, 150, 200 and 250Gy on garlic, upon the α-tocopherol concentration were studied. The α-tocopherol contents were established by high performance liquid chromatography (HPLC), after direct hexane extraction from the garlic samples. The α-tocopherol was determined through normal phase column, and mobile phase was composed by hexane: iso-propyl alcohol (99:01 v/v), with 2mL/min flow rate and fluorescence detector. It is statistically shown that an irradiation dose of up to 150 Gy does not affect the garlic α-tocopherol content. (author)

  8. Determination of technetium-99 in soil samples by high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Muto, Toshio; Shimokawa, Toshinari [Tokyo Metropolitan Isotope Research Center (Japan)

    1997-03-01

    A new powerful analytical technique viz. high performance liquid chromatography(HPLC) coupled to inductively coupled plasma mass spectrometry(HPLC/ICP-MS) has been applied to the determination of technetium-99({sup 99}Tc) in soils as a typical environmental sample. Technetium was enriched in a solution from incinerated soil samples by leaching in HNO{sub 3} and passed through `TEVA resin` column. The solution was injected into HPLC/ICP-MS system to eliminate the interfering elements (i.e. Ru and Mo) and to determine the {sup 99}Tc concentration at the same time. The concentrations of {sup 99}Tc in the incinerated soils were found to be 0.49Bq/kg(0.77ng/kg)-1.4Bq/kg(2.2ng/kg) with the determination limit of 0.02Bq/kg(0.03ng/kg(0.03ppt)). The results indicate the following findings; 1) the determination of {sup 99}Tc by ICP-MS after strict elimination of the interfering elements by HPLC brings about the improvement in their reliability; 2) the detection limits identified are much lower compared with those by conventional ICP-MS methods because of the concentration of {sup 99}Tc to smaller volume, which is due to only 100{mu}l of samples could be measured by HPLC/ICP-MS system; 3) sample preparation could be simplified because of strict elimination of the interfering elements by HPLC. This research showed that HPLC/ICP-MS system is very effective to determine {sup 99}Tc in environmental samples. (author)

  9. Determination of technetium-99 in soil samples by high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    A new powerful analytical technique viz. high performance liquid chromatography(HPLC) coupled to inductively coupled plasma mass spectrometry(HPLC/ICP-MS) has been applied to the determination of technetium-99(99Tc) in soils as a typical environmental sample. Technetium was enriched in a solution from incinerated soil samples by leaching in HNO3 and passed through 'TEVA resin' column. The solution was injected into HPLC/ICP-MS system to eliminate the interfering elements (i.e. Ru and Mo) and to determine the 99Tc concentration at the same time. The concentrations of 99Tc in the incinerated soils were found to be 0.49Bq/kg(0.77ng/kg)-1.4Bq/kg(2.2ng/kg) with the determination limit of 0.02Bq/kg(0.03ng/kg(0.03ppt)). The results indicate the following findings; 1) the determination of 99Tc by ICP-MS after strict elimination of the interfering elements by HPLC brings about the improvement in their reliability; 2) the detection limits identified are much lower compared with those by conventional ICP-MS methods because of the concentration of 99Tc to smaller volume, which is due to only 100μl of samples could be measured by HPLC/ICP-MS system; 3) sample preparation could be simplified because of strict elimination of the interfering elements by HPLC. This research showed that HPLC/ICP-MS system is very effective to determine 99Tc in environmental samples. (author)

  10. Determination of boron in nuclear materials at subppm levels by high pressure liquid chromatography (HPLC)

    International Nuclear Information System (INIS)

    Experiments were conducted for the determination of boron in U3O8 powder, aluminium metal and milliQ water using dynamically modified Reversed Phase High Pressure Liquid Chromatography (RP-HPLC) and using two precolumn chromogenic agents viz. chromotropic acid and curcumin for complexing boron. The complex was separated from the excess of reagent and determined by HPLC. When present in subppm levels, chromotropic acid was used successfully only for determination boron in water samples. For determination of boron at subppm levels in uranium and aluminium samples, curcumin was used as the precolumn chromogenic agent. The boron curcumin complex (rosocyanin) was formed after extraction of boron with 2-ethyl-l, 3-hexane diol (EHD). The rosocyanin complex was then separated from excess curcumin by displacement chromatography. Linear calibration curves for boron amounts in the range of 0.02 μg to 0.5 μg were developed with correlation coefficients varying from 0.997 to 0.999 and were used for the determination of boron in aluminium and uranium samples. Precision of about 10% was achieved in samples containing less than 1 ppmw of boron. Detection limit of this method is 0.01 μg boron. (author)

  11. Study of HPLC/ICP-MS coupling for the As speciation; Estudo de um acoplamento de HPLC/ICP-MS para a especiacao do As

    Energy Technology Data Exchange (ETDEWEB)

    Cortez, Bruna C.G.; Oliveira, Arno Heeren de [Minas Gerais Univ., Belo Horizonte, MG (Brazil). Dept. de Engenharia Nuclear]. E-mail: brunacortez2004@yahoo.com.br; heeren@nuclear.ufmg.br

    2005-07-01

    Trace metals in the environment may provide benefit or risk to humans, other life forms, and the environment. More robust and information-rich trace and ultra-trace analyses are needed to all adequate risk/benefit assessments. Further, it is no longer adequate to consider only the total trace metal or metalloid, because the impact of elements on ecological systems or biological organisms is not necessarily given by total element concentrations alone. It is necessary to determine the chemical form (species) of the element, primarily the oxidation state or the organometallic nature, because different species of the same metal can range from essential to innocuous to toxic. The actual toxicity levels from different arsenic compounds vary greatly. Inorganic arsenic is considered the most acutely toxic form; arsenite (As{sup III}) is more toxic than arsenate (As{sup V}). The chronic toxicity of arsenic compounds is currently not well understood and is actively being researched. In this study, the viability of the ICP-MS detector coupled with High Performance Liquid Chromatography (HPLC) was tested in 21 water samples from the Das Velhas River, Minas Gerais state, in Brazil. The results showed that the low detection limits and the ease coupling HPLC system - which offers a rugged and versatile separation technique - makes ICP-MS a successful detection method for arsenic speciation analysis. (author)

  12. Assessment of radiochemical purity of [{sup 18}F]fludeoxyglucose by high pressure liquid chromatography (HPLC)

    Energy Technology Data Exchange (ETDEWEB)

    Lacerda, Aline E.; Silva, Juliana B.; Silveira, Marina B.; Ferreira, Soraya Z., E-mail: radiofarmacoscdtn@cdtn.b [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil). Unidade de Pesquisa e Producao de Radiofarmacos

    2011-07-01

    The quality control of [{sup 18}F]fludeoxyglucose ({sup 18}FDG) has received attention due to its increasing clinical use. Although the quality requirements of {sup 18}FDG are established in various pharmacopoeia, the suitability of all testing methods used should be verified under actual conditions of use and documented. The aim of this study was to develop a high pressure liquid chromatography (HPLC) method for radiochemical purity evaluation of {sup 18}FDG, based on pharmacopoeia references, and to verify its suitability for routine quality control in our centre. HPLC analysis was performed with an Agilent HPLC. {sup 18}FDG and impurities were separated on an anion-exchange column by isocratic elution with 0.1 M NaOH as the mobile phase. Detection was accomplished with refractive index and NaI (Tl) scintillation detectors. The flow rate of the mobile phase was set at 0.8 mL/min and the column temperature was kept at 35 deg C. Specificity, linearity, precision and robustness were assessed to verify if the method was adequate for its intended purpose. Retention time of {sup 18}FDG was not affected by the presence of other components of the formulation and a good peak resolution was achieved. The analytical curve of {sup 18}FDG was linear, with a correlation coefficient value of 0.9995. Intraday repeatable precision, reported as the relative standard deviation, was 0.11%. Analytical procedure remained unaffected by small variations in mobile phase flow rate. Results evidenced that HPLC is suitable for radiochemical purity evaluation of {sup 18}FDG, considering operational conditions of our laboratory. (author)

  13. Phosphorus speciation by coupled HPLC-ICPMS: low level determination of reduced phosphorus in natural materials

    Science.gov (United States)

    Atlas, Zachary; Pasek, Matthew; Sampson, Jacqueline

    2015-04-01

    Phosphorus is a geologically important minor element in the Earth's crust commonly found as relatively insoluble apatite. This constraint causes phosphorus to be a key limiting nutrient in biologic processes. Despite this, phosphorus plays a direct role in the formation of DNA, RNA and other cellular materials. Recent works suggest that since reduced phosphorus is considerably more soluble than oxidized phosphorus that it was integrally involved in the development of life on the early Earth and may continue to play a role in biologic productivity to this day. This work examines a new method for quantification and identification of reduced phosphorus as well as applications to the speciation of organo-phosphates separated by coupled HPLC - ICP-MS. We show that reduced phosphorus species (P1+, P3+ and P5+) are cleanly separated in the HPLC and coupled with the ICPMS reaction cell, using oxygen as a reaction gas to effectively convert elemental P to P-O. Analysis at M/Z= 47 producing lower background and flatter baseline chromatography than analyses performed at M/Z = 31. Results suggest very low detection limits (0.05 μM) for P species analyzed as P-O. Additionally we show that this technique has potential to speciate at least 5 other forms of phosphorus compounds. We verified the efficacy of method on numerous materials including leached Archean rocks, suburban retention pond waters, blood and urine samples and most samples show small but detectible levels of reduced phosphorus and or organo-phaospates. This finding in nearly all substances analyzed supports the assumption that the redox processing of phosphorus has played a significant role throughout the history of the Earth and it's presence in the present environment is nearly ubiquitous with the reduced oxidation state phosphorus compounds, phosphite and hypophosphite, potentially acting as significant constituents in the anaerobic environment.

  14. Separation and Detection of Ceramides by HPLC Followed by Evaporative Light-Scattering Detection and Thin Layer Chromatography

    Institute of Scientific and Technical Information of China (English)

    张琳; 周全; 傅学奇; 陈国强

    2002-01-01

    Ceramides are important signaling molecules involved in a variety of cellular processes, including cell growth, differentiation, and apoptosis. Currently, different methods are used for ceramide analysis, some of which are insensitive or cumbersome. This paper described methods utilizing thin layer chromatography (TLC) and high-performance liquid chromatography (HPLC) followed by evaporative light scattering detection (ELSD) to detect ceramide directly in cell extracts without derivatization, which was proved to be efficient and reproducible. Five kinds of ceramides were used as standards. Both TLC and normal-phase HPLC/ELSD results indicate that yeast contains several kinds of ceramides.

  15. 运用HPLC-MS对鸦胆子油自微乳给药系统肠吸收的研究%High-performance Liquid Chromatography Coupled with Mass Spectrometric Method for the Intestinal Absorption Study of Brucea Javanica Oil SMEDDS

    Institute of Scientific and Technical Information of China (English)

    陈瑾瑾; 张懿; 王睿锐; 李盈; 沈琦; 马依然

    2012-01-01

    Objective: To develop a rapid, sensitive and selective high-performance liquid chromatography coupled with mass spectrometric method (HPLC-MS) for detection oleic acid and linoleic acid. Methods: The chromatographic separation was achieved on C18 column at 35℃, with a mobile phase consisting of methanol-distilled water (95:5, v/v) at a flow rate of 0.4 mL/min. An in-vitro diffusion chamber system across isolated rat intestinal membranes was chosen as a model. A self-microemulsifying drug delivery system was used to enhance the intestinal absorption of bruces javanica oil. Results: Oleic acid and linoleic acid were separated with retention times of 10.46 ± 0.02 and 8.55 ± 0.01 min, respectively. A good linear relationship for oleic acid and linoleic acid were in the range of 0.50~50.0 ng/mL(oleic acid) and 5.06~101.2 ng/mL(linoleic acid) , respectively. The mean absolute recoveries of oleic acid and linoleic acid determined in middle concentrations were 97.49± 3.11 % and 105.76± 3.13 % respectively. The coefficients of variation for inter-day and intra-day assay were less than 5 %. The absorption of oleic acid and linoleic acid in bruces javanica oil were 2.8-fold and 4.1-fold enhancement in the presence of the self-microemulsifying drug delivery system respectively, compared with brucea javanica oil alone. Conclusion: HPLC-MS method will be of great utility in routine quality control procedure for the determination of oleic acid and linoleic acid in absorption experiments.%目的:建立高效液相色谱-串联质谱法检测油酸和亚油酸含量的方法,从而对鸦胆子油自微乳给药系统中鸦胆子油的肠吸收进行研究.方法:以甲醇-水(95∶5 v/v)为流动相,流速为0.4 mL/min,柱温为35℃作为高效液相色谱的检测条件.利用大鼠小肠膜建立体外药物扩散体系研究鸦胆子油的肠吸收特性.结果:油酸和亚油酸的保留时间分别为10.46± 0.02和8.55±0.01 min,线性范围分别为0.50~50.0 ng

  16. Development of On-Line High Performance Liquid Chromatography (HPLC-Biochemical Detection Methods as Tools in the Identification of Bioactives

    Directory of Open Access Journals (Sweden)

    Elizabeth Joubert

    2012-03-01

    Full Text Available Biochemical detection (BCD methods are commonly used to screen plant extracts for specific biological activities in batch assays. Traditionally, bioactives in the most active extracts were identified through time-consuming bio-assay guided fractionation until single active compounds could be isolated. Not only are isolation procedures often tedious, but they could also lead to artifact formation. On-line coupling of BCD assays to high performance liquid chromatography (HPLC is gaining ground as a high resolution screening technique to overcome problems associated with pre-isolation by measuring the effects of compounds post-column directly after separation. To date, several on-line HPLC-BCD assays, applied to whole plant extracts and mixtures, have been published. In this review the focus will fall on enzyme-based, receptor-based and antioxidant assays.

  17. INTERFERENCE OF CARBAMYLATED AND ACETYLATED HEMOGLOBINS IN ASSAYS OF GLYCOHEMOGLOBIN BY HPLC, ELECTROPHORESIS, AFFINITY-CHROMATOGRAPHY, AND ENZYME-IMMUNOASSAY

    NARCIS (Netherlands)

    WEYKAMP, CW; PENDERS, TJ; SIEBELDER, CWM; MUSKIET, FAJ; VANDERSLIK, W

    1993-01-01

    In vitro-synthesized carbamylated and acetylated hemoglobins interfered in assays of glycohemoglobin by HPLC and electrophoresis but had no effects on results obtained by affinity chromatography and enzyme immunoassay. Correlations between long-term serum urea concentrations and glycohemoglobin perc

  18. Analysis of Naturally Occurring Phenolic Compounds in Aromatic Plants by RP-HPLC Coupled to Diode Array Detector (DAD) and GC-MS after Silylation

    OpenAIRE

    Charalampos Proestos; Michael Komaitis

    2013-01-01

    The following aromatic plants of Greek origin, Origanum dictamnus (dictamus), Eucalyptus globulus (eucalyptus), Origanum vulgare L. (oregano), Mellisa officinalis L. (balm mint) and Sideritis cretica (mountain tea), were examined for the content of phenolic substances. Reversed phase HPLC coupled to diode array detector (DAD) was used for the analysis of the plant extracts. The gas chromatography-mass spectrometry method (GC-MS) was also used for identification of phenolic compounds after sil...

  19. Analysis of alcohol dehydrogenase inhibitors from Desmodium styracifolium using centrifugal ultrafiltration coupled with HPLC-MS

    Directory of Open Access Journals (Sweden)

    Liu Liangliang

    2015-01-01

    Full Text Available Alcohol dehydrogenase (ADH inhibitors play an important role in the treatment of human methanol or ethylene glycol poisoning and the suppression of acetaldehyde accumulation in alcoholics. In this study, centrifugal ultrafiltration coupled with high performance liquid chromatography-mass spectrometry (HPLC-MS was utilized to screen and identify ADH inhibitors from ethyl acetate extract of Desmosium styracifolium (Osb. Merr. The experiment conditions of centrifugal ultrafiltration were optimized. At the optimum conditions (ADH concentration: 37.5 μg mL-1, incubation time: 90 min, pH: 7.0 and temperature: 15°C, formononetin and aromadendrin were successfully screened and identified from ethyl acetate extract of Desmodium styracifolium. The screening result was verified by ADH inhibition assays. The IC50 values of formononetin and aromadendrin were 70.8 and 84.7 μg mL-1, which were accorded with the binding degrees of them. Aromadendrin was first reported to have inhibitory activity on ADH. This method provided an effective way to screen active compounds from natural products.

  20. Adulteration and cultivation region identification of American ginseng using HPLC coupled with multivariate analysis

    OpenAIRE

    Yu, Chunhao; Wang, Chong-Zhi; Zhou, Chun-Jie; Wang, Bin; Han, Lide; Zhang, Chun-Feng; Wu, Xiao-hui; Yuan, Chun-Su

    2014-01-01

    American ginseng (Panax quinquefolius) is originally grown in North America. Due to price difference and supply shortage, American ginseng recently has been cultivated in northern China. Further, in the market, some Asian ginsengs are labeled as American ginseng. In this study, forty-three American ginseng samples cultivated in the USA, Canada or China were collected and 14 ginseng saponins were determined using HPLC. HPLC coupled with hierarchical cluster analysis and principal component ana...

  1. Comparative analysis of steroidal saponins in four Dioscoreae herbs by high performance liquid chromatography coupled with mass spectrometry.

    Science.gov (United States)

    Guo, Long; Zeng, Su-Ling; Zhang, Yu; Li, Ping; Liu, E-Hu

    2016-01-01

    Steroidal saponins, which exhibit multiple pharmacological effects, are the major bioactive constituents in herbal medicines from Dioscoreae species. In this study, a sensitive method based on high performance liquid chromatography-mass spectrometry (HPLC-MS) was established and validated for qualitative and quantitative analysis of steroidal saponins in four Dioscoreae herbs including Dioscoreae Nipponica Rhizome (DNR) and Dioscoreae Hypoglaucae Rhizome (DHR), Dioscoreae Spongiosae Rhizome (DSR) and Dioscoreae Rhizome (DR). A total of eleven steroidal saponins were identified by high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC-QTOF/MS). Furthermore, seven major steroidal saponins was simultaneous quantified using a high performance liquid chromatography coupled with triple quadrupole mass spectrometry (HPLC-QQQ/MS). The qualitative and quantitative analysis results indicated that the chemical composition of DNR, DHR and DSR samples exhibited a high level of global similarity, while the ingredients in DR varied greatly from the other three herbs. Moreover, principal component analysis (PCA) and hierarchical clustering analysis (HCA) were performed to compare and discriminate the Dioscoreae herbs based on the quantitative data. The results demonstrated the qualitative and quantitative analysis of steroidal saponins based on HPLC-MS is a feasible method for quality control of Dioscoreae herbs. PMID:26344383

  2. Determination of Benzene, Toluene and Xylene (BTX Concentrations in Air Using HPLC Developed Method Compared to Gas Chromatography

    Directory of Open Access Journals (Sweden)

    Abdulrahman Bahrami

    2011-01-01

    Full Text Available A new method for analysis of benzene, toluene, and xylene (BTX using High Performance Liquid Chromatography-UV detection (HPLC-UV is described and compared to the gas chromatography (GC method. A charcoal adsorption tube connected to a small pump was used to obtain samples from an atmosphere chamber standard. Samples were extracted with methanol and analyzed by HPLC-UV. Chromatography was isocratic in a mobile phase consisting of water-methanol (30-70. The flow rate was set at 1 ml/min. The analyses were completely separated and were quantified using both methods. The results demonstrated no statistically significant differences between BTX concentrations between the two analytical methods with a correlation coefficient of 0.98-0.99. The GC method provided higher sensitivity than HPLC, but the HPLC determination of BTX were applicable to real samples because its sensivity was lower than the thershold limit recommended by the American Conference of Governmental Industrial Hygienist (ACGIH for an 8-hour workday.

  3. Electrochemical detection coupled with high-performance liquid chromatography in pharmaceutical and biomedical analysis: a mini review.

    Science.gov (United States)

    Wang, Chengyin; Xu, Jianyun; Zhou, Guiyou; Qu, Qishu; Yang, Gongjun; Hu, Xiaoya

    2007-08-01

    Recent advances in electrochemical detection techniques coupled with high-performance liquid chromatography (HPLC-ECD) in pharmaceutical and biomedical analysis are reviewed. ECD classification and modes including common amperometric, coulometric, conductimetric, and potentiometric detector, are outlined and the some typical examples of determinations in pharmaceutical and biomedical analysis are described. The electrochemical detection system can offer superior merits over other detectors commonly used with HPLC. These techniques have great potential owing to their prominent characteristics in high-throughput screening procedures of drugs in various matrices. Fundamental 67 references from last 5 years related with a field are cited in this review. PMID:17979637

  4. Determination of selenomethionine, selenocysteine, and inorganic selenium in eggs by HPLC-inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lipiec, Elzbieta; Siara, Grzegorz [CNRS/UPPA, Laboratoire de Chimie Analytique Bio-Inorganique et Environnement, Pau (France); Warsaw University of Technology, Warsaw (Poland); Bierla, Katarzyna; Ouerdane, Laurent; Szpunar, Joanna [CNRS/UPPA, Laboratoire de Chimie Analytique Bio-Inorganique et Environnement, Pau (France)

    2010-05-15

    A method for the simultaneous determination of selenomethionine (SeMet), selenocysteine (SeCys), and selenite [Se(IV)] in chicken eggs was developed. A sample preparation protocol including defatting, protein denaturation, and carbamidomethylation was optimized in order to achieve complete protein digestion and to avoid SeCys losses. Quantification was carried out by reversed-phase HPLC-inductively coupled plasma mass spectrometry (ICP MS) after quantitative isolation of the selenium-containing fraction by size-exclusion liquid chromatography. The detection limits were 0.06, 0.003, and 0.01 {mu}g g{sup -1} (dry weight) for SeCys, Se(IV) and SeMet, respectively, and the precision was 5-10%. The end products of carbamidomethylation of the different selenium species were identified for the first time by electrospray QTOF MS after custom-designed 2D HPLC purification. Differences in selenium speciation in egg yolk and white were highlighted, the yolk containing more SeCys and the white more SeMet. An insight into selenium bioaccessibility in eggs was obtained by digestion with simulated gastric and gastrointestinal juices and size-exclusion HPLC-ICP MS. (orig.)

  5. Analysis of Flavonoids in Lotus (Nelumbo nucifera) Leaves and Their Antioxidant Activity Using Macroporous Resin Chromatography Coupled with LC-MS/MS and Antioxidant Biochemical Assays

    OpenAIRE

    Ming-Zhi Zhu; Wei Wu; Li-Li Jiao; Ping-Fang Yang; Ming-Quan Guo

    2015-01-01

    Lotus (Nelumbo nucifera) leaves, a traditional Chinese medicinal herb, are rich in flavonoids. In an effort to thoroughly analyze their flavonoid components, macroporous resin chromatography coupled with HPLC-MS/MS was employed to simultaneously enrich and identify flavonoids from lotus leaves. Flavonoids extracted from lotus leaves were selectively enriched in the macroporous resin column, eluted subsequently as fraction II, and successively subjected to analysis with the HPLC-MS/MS and bio...

  6. Arsenic speciation in soil using high performance liquid chromatography/inductively coupled plasma/mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bass, D.A.; Yaeger, J.S.; Parish, K.J.; Crain, J.S.; Kiely, J.T.; Gowdy, M.J. [Argonne National Lab., IL (United States); Mohrman, G.B.; Besmer, M.G. [Rocky Mountain Arsenal, Commerce City, CO (United States)

    1996-08-01

    A method has been developed to identify and quantify As(III), As(V), and organoarsenic compounds in soil samples from the Rocky Mountain Arsenal (RMA) by high performance liquid chromatography/inductively coupled plasma/mass spectrometry (HPLC/ICP/MS). The soils were extracted using tetrabutylammonium hydroxide (TBAH) and sonication. The percentages of As(III), As(V), and organoarsenic species extracted from soil samples were 30, 50, and 100 respectively. The arsenic species were not altered during the extraction process. They were separated by reversed-phase, ion-pairing, HPLC using a microbore Inertsil-ODS{trademark} column. The HPLC column effluent was introduced into an ICP/MS system using a direct injection nebulizer (DIN). Detection limits of less than 1 pg were readily obtained for each arsenic species. Internal standards are recommended to increase accuracy and precision. Soil samples spiked with arsenic oxide, sodium arsenate, dimethylarsinic acid (DMAA), and chlorovinyl arsenious acid (CVAA) were extracted, identified and quantified with the HPLC/ICP/MS system. The soil samples were analyzed in support of the analytical needs of a thermal desorption treatability study being conducted at the RMA.

  7. High performance thin layer chromatography (HPTLC) and high performance liquid chromatography (HPLC) for the qualitative and quantitative analysis of Calendula officinalis-advantages and limitations.

    Science.gov (United States)

    Loescher, Christine M; Morton, David W; Razic, Slavica; Agatonovic-Kustrin, Snezana

    2014-09-01

    Chromatography techniques such as HPTLC and HPLC are commonly used to produce a chemical fingerprint of a plant to allow identification and quantify the main constituents within the plant. The aims of this study were to compare HPTLC and HPLC, for qualitative and quantitative analysis of the major constituents of Calendula officinalis and to investigate the effect of different extraction techniques on the C. officinalis extract composition from different parts of the plant. The results found HPTLC to be effective for qualitative analysis, however, HPLC was found to be more accurate for quantitative analysis. A combination of the two methods may be useful in a quality control setting as it would allow rapid qualitative analysis of herbal material while maintaining accurate quantification of extract composition. PMID:24880991

  8. Characterization of Arsenic Biotransformation Products from an Open Anaerobic Degradation of Fucus distichus by Hydride Generation Gas Chromatography Atomic Absorption Spectrometry and High Performance Liquid Chromatography Inductively Coupled Plasma Mass Spectrometry

    OpenAIRE

    Abiodun A. Ojo; Onasanya, Amos

    2013-01-01

    This work reports on the isolation and determination of biotransformation products obtained from the organoarsenic compounds that are present in Fucus distichus when it was subjected to an open anaerobic decomposition by using the Hydride Generation Gas Chromatography Atomic Absorption Spectrometry (HG-GC-AAS) and High Performance Liquid Chromatography Inductively Coupled Plasma Mass Spectrometry (HPLC-ICP-MS). The seaweed and filtrate residues obtained from the open anaerobic degradation pro...

  9. Capacitively coupled contactless conductivity detection and sequential injection analysis in capillary electrophoresis and capillary electro-chromatography

    OpenAIRE

    Mai, Thanh Duc

    2011-01-01

    This thesis focuses on the applications of capacitively coupled contactless conductivity detection (C4D) in capillary electrophoresis (CE) hybridized with high-performance liquid chromatography (HPLC), i.e. in capillary electrochromatography and pressure-assisted capillary electrophoresis, as well as on the development and applications of an extension of CE-C4D with sequential injection analysis (SIA). At first, the in-house built C4D was used for electro-chromatographic determinations of...

  10. Analysis of ochratoxin A in pig tissues using high pressure liquid chromatography (HPLC) and liquid chromatography tandem mass spectrometry (LC/MS/MS) as confirmative methods

    OpenAIRE

    Milićević Dragan R.; Jurić Verica B.; Stefanović Srđan M.; Vesković-Moračanin Slavica M.; Janković Saša I.

    2009-01-01

    Two different analytical methods for the determination and confirmation of ochratoxin A (OTA) in blood serum, kidney and liver of pigs have been compared. Sample clean-up was based on liquid-liquid phase extraction. The detection of OTA was accomplished with high-performance liquid chromatography (HPLC) combined either with fluorescence detection (FL) or electro spray ionization (ESI+) tandem mass spectrometry (MS-MS). Comparative method evaluation was based on the investigation of 82 samples...

  11. Development and validation of methodology for technetium-99m radiopharmaceuticals using high performance liquid chromatography (HPLC)

    International Nuclear Information System (INIS)

    Radiopharmaceuticals are compounds, with no pharmacological action, which have a radioisotope in their composition and are used in Nuclear Medicine for diagnosis and therapy of several diseases. In this work, the development and validation of an analytical method for 99mTc-HSA, 99mTc-EC, 99mTc-ECD and 99mTc-Sestamibi radiopharmaceuticals and for some raw materials were carried out by high performance liquid chromatography (HPLC). The analyses were performed in a Shimadzu HPLC equipment, LC-20AT Prominence model. Some impurities were identified by the addition of a reference standard substance. Validation of the method was carried out according to the criteria defined in RE n. 899/2003 of the National Sanitary Agency (ANVISA). The results for robustness of the method showed that it is necessary to control flow rate conditions, sample volume, pH of the mobile phase and temperature of the oven. The analytical curves were linear in the concentration ranges, with linear correlation coefficients (r2) above 0.9995. The results for precision, accuracy and recovery showed values in the range of 0.07-4.78%, 95.38-106.50% and 94.40-100.95%, respectively. The detection limits and quantification limits varied from 0.27 to 5.77 μg mL-1 and 0.90 to 19.23 μg mL-1, respectively. The values for HAS, EC, ECD and MIBI in the lyophilized reagents were 8.95; 0.485; 0.986 and 0.974 mg L-1, respectively. The mean radiochemical purity for 99mTc-HSA, 99mTc-EC, 99mTc-ECD and 99mTc-Sestamibi was (97.28 ± 0.09)%, (98.96 ± 0.03)%, (98.96 ± 0.03)% and (98.07 ± 0.01)%, respectively. All the parameters recommended by ANVISA were evaluated and the results are below the established limits. (author)

  12. Preparative Isolation of Polar Antioxidant Constituents from Abies koreana Using Centrifugal Partition Chromatography Guided by DPPH center dot-HPLC Experiment

    NARCIS (Netherlands)

    Jeon, Je-Seung; Kim, Ji Hoon; Park, Chae Lee; Kim, Chul Young

    2015-01-01

    Preparative separation of antioxidant constituents from the leaves of Abies koreana Wilson (Pinaceae) was performed by centrifugal partition chromatography (CPC) with a two-phase solvent system of ethyl acetate-isopropanol-water (9:1:10, v/v) target-guided by DPPH•-HPLC experiment. In DPPH•-HPLC exp

  13. Evaluation of aminoacids in irradiated beans (Vigna unguiculata (L.) Walp) by high performance liquid chromatography (HPLC)

    International Nuclear Information System (INIS)

    Fradinho-bean (Vigna unguiculata (L.) Walp) is originated from Africa and is known in Brazil as 'caupi', 'corda' or 'macassar'. It is grown in the interior of Northeast Brazil (semi-arid region) and can be found in parts of the North, being one of the most important components of people's diet in those regions. The Northeast area produces around 429,375 ton of fradinho-bean per year. Leguminous plants are very important sources of proteins, vitamins, carbohydrates and minerals. This kind of bean is an excellent source of proteins (around 23- 25% of its nutritional content), being superior to regular beans (Phaseolus vulgaris). The irradiation process is an alternative to avoid post-harvesting losses, without changing the nutritional value of food. This study has the objective to evaluate the effect of different gamma irradiation doses (0.0; 0.5; 1.0; 2.5; 5.0 and 10.0 kGy) on aminoacid content of fradinho-bean by high performance liquid chromatography (HPLC) and the accompanying of the grains during storage time of 6 months. After irradiation, the bean grains went through a milling process in order to make flour for posterior extraction. A liquid chromatographer Waters, model Alliance 2695, with fluorescent detector Waters 2475, having a mobile phase with gradient elution of sodium acetate. acetonitrile and Milli-Q water, was employed. The flux used was 1 mL/min and the injection volume of 10 μL. The column (C 18 150.0 x 3.9 mm) was kept at 36 deg C. The results show that gamma irradiation is a promise process for fradinho bean during conservation storage time of 6 months, until the dose of 10.0 kGy. Even the most radio-sensitive aminoacids like aromatics and basic lateral chains were preserved. (author)

  14. Evaluation of aminoacids in irradiated beans (Vigna unguiculata (L.) Walp) by high performance liquid chromatography (HPLC)

    Energy Technology Data Exchange (ETDEWEB)

    Lima, Keila S. Cople; Souza, Luciana B.; Coelho, Maysa J.; Lima, Antonio L. Santos; Hernandes, Nilber K. [Instituto Militar de Engenharia (IME), Rio de Janeiro, RJ (Brazil). Secao de Engenharia Nuclear]. E-mail: keila@ime.eb.br; Godoy, Ronoel L.O. [EMBRAPA Agroindustria de Alimentos, Rio de Janeiro, RJ (Brazil)]. E-mail: ronoel@ctaa.embrapa.br

    2007-07-01

    Fradinho-bean (Vigna unguiculata (L.) Walp) is originated from Africa and is known in Brazil as 'caupi', 'corda' or 'macassar'. It is grown in the interior of Northeast Brazil (semi-arid region) and can be found in parts of the North, being one of the most important components of people's diet in those regions. The Northeast area produces around 429,375 ton of fradinho-bean per year. Leguminous plants are very important sources of proteins, vitamins, carbohydrates and minerals. This kind of bean is an excellent source of proteins (around 23- 25% of its nutritional content), being superior to regular beans (Phaseolus vulgaris). The irradiation process is an alternative to avoid post-harvesting losses, without changing the nutritional value of food. This study has the objective to evaluate the effect of different gamma irradiation doses (0.0; 0.5; 1.0; 2.5; 5.0 and 10.0 kGy) on aminoacid content of fradinho-bean by high performance liquid chromatography (HPLC) and the accompanying of the grains during storage time of 6 months. After irradiation, the bean grains went through a milling process in order to make flour for posterior extraction. A liquid chromatographer Waters, model Alliance 2695, with fluorescent detector Waters 2475, having a mobile phase with gradient elution of sodium acetate. acetonitrile and Milli-Q water, was employed. The flux used was 1 mL/min and the injection volume of 10 {mu}L. The column (C 18 150.0 x 3.9 mm) was kept at 36 deg C. The results show that gamma irradiation is a promise process for fradinho bean during conservation storage time of 6 months, until the dose of 10.0 kGy. Even the most radio-sensitive aminoacids like aromatics and basic lateral chains were preserved. (author)

  15. Design and implementation of an automated liquid-phase microextraction-chip system coupled on-line with high performance liquid chromatography

    DEFF Research Database (Denmark)

    Li, Bin; Petersen, Nickolaj J.; Payán, María D Ramos;

    2014-01-01

    An automated liquid-phase microextraction (LPME) device in a chip format has been developed and coupled directly to high performance liquid chromatography (HPLC). A 10-port 2-position switching valve was used to hyphenate the LPME-chip with the HPLC autosampler, and to collect the extracted...... analytes, which then were delivered to the HPLC column. The LPME-chip-HPLC system was completely automated and controlled by the software of the HPLC instrument. The performance of this system was demonstrated with five alkaloids i.e. morphine, codeine, thebaine, papaverine, and noscapine as model analytes....... The composition of the supported liquid membrane (SLM) and carrier was optimized in order to achieve reasonable extraction performance of all the five alkaloids. With 1-octanol as SLM solvent and with 25mM sodium octanoate as anionic carrier, extraction recoveries for the different opium alkaloids...

  16. Adulteration and cultivation region identification of American ginseng using HPLC coupled with multivariate analysis.

    Science.gov (United States)

    Yu, Chunhao; Wang, Chong-Zhi; Zhou, Chun-Jie; Wang, Bin; Han, Lide; Zhang, Chun-Feng; Wu, Xiao-Hui; Yuan, Chun-Su

    2014-10-01

    American ginseng (Panax quinquefolius) is originally grown in North America. Due to price difference and supply shortage, American ginseng recently has been cultivated in northern China. Further, in the market, some Asian ginsengs are labeled as American ginseng. In this study, forty-three American ginseng samples cultivated in the USA, Canada or China were collected and 14 ginseng saponins were determined using HPLC. HPLC coupled with hierarchical cluster analysis and principal component analysis was developed to identify the species. Subsequently, an HPLC-linear discriminant analysis was established to discriminate cultivation regions of American ginseng. This method was successfully applied to identify the sources of 6 commercial American ginseng samples. Two of them were identified as Asian ginseng, while 4 others were identified as American ginseng, which were cultivated in the USA (3) and China (1). Our newly developed method can be used to identify American ginseng with different cultivation regions. PMID:25044150

  17. Modernization of Chinese herbal compound and the high performance liquid chromatography tandem mass spectrometry (HPLC-MS)

    Institute of Scientific and Technical Information of China (English)

    LI Wen-lan; SUN Zhi; DU Juan

    2008-01-01

    Chinese herbal compound is playing an important role on curing human diseases. And it has been a trend that Chinese herbal compound is being used all over the world in 21 century. However, our Chinese herbal compound is facing serious challenge for the lack of canonical system of quality criterion for Chinese herbal compound so it has been a urgent problem to set up the quality control standards and reveal therapeutic basis of Chinese herbal compound. In order to give full play to the advantages of Chinese herbal compound, modern scientific and technological is used to research of Chinese herbal compound, especially the high performance liquid chromatography tandem mass spectrometry(HPLC-MS), because it is high sensitive, rapid, and obtain more information. It is very necessary that HPLC-MS is uesed to elucidate the effective components of basic substances of Chinese Herbal Compound, and endow traditional Chinese medicine with modern scientific connotation.

  18. Analysis and characterization. HPLC-ICP-MS coupling and application to speciation; Analyse et caracterisation. Couplage HPLC-ICP-MS et application a la speciation

    Energy Technology Data Exchange (ETDEWEB)

    Potin-Gautier, M. [Pau Univ., 64 (France); Casiot, C. [Pau Univ., Chimie et Microbiologie de l' Eau, 64 (France)

    2001-12-01

    In this work, the general principles of the HPLC-ICP-MS coupling technique are presented (chromatographic modes, types of columns used, ICP-MS technology) as well as the constraints due to the coupling (introduction systems of the eluant in the ICP-MS, problems inherent in the moving phase...). The last part deals with the main applications of the HPLC-ICP-MS. It concerns particularly the speciation of trace elements: that is to say the separation and quantification of their different chemical states in a given medium. Among the application fields is the environment (pollution control). (O.M.)

  19. Fast HPLC method using ion-pair and hydrophilic interaction liquid chromatography for determination of phenylephrine in pharmaceutical formulations.

    Science.gov (United States)

    Dousa, Michal; Gibala, Petr

    2010-01-01

    A rapid procedure based on a direct extraction and HPLC determination with fluorescence detection of phenylephrine in pharmaceutical sachets that include a large excess of paracetamol (65 + 1, w/w), ascorbic acid (5 + 1, w/w), and other excipients (aspartame and sucrose) was developed and validated. The final optimized chromatographic method for ion-pair chromatography used an XTerra RP18 column, 3 microm particle size, 50 x 3.0 mm id. The mobile phase consisted of a mixture of acetonitrile and buffer (10 mM sodium octane-1-sulfonate, adjusted with H3PO4 to pH 2.2; 200 + 800, v/v), with a constant flow rate of 0.3 mL/min. The separation was carried out at 30 degrees C, and the injection volume was 3 microL. Fluorescence detection was performed at excitation and emission wavelengths of 275 and 310 nm, respectively. The mobile phase parameters, such as the organic solvent fraction (acetonitrile) in mobile phase as an organic modifier, the concentration of sodium octane-1-sulfonate as a counter-ion, temperature, and pH of mobile phase, were studied. As an alternative to ion-pair chromatography, hydrophilic interaction liquid chromatography (HILIC) was investigated using a Luna HILIC column, 3 microm, 100 x 4.6 mm id. The mobile phase consisted of acetonitrile and buffer (5 mM potassium dihydrogen phosphate, adjusted with H3PO4 to pH 2.5; 750 + 250, v/v) at a flow rate of 0.8 mL/min. The separation was carried out at 25 degrees C, and the injection volume was 5 microL. The proposed method has an advantage of a very simple sample pretreatment, and is much faster than the currently utilized HPLC methods using gradient elution and UV detection. Commercial samples of sachets were successfully analyzed by the proposed HPLC method. PMID:21140654

  20. Lead speciation in rainwater by isotope dilution-high performance liquid chromatography-inductively coupled plasma-mass spectrometry

    Science.gov (United States)

    Ebdon, Les; Hill, Steve J.; Rivas, Cristina

    1998-02-01

    A new method for lead speciation in rainwater by isotope dilution analysis (IDA) using directly coupled high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) is described and demonstrated. Samples containing trimethyllead (TML) chloride and triethyllead (TEL) chloride in the presence of large amounts of inorganic lead have been analysed by HPLC-ICP-MS using reverse phase ion-pairing chromatography. The detection limit for the procedure is 3 ng g -1 for TML as Pb and 14 ng g -1 for TEL as Pb, with a linear range exceeding 1000 ng g -1 and a relative standard deviation of 4% for TML in the range 50-1000 ng g -1. TML chloride isotopically enriched in the stable 206 isotope was prepared and used to enhance the accuracy of the method by isotope dilution analysis. The IDA-HPLC-ICP-MS method was successfully applied to the analysis of a sample of artificial rainwater used in a collaborative study.

  1. On-line coupled high performance liquid chromatography-gas chromatography for the analysis of contamination by mineral oil. Part 1: method of analysis.

    Science.gov (United States)

    Biedermann, Maurus; Grob, Koni

    2012-09-14

    For the analysis of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH), on-line coupled high performance liquid chromatography-gas chromatography-flame ionization detection (HPLC-GC-FID) offers important advantages: it separates MOSH and MOAH in robust manner, enables direct injection of large aliquots of raw extracts (resulting in a low detection limit), avoids contamination of the sample during preparation and is fully automated. This review starts with an overview of the technology, particularly the fundamentals of introducing large volumes of solvent into GC, and their implementation into various transfer techniques. The main part deals with the concepts of MOSH and MOAH analysis, with a thorough discussion of the choices made. It is followed by a description of the method. Finally auxiliary tools are summarized to remove interfering components, enrich the sample in case of a high fat content and obtain additional information about the MOSH and MOAH composition. PMID:22770383

  2. Metabolite Profile of Salidroside in Rats by Ultraperformance Liquid Chromatography Coupled with Quadrupole Time-of-Flight Mass Spectrometry and High-Performance Liquid Chromatography Coupled with Quadrupole-Linear Ion Trap Mass Spectrometry.

    Science.gov (United States)

    Hu, Zhiwei; Wang, Ziming; Liu, Yong; Wu, Yan; Han, Xuejiao; Zheng, Jian; Yan, Xiufeng; Wang, Yang

    2015-10-21

    In the present work, the salidroside metabolite profile in rat urine was investigated, and subsequently the metabolic pathways of salidroside were proposed. After administrations of salidroside at an oral dose of 100 or 500 mg/kg, rat urine samples were collected and pretreated with methanol to precipitate the proteins. The pretreated samples were analyzed by an Acquity ultraperformance liquid chromatography (UPLC) coupled with an HSS T3 column and detected by quadrupole time-of-flight mass spectrometry (Q-TOF-MS) or high-performance liquid chromatography coupled with hybrid triple-quadrupole linear ion trap mass spectrometry (HPLC/Q-trap-MS). A total of eight metabolites were detected and identified on the basis of the characteristics of their protonated ions in the urine samples. The results elucidated that salidroside was metabolized via glucuronidation, sulfation, deglycosylation, hydroxylation, methylation, and dehydroxylation pathways in vivo. PMID:26461036

  3. Melanin determination by high performance liquid chromatography (HPLC) for K. marxianus

    Science.gov (United States)

    Ultraviolet light (UV) mutated K. marxianus was found to turn dark brown during a growth assay. This brown color was hypothesized to be melanin overproduction influenced by the UV exposure. Cell cultures were oxidized and HPLC analyzed to determine melanin concentrations. The resulting melanin con...

  4. Comparison of standard and reaction cell inductively coupled plasma mass spectrometry in the determination of chromium and selenium species by HPLC-ICP-MS

    International Nuclear Information System (INIS)

    Elemental speciation is becoming a common analytical procedure for geochemical investigations. The various redox species of environmentally relevant metals can have vastly different biogeochemical properties, including sorption, solubility, bioavailability, and toxicity. The use of high performance liquid chromatography (HPLC) coupled to elemental specific detectors, such as inductively coupled plasma mass spectrometry (ICP-MS), has become one of the most important speciation methods employed. This is due to the separation versatility of HPLC and the sensitive and selective detection capabilities of ICP-MS. The current study compares standard mode ICP-MS to recently developed reaction cell (RC) ICP-MS, which has the ability to remove or reduce many common polyatomic interferences that can limit the ability of ICP-MS to quantitate certain analytes in complex matrices. Determination of chromium and selenium redox species is achieved using ion-exchange chromatography with elemental detection by standard and RC-ICP-MS, using various chromium and selenium isotopes. In this study, method performance and detection limits for the various permutations of the method (isotope monitored or ICP-MS detection mode) were found to be comparable and generally less than 1 μg L-1. The method was tested on synthetic laboratory samples, surface water, groundwater, and municipal tap water matrices

  5. Comparison of standard and reaction cell inductively coupled plasma mass spectrometry in the determination of chromium and selenium species by HPLC-ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Bednar, A.J. [U.S. Army Engineer Research and Development Center, Environmental Laboratory, 3909 Halls Ferry Rd., Vicksburg, MS 39180 (United States)], E-mail: Anthony.J.Bednar@erdc.usace.army.mil; Kirgan, R.A.; Jones, W.T. [U.S. Army Engineer Research and Development Center, Environmental Laboratory, 3909 Halls Ferry Rd., Vicksburg, MS 39180 (United States)

    2009-01-19

    Elemental speciation is becoming a common analytical procedure for geochemical investigations. The various redox species of environmentally relevant metals can have vastly different biogeochemical properties, including sorption, solubility, bioavailability, and toxicity. The use of high performance liquid chromatography (HPLC) coupled to elemental specific detectors, such as inductively coupled plasma mass spectrometry (ICP-MS), has become one of the most important speciation methods employed. This is due to the separation versatility of HPLC and the sensitive and selective detection capabilities of ICP-MS. The current study compares standard mode ICP-MS to recently developed reaction cell (RC) ICP-MS, which has the ability to remove or reduce many common polyatomic interferences that can limit the ability of ICP-MS to quantitate certain analytes in complex matrices. Determination of chromium and selenium redox species is achieved using ion-exchange chromatography with elemental detection by standard and RC-ICP-MS, using various chromium and selenium isotopes. In this study, method performance and detection limits for the various permutations of the method (isotope monitored or ICP-MS detection mode) were found to be comparable and generally less than 1 {mu}g L{sup -1}. The method was tested on synthetic laboratory samples, surface water, groundwater, and municipal tap water matrices.

  6. High-performance liquid chromatography on-line coupled to high-field NMR and mass spectrometry for structure elucidation of constituents of Hypericum perforatum L

    DEFF Research Database (Denmark)

    Hansen, S. H.; Jensen, A. G.; Cornett, Claus;

    1999-01-01

    The on-line separation and structure elucidation of naphthodianthrones, flavonoids, and other constituents of an extract from Hypericum perforatum L, using high performance liquid chromatography (HPLC) coupled on-line with ultraviolet-visible, nuclear magnetic resonance (NMR), and mass spectrometry...... (MS) is described. A conventional reversed-phase HPLC system using ammonium acetate as the buffer substance in the eluent tvas used, and proton NMR spectra were obtained on a 500 MHz NMR instrument. The MS and MS/MS analyses were performed using negative electrospray ionization, In the present study...

  7. Separation and identification of moxifloxacin impurities in drug substance by high-performance liquid chromatography coupled with ultraviolet detection and Fourier transform ion cyclotron resonance mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    Cai Sheng Wu; Zhi Xin Jia; Bao Ming Ning; Jin Lan Zhang; Song Wu

    2012-01-01

    In this paper,a high-performance liquid chromatography coupled with ultraviolet detection and Fourier transform-ion cyclotron resonance mass spectrometry (HPLC-UV/FTICRMS) method was described for the investigation of impurity profile in moxifloxacin (MOX) drug substance and chemical reference substance.Ten impurities were detected by HPLC-UV,while eight impurities were identified by using the high accurate molecular mass combined with multiple-stage mass spectrometric data and fragmentation rules.In addition,to our knowledge,five impurities were founded for the first time in MOX drug substance.

  8. Report on three aliphatic dimethylarsinoyl compounds as common minor constituents in marine samples. An investigation using high-performance liquid chromatography inductively coupled plasma mass spectrometry and electrospray ionisation tandem mass spectrometry

    DEFF Research Database (Denmark)

    Sloth, Jens Jørgen; Larsen, Erik Huusfeldt; Julshamn, K.

    2005-01-01

    chromatography/inductively coupled plasma mass spectrometry (HPLC/ICPMS). Eluate fractions from the HPLC/ICPMS analyses containing the compounds in question were collected and subjected to analysis by electrospray ionisation tandem mass spectrometry (ESI-MS/MS), which provided supportive evidence for the...... DMAA and DMAE supports a proposed biosynthesis of arsenobetaine (AB) from dimethylarsinoylribosides. Alternative proposals, which explain the presence of the compounds in marine samples, are addressed briefly in the paper....

  9. Simultaneous determination of the major isosteroidal alkaloids and their glucosides in the bulbs of Fritillaria by high performance liquid chromatography coupled with evaporative light scattering detection%HPLC-ELSD法测定贝母中异甾类生物碱及糖苷类成分的含量

    Institute of Scientific and Technical Information of China (English)

    李萍; 曾令杰; 李松林; 毕志明; 林鸽

    2004-01-01

    目的建立同时测定贝母中5种异甾类生物碱--peimissine, imperialine, sinpeinine A, imperialine-3β-glucoside和yibeinoside A含量的HPLC分析方法.方法 C18柱;流动相:乙腈-水(含0.1%二乙胺);梯度洗脱,流速1.0 mL·min-1;检测器:Alltech 500蒸发光散射检测器(ELSD).结果线性范围为peimissine 13.1~288.2 mg·L-1(r2=0.997 5), imperialine-3β-glucoside 7.7~169.4 mg·L-1 (r2=0.999 3), yibeinoside A 7.3~160.6 mg·L-1 (r2=0.999 7), imperialine 16.5~363.0 mg·L-1 (r2=0.999 2), sinpeinine A 8.7~191.4 mg·L-1 (r2=0.994 2). 5个化合物的精密度和重现性RSD均<5%.结论本方法简便、有效、可行,可用于贝母中5种异甾类生物碱的含量测定.%Aim To establish an HPLC-ELSD method for the simultaneous determination of five major bioactive isosteroidal alkaloids and gluco-alkaloids in the bulbs of Fritillaria namely peimissine, imperialine, sinpeinine A, imperialine-3β-glucoside and yibeinoside A. Methods A Nova-Pak C18 column (150 mm×3.9 mm ID) was used. The chromatography was carried out with a linear gradient programming. The mobile phase was acetonitrile-water (containing 0.1% diethylamine) and the flow rate was 1.0 mL*min-1. Results The linear range of peimissine was 13.1-288.2 mg*L-1 (r2=0.997 5), imperialine-3β-glucoside 7.7-169.4 mg·L-1 (r2=0.999 3), yibeinoside A 7.3-160.6 mg·L-1 (r2=0.999 7), imperialine 16.5-363.0 mg·L-1 (r2=0.999 2), sinpeinine A 8.7-191.4 mg·L-1 (r2=0.994 2). Conclusion The method is accurate with overall intra- and inter-day variation less than 5% and recovery more than 95%. The method was successfully applied to analyze five major bioactive alkaloids and gluco-alkaloids in three Fritillaria bulbs.

  10. Examples of high performance liquid chromatography (HPLC) application in marine ecology studies in the northern Adriatic

    OpenAIRE

    Flander Putrle, Vesna

    2010-01-01

    Photosynthetic pigments have proved to be useful biomarkers of the abundance, composition and physiological status of the phytoplankton biomass in the marine environment. Using HPLC pigment analysis, we determined phytoplankton community structure in three different marine environments: in the area of a fish farm, in the area of sewage outlets, and in the mucilaginous aggregates. At the reference site we observed seasonal changes with prevalence of fucoxanthin-containing phytoplankton (i.e. d...

  11. Oxidative damage in human DNA and urine analyzed by HPLC- electrochemical detection (HPLC-EC) and gas chromatography-mass spectrometry (GC/MS)

    International Nuclear Information System (INIS)

    Reactive oxygen species (ROS) may lead to the oxidative DNA damage representing an early step in chemical carcinogenesis and the progression of tumors. The oxidative stress has been suggested as a possible mechanism of non-genotoxic chemical carcinogenesis. The oxidation to DNA may include modified bases, strand breaks and AP-sites. We have studied oxidative DNA damage using 7,8-dihydro-8-oxodeoxyguanosine (8-oxodG) and thymine glycol (TG) as biomarkers for occupational exposure to diesel exhaust. DNA was extracted from lymphocyte of 19 exposed bus garage and waste collection workers, and 18 controls. The measurement of 8-oxodG was carried out by HPLC coupled with an EC detector. High individual variations of 8-oxodG levels were observed, however, the mean 8-oxodG obtained from the exposed workers (4.8/10E5 dG) was not statistically different from the control persons (4.1/10E5 dG). Thymine glycol (TG) in urine of exposed and control persons was analyzed with TG-d4 as an internal standard. Five ml of urine was treated with the affinity column and C18 cartridges, then HPLC separations were processed. The fractions containing endogenous TG and the deuterated internal standard were derivatized with BSTFA and acetonitrile (4/1). The GC/MS analysis was performed with JMS-700 GC/MS of JEOL by the high resolution SIM mode. The TG levels in human urine were low and the purification procedure of urine samples needs to be further developed. Supported by Academy of Finland

  12. Ultra-high efficiency moving wire combustion interface for on-line coupling of HPLC

    OpenAIRE

    Thomas, Avi T.; Ognibene, Ted; Daley, Paul; Turteltaub, Ken; Radousky, Harry; Bench, Graham

    2011-01-01

    We describe a 100% efficient moving-wire interface for on-line coupling of high performance liquid chromatography which transmits 100% of carbon in non-volatile analytes to a CO2 gas accepting ion source. This interface accepts a flow of analyte in solvent, evaporates the solvent, combusts the remaining analyte, and directs the combustion products to the instrument of choice. Effluent is transferred to a periodically indented wire by a coherent jet to increase efficiency and maintain peak res...

  13. Speciation of arsenic animal feed additives by microbore high-performance liquid chromatography with inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Pergantis, S A; Heithmar, E M; Hinners, T A

    1997-10-01

    Phenylarsonic compounds have been used as poultry and swine feed additives for the purpose of growth promotion and disease prevention. Owing to the lack of suitable analytical methods, however, knowledge of their metabolism, environmental fate and impact remains incomplete. In order to compensate for this, analytical procedures were developed that allow the speciation of arsenic animal feed additives by using microbore high-performance liquid chromatography (microHPLC) coupled on-line with ICP-MS. More specifically, reversed-phase (RP) chromatographic methods were optimised to achieve the separation of various phenylarsonic acids from each other and from the more toxic inorganic arsenic compounds. This mode of chromatography, however, exhibits limitations, especially in the presence of naturally occurring organoarsenic compounds. The application of RP ion-pairing chromatography eliminates such shortcomings by minimising the co-elution of arsenic species. In general, the microHPLC-ICP-MS methods developed in this study provide high selectivity, extremely good sensitivity, low limits of detection (low-ppb or sub-pg amounts of As), require small sample volumes (< 1 microliter), minimise waste and operate most efficiently under low mobile-phase flow rates (15-40 microliters min-1), which are compatible for use with other types of mass spectrometers, e.g., electrospray. Reference materials containing naturally occurring arsenic compounds were spiked with phenylarsonic compounds and then analysed by using the procedures developed in this study. PMID:9463956

  14. Resonance light scattering determination of 6-mercaptopurine coupled with HPLC technique

    Science.gov (United States)

    Li, Ai Ping; Peng, Jing Dong; Zhou, MingQiong; Zhang, Jin

    2016-02-01

    A simple, fast, costless, sensitive and selective method of resonance light scattering coupled with HPLC was established for the determination of 6-mercaptopurine in human urine sample. In a Britton-Robinson buffer solution of pH 5.5, the formation of coordination complex between 6-mercaptopurine and metal palladium (II) led to enhance the RLS intensity of the system. The RLS signal was detected by fluorescence detector at λex = λem = 315 nm. The analytical parameters were provided by the coupled system, the linear of 6-mercaptopurine response from 0.0615 to 2.40 μg L- 1 and the limit of detection (S/N = 3) was 0.05 μg L- 1. The presented method has been applied to determine 6-mercaptopurine in human urine samples which obtained satisfactory results. Moreover, the reaction mechanism and possible reasons for enhancement of RLS were fully discussed.

  15. Analysis of Currently Available Analgesic Tablets by Modern Liquid Chromatography: An Undergraduate Laboratory Introduction to HPLC.

    Science.gov (United States)

    Kagel, R. A.; Farwell, S. O.

    1983-01-01

    Background information, procedures, and results, are provided for an undergraduate experiment in which analgesic tablets are analyzed using liquid chromatography. The experiment, an improved, modified version of the Waters Associates Inc. experiment, is simple to prepare, requiring little glassware and minimal sample manipulation by students. (JN)

  16. Analytical capabilities of high performance liquid chromatography - Atmospheric pressure photoionization - Orbitrap mass spectrometry (HPLC-APPI-Orbitrap-MS) for the trace determination of novel and emerging flame retardants in fish.

    Science.gov (United States)

    Zacs, D; Bartkevics, V

    2015-10-22

    A new analytical method was established and validated for the analysis of 27 brominated flame retardants (BFRs), including so called "emerging" and "novel" BFRs (EBFRs and NBFRs) in fish samples. High performance liquid chromatography (HPLC) coupled to Orbitrap mass spectrometry (Orbitrap-MS) employing atmospheric pressure photoionization (APPI) interface operated in negative mode was used for the identification/quantitation of contaminants. HPLC-Orbitrap-MS analysis provided a fast separation of selected analytes within 14 min, thus demonstrating a high throughput processing of samples. The developed methodology was tested by intralaboratory validation in terms of recovery, repeatability, linear calibration ranges, instrumental and method limits of quantitation (i-LOQ and m-LOQ), and where possible, trueness was verified by analysis of certified reference materials (CRMs). Recoveries of analytes were between 80 and 119%, while the repeatability in terms of relative standard deviations (RSDs) was in the range from 1.2 to 15.5%. The measured values for both analyzed CRMs agreed with the provided consensus values, revealing the recovery of reference concentrations in 72-119% range. The elaborated method met the sensitivity criterion according to Commission Recommendation 2014/118/EU on monitoring of BFRs in food products for majority of the compounds. The concentrations of polybrominated diphenyl ethers (PBDEs) in real samples determined by HPLC-APPI-Orbitrap-MS method and validated gas chromatography-high-resolution mass spectrometry (GC-HRMS) method were found to be in a good agreement. PMID:26526911

  17. Determination of heavy metal complexes with humic substances by HPLC/ICP-MS coupling using on-line isotope dilution technique

    Energy Technology Data Exchange (ETDEWEB)

    Vogl, J.; Heumann, K.G. [Johannes Gutenberg-University Mainz, Institute of Inorganic Chemistry and Analytical Chemistry, Becherweg 24, D-55099 Mainz (Germany)

    1997-10-01

    An isotope dilution mass spectrometric (IDMS) method has been developed for the simultaneous determination of the complexes of 11 heavy metals (Ag, Cd, Cu, Mo, Ni, Pb, Tl, U, W, Zn and Zr) with humic substances (HS) by coupling HPLC with ICP-MS and applying the on-line isotope dilution technique. The HPLC separation was carried out with size exclusion chromatography. This HPLC/ICP-IDMS method was applied to samples from a brown water, ground water, sewage and seepage water as well as for a sample containing isolated fulvic acids. The total contents of heavy metals and of their complexes were analyzed in these samples with detection limits in the range of 5-110 ng/L. The analysis of heavy metal/HS complexes from the different waters resulted in characteristic fingerprints of the distribution pattern of heavy metals in the separated HS fractions. A comparison between the total heavy metal concentrations and their portions bound to humic substances showed distinct differences for the various metals. Simultaneous {sup 12}C detection was used for the characterization of HS complexes not identified by UV detection and for the determination of relative DOC concentrations of chromatographic peaks. (orig.) With 4 figs., 2 tabs., 10 refs.

  18. Speciation of mercury by chromatography coupled with atomic spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Armstrong, H.E.L

    2000-03-01

    A commercial GC-AFS instrument has been developed and optimised for the speciation of organomercury. This instrument couples a GC oven to a modified atomic fluorescence detector via a ceramic pyrolyser. Organomercury compounds in dichloromethane solvent were directly injected through a Programmable Temperature Vaporiser Injector onto a DB1 Megabore column. Once separated, the compounds eluted from the column and were atomised in the pyrolyser then detected by AFS. The direct injection technique, ceramic pyrolysis design and argon purged detector have improved previous instrument designs by enhancing and maintaining sensitivity. The instrumental limit of detection was determined to be 0.25 pg Hg absolute. Methods were developed for the extraction of methylmercury from a variety of marine samples. The techniques were validated using mussel homogenate and dogfish liver (IAEA 142, SRM 8044 and DOLT-2) certified reference materials. An interlaboratory comparison exercise was participated in and a method was developed for the determination of methylmercury in Fucus sea plant (IAEA 140). A concentration of 0.63 {+-} 0.006 ng g{sup -1} was reported. The material is now certified at 0.626 {+-} 0.139 ng g{sup -1}. Of all the participating laboratories, this was the closest result to the certified value. The instrument and methods were also applied to soil and sediment samples. Once again validation was performed with a CRM sediment, IAEA 356. Although this material has been reported to give positive artifact formation when using a steam distillation sample preparation procedure, good agreement and no artifacts were observed upon analysis. A further contaminated land, an uncontaminated soil and sediment sample were also studied. For all the samples studied by GC-AFS total mercury measurements were also made following an appropriate digestion procedure and CV-AFS. A gas chromatograph was also coupled with ICP-MS and HPLC was coupled to CV-AFS as comparative techniques. Both

  19. Speciation of mercury by chromatography coupled with atomic spectrometry

    International Nuclear Information System (INIS)

    A commercial GC-AFS instrument has been developed and optimised for the speciation of organomercury. This instrument couples a GC oven to a modified atomic fluorescence detector via a ceramic pyrolyser. Organomercury compounds in dichloromethane solvent were directly injected through a Programmable Temperature Vaporiser Injector onto a DB1 Megabore column. Once separated, the compounds eluted from the column and were atomised in the pyrolyser then detected by AFS. The direct injection technique, ceramic pyrolysis design and argon purged detector have improved previous instrument designs by enhancing and maintaining sensitivity. The instrumental limit of detection was determined to be 0.25 pg Hg absolute. Methods were developed for the extraction of methylmercury from a variety of marine samples. The techniques were validated using mussel homogenate and dogfish liver (IAEA 142, SRM 8044 and DOLT-2) certified reference materials. An interlaboratory comparison exercise was participated in and a method was developed for the determination of methylmercury in Fucus sea plant (IAEA 140). A concentration of 0.63 ± 0.006 ng g-1 was reported. The material is now certified at 0.626 ± 0.139 ng g-1. Of all the participating laboratories, this was the closest result to the certified value. The instrument and methods were also applied to soil and sediment samples. Once again validation was performed with a CRM sediment, IAEA 356. Although this material has been reported to give positive artifact formation when using a steam distillation sample preparation procedure, good agreement and no artifacts were observed upon analysis. A further contaminated land, an uncontaminated soil and sediment sample were also studied. For all the samples studied by GC-AFS total mercury measurements were also made following an appropriate digestion procedure and CV-AFS. A gas chromatograph was also coupled with ICP-MS and HPLC was coupled to CV-AFS as comparative techniques. Both approaches were

  20. Determination of bisphenol A in canned foods by immunoaffinity chromatography, HPLC, and fluorescence detection.

    Science.gov (United States)

    Braunrath, R; Podlipna, D; Padlesak, S; Cichna-Markl, M

    2005-11-16

    Bisphenol A (BPA) concentrations were determined in canned beverages, fruits, vegetables, and fat-containing foodstuffs bought in Austrian supermarkets. The analysis method consisted of sol-gel immunoaffinity chromatography followed by high-performance liquid chromatography with fluorescence detection. With one exception traces of BPA were detected in all samples. BPA recovery strongly depended on the food matrix, ranging from 27% in goulash to 103% in a lemon soft drink. The results obtained allow a more realistic picture of the BPA exposure caused by cans with an epoxy resin protective coating because--in contrast to several previous studies--only those fractions of the can contents that are actually consumed were analyzed. BPA concentrations ranging from 0.1 ng/mL (lemon soft drink) to 38 ng/g (ready-to eat soup from Thailand) were significantly lower than the European Union migration limit of 0.6 mg of BPA/kg of food. PMID:16277382

  1. Characterization and evaluation of two-dimensional microfluidic chip-HPLC coupled to tandem mass spectrometry for quantitative analysis of 7-aminoflunitrazepam in human urine.

    Science.gov (United States)

    Bai, Hsin-Yu; Lin, Shu-Ling; Chan, Shen-An; Fuh, Ming-Ren

    2010-10-01

    Microfluidic chip-based high-performance-liquid-chromatography coupled to mass spectrometry (chip-HPLC-MS) has been widely used in proteomic research due to its enhanced sensitivity. We employed a chip-HPLC-MS system for determining small molecules such as drug metabolites in biological fluids. This chip-HPLC-MS system integrates a microfluidic switch, a 2-dimensional column design including an enrichment column (160 nL) for sample pre-concentration and an analytical column for chromatographic separation, as well as a nanospray emitter on a single polyimide chip. In this study, a relatively large sample volume (500 nL) was injected into the enrichment column for pre-concentration and an additional 4 μL of the initial mobile phase was applied to remove un-retained components from the sample matrix prior to chromatographic separation. The 2-dimensional column design provides the advantages of online sample concentration and reducing matrix influence on MS detection. 7-Aminoflunitrazepam (7-aminoFM2), a major metabolite of flunitrazepam (FM2), was determined in urine samples using the integrated chip-HPLC-MS system. The linear range was 0.1-10 ng mL(-1) and the method detection limit (signal-to-noise ratio of 3) was 0.05 ng mL(-1) for 7-aminoFM2. After consecutive liquid-liquid extraction (LLE) and solid-phase extraction (SPE), the chip-HPLC-MS exhibited high correlation between 7-aminoFM2 spiked Milli-Q water and 7-aminoFM2 spiked urine samples. This system also showed good precision (n = 5) and recovery for spiked urine samples at the levels of 0.1, 1.0, and 10 ng mL(-1). Intra-day and inter-day precision were 2.0-7.1% and 4.3-6.0%, respectively. Clinical urine samples were also analyzed by this chip-HPLC-MS system and acceptable relative differences (-1.3 to -13.0%) compared with the results using a GC-MC method were determined. Due to its high sensitivity and ease of operation, the chip-HPLC-MS system can be utilized for the determination of small molecules such

  2. Pharmacokinetic study of unbound forsythiaside in rat blood and bile by microdialysis coupled with HPLC method.

    Science.gov (United States)

    Chu, Yang; Wang, Xiangyang; Guo, Jiahua; Li, Wei; Ma, Xiaohui; Zhu, Yonghong

    2012-09-01

    In the present study, an in vivo microdialysis sampling method coupled to HPLC was applied for the determination of unbound forsythiaside in rat blood and bile. Microdialysis probes were inserted into the jugular vein and bile duct of rats, and then blood and bile dialysates were collected at regular time intervals after intravenous administration of forsythiaside (50 mg/kg). Dialysate were directly injected into HPLC system. Forsythiaside was separated on a C₁₈ column eluted with the mobile phase of acetonitrile-water-formic acid (16:84:0.2, v/v/v) at a flow rate of 0.8 mL/min. The wavelength of the ultraviolet detector was set at 332 nm. The lowest limit quantification was 0.2 μg/mL for forsythiaside. Excellent linearity was found to be over a concentrate range of 0.2-100 μg/mL. The main pharmacokinetic parameters of unbound forsythiaside in rat blood and bile were obtained, Furthermore, the bile-to-blood distribution ratio (AUC(bile)/AUC(blood)) of forsythiaside was 0.32 ± 0.06. The results indicated that forsythiaside went through hepatobiliary excretion. PMID:22314894

  3. Analysis of opiates, cocaine and metabolites in urine by high-performance liquid chromatography with diode array detection (HPLC-DAD).

    Science.gov (United States)

    Fernández, P; Vázquez, C; Morales, L; Bermejo, A M

    2005-01-01

    An analytical method is proposed for the simultaneous determination of morphine, codeine, 6-acetyl-morphine (MAM), cocaine, benzoylecgonine (BEG), cocaethylene, methadone and 2-ethylen-1,5-dimethyl-3,3-diphenylpyrrolidine (EDDP) in urine using high performance liquid chromatography coupled to a diode array detector (HPLC-DAD). The selection of working wavelengths is based on the highest chromatographic response for each component: 233 nm for cocaine, BEG and cocaethylene; 285 nm for morphine, codeine and MAM; and 292 nm for methadone and EDDP. The mobile phase, which is a mixture of acetonitrile and 0.02 M phosphate buffer at pH 6.53, was eluted in gradient mode through an XTerra RP-8 column (250 mm x 4.6 mm i.d., 5 microm particle size). After applying a solid-phase extraction procedure with Bond Elut Certify cartridges, the recoveries obtained were between 60% (EDDP) and 97% (cocaethylene). A good linearity of the method in the 0.1-10 microg mL(-1) range of urinary concentrations was obtained because the coefficient of correlation exceeded 0.99 for each drug. The precision and accuracy were quite good, with values of heroin and[sol ]or cocaine. PMID:15895479

  4. Preparative separation and purification of bufadienolides from ChanSu by high-speed counter-current chromatography combined with preparative HPLC

    OpenAIRE

    Jialian Li; Yongqing Zhang; Yunliang Lin; Xiao Wang; Lei Fang; Yanling Geng; Qinde Zhang

    2013-01-01

    Eight bufadienolides were successfully isolated and purified from ChanSu by high-speed counter-current chromatography (HSCCC) combined with preparative HPLC (prep-HPLC). First, a stepwise elution mode of HSCCC with the solvent system composed of petroleum ether - ethyl acetate - methanol - water (4:6:4:6, 4:6:5:5, v/v) was employed and four bufadienolides, two partially purified fractions were obtained from 200 mg of crude extract. The partially purified fractions III and VI were then further...

  5. Quantification of nucleotides by ICPMS: coupling of ICPMS with capillary electrophoresis or capillary HPLC

    International Nuclear Information System (INIS)

    Full text: Quantification of nucleotides in small volumes of biological samples has eagerly been demanded. A method using ICPMS coupled with capillary electrophoresis or capillary liquid chromatography is reported. A new interface system, which consists of a double tube nebulizer inserted with a fused silica capillary tube and a cylinder mini-chamber with a sheath gas inlet, was designed. Moreover, the surface conditions of the sampling and skimmer cones, and the introduction of H2 gas into the plasma were found to significantly improve the signal/background ratio for phosphorus determination at m/z 31. (author)

  6. Analysis of potassium iodate reduction in tissue homogenates using high performance liquid chromatography-inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Cao, Xiaoxiao; Ma, Wei; Liu, Liejun; Xu, Jing; Wang, Haiyan; Li, Xiuwei; Wang, Jiangqing; Zhang, Jianhua; Wang, Zexi; Gu, Yunyou

    2015-10-01

    Potassium iodate (KIO3) and potassium iodide (KI) are the major salt iodization agents used worldwide. Unlike iodide (I(-)), iodate (IO3(-)) should be reduced to I(-) before it can be effectively used by the thyroid. In this study, we developed a new method for analyzing IO3(-) and I(-) in tissue homogenates using high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry (HPLC-ICP-MS). We further applied the method to demonstrate the KIO3 reduction process by tissues in vitro. The effects of KIO3 on the total antioxidative activity (TAA) and reduced nicotinamide adenine dinucleotide phosphate (NADPH) were also investigated here. Finally, we found that IO3(-) can be reduced to I(-) by tissue homogenates and IO3(-) irreversibly decreases the antioxidant capability of tissues. Our studies suggest that KIO3 might have a big effect on the redox balance of tissue and would further result in oxidative stress of organisms. PMID:26302905

  7. High performance liquid chromatography (HPLC) evaluation of carotenoids in irradiated guavas

    International Nuclear Information System (INIS)

    The use of ionizing gamma irradiation has shown very effective as an auxiliary technology for the decrease of post-harvest waste, grains disinfestation, pathogenic microorganisms control, increase in shelf life for meats, fruits, vegetables and bulbs and tubercles sprouts inhibition, maintaining nutritional quality. The carotenoids are pigments widely found in fruits and vegetables and are beneficial to human being health. This work was undergone using the irradiator with cesium source at the Army Technological Center, Brazil, with maximum dose rate of 2 kGy per hour. The objective is to evaluate the low gamma radiation doses (0.5, 1.0 and 1.5 kGy) influence in the total carotenoid and content lycopene in guavas CV Pal uma, with excellent weight classification. The total carotenoid content was extracted from the guava with acetone and moved to petroleum ether and determined by spectrophotometer at 450 nm. The determination of lycopene was accomplished by HPLC. The results showed that, in spite of lycopene loss with irradiation, the best dose was 0.5 kGy. (author)

  8. [Determination of total sulfite in wine by high performance liquid chromatography(HPLC) with fluorescence detection].

    Science.gov (United States)

    Wei, F; Chen, M S; Yu, L; Chang, L; Li, D M

    1999-11-01

    A highly sensitive fluorometric method for the determination of total sulfite in wine is reported. The strong fluorescent derivatives formed by the quantitative reaction of sulfite in wine and N-(9-acridinyl) maleimide(NAM) in aqueous solution under mild conditions was injected into the HPLC. Separation was performed on an ODS column(200 mm x 5 mm) with a mobile phase of V(CH3CN):V(0.1 mo/L NH4AC) = 25:75 at a flow rate of 1.0 mL/min and detected by fluorometry at 455 nm(excitation at 365 nm). There was a good linear calibration curve in the range from 0.25-4 mg/L(r = 0.9998), The limit of detection was 1 ng. Sulfite mass concentration in wine has been determined by this method with good results and recoveries. This method is simple, rapid and reliable, and a sample size of only 1 mL is required to complete an analysis. PMID:12552699

  9. Fingerprinting of complex mixtures with the use of high performance liquid chromatography, inductively coupled plasma atomic emission spectroscopy and chemometrics

    International Nuclear Information System (INIS)

    The molecular and metal profile fingerprints were obtained from a complex substance, Atractylis chinensis DC-a traditional Chinese medicine (TCM), with the use of the high performance liquid chromatography (HPLC) and inductively coupled plasma atomic emission spectroscopy (ICP-AES) techniques. This substance was used in this work as an example of a complex biological material, which has found application as a TCM. Such TCM samples are traditionally processed by the Bran, Cut, Fried and Swill methods, and were collected from five provinces in China. The data matrices obtained from the two types of analysis produced two principal component biplots, which showed that the HPLC fingerprint data were discriminated on the basis of the methods for processing the raw TCM, while the metal analysis grouped according to the geographical origin. When the two data matrices were combined into a one two-way matrix, the resulting biplot showed a clear separation on the basis of the HPLC fingerprints. Importantly, within each different grouping the objects separated according to their geographical origin, and they ranked approximately in the same order in each group. This result suggested that by using such an approach, it is possible to derive improved characterisation of the complex TCM materials on the basis of the two kinds of analytical data. In addition, two supervised pattern recognition methods, K-nearest neighbors (KNNs) method, and linear discriminant analysis (LDA), were successfully applied to the individual data matrices-thus, supporting the PCA approach

  10. Fingerprinting of complex mixtures with the use of high performance liquid chromatography, inductively coupled plasma atomic emission spectroscopy and chemometrics

    Energy Technology Data Exchange (ETDEWEB)

    Ni Yongnian [Department of Chemistry, Nanchang University, Nanchang, Jiangxi 330047 (China)], E-mail: ynni@ncu.edu.cn; Peng Yunyan [Department of Chemistry, Nanchang University, Nanchang, Jiangxi 330047 (China); Kokot, Serge [Inorganic Materials Program, School of Physical and Chemical Sciences, Queensland University of Technology, Brisbane, Queensland 4001 (Australia)

    2008-05-26

    The molecular and metal profile fingerprints were obtained from a complex substance, Atractylis chinensis DC-a traditional Chinese medicine (TCM), with the use of the high performance liquid chromatography (HPLC) and inductively coupled plasma atomic emission spectroscopy (ICP-AES) techniques. This substance was used in this work as an example of a complex biological material, which has found application as a TCM. Such TCM samples are traditionally processed by the Bran, Cut, Fried and Swill methods, and were collected from five provinces in China. The data matrices obtained from the two types of analysis produced two principal component biplots, which showed that the HPLC fingerprint data were discriminated on the basis of the methods for processing the raw TCM, while the metal analysis grouped according to the geographical origin. When the two data matrices were combined into a one two-way matrix, the resulting biplot showed a clear separation on the basis of the HPLC fingerprints. Importantly, within each different grouping the objects separated according to their geographical origin, and they ranked approximately in the same order in each group. This result suggested that by using such an approach, it is possible to derive improved characterisation of the complex TCM materials on the basis of the two kinds of analytical data. In addition, two supervised pattern recognition methods, K-nearest neighbors (KNNs) method, and linear discriminant analysis (LDA), were successfully applied to the individual data matrices-thus, supporting the PCA approach.

  11. Chromatographic fingerprinting analysis of Zhizhu Wan preparation by high-performance liquid chromatography coupled with photodiode array detector

    Directory of Open Access Journals (Sweden)

    Hui Sun

    2014-01-01

    Full Text Available Background: Traditional Chinese medicine (TCM formula has been used for over 1000 years and most of them contain complicate chemical constituents. Chromatographic fingerprinting has been widely accepted as a crucial method for qualitative and quantitative analyses for TCM. Zhi Zhu Wan (ZZW, a classical Chinese medical formula, has been commonly used for the treatment of gastrointestinal disease, which pose a serious challenge to its quality control. Materials and Methods: In this work, a sensitive and reliable method of high-performance liquid chromatography coupled with photodiode array detector (HPLC-PDA was developed to control the quality of ZZW for chemical fingerprint analysis and quantitative analysis of four major bioactive constituents, including hesperidin, naringin, neohesperidin, and atractylenolide I. The chromatographic separation was performed on a Waters Symmetry C18 column (4.6 mm × 250 mm, 5 μm particle size, with an aqueous 0.095% phosphate acid and acetonitrile mobile phase gradient. Results: Optimization of other experimental conditions was validated with satisfactory accuracy, precision, repeatability, and recovery. In quantitative analysis, the four components showed good regression (R > 0.9994 within test ranges, and the recovery method ranged from 99.32% to 100.630%. HPLC fingerprints of the ZZW samples were compared by performing similarity analysis. Conclusion: The results indicated that the newly developed HPLC-PDA fingerprint method would be suitable for quality control of ZZW.

  12. Relative Quantification of Sites of Peptide and Protein Modification Using Size Exclusion Chromatography Coupled with Electron Transfer Dissociation

    Science.gov (United States)

    Xie, Boer; Sharp, Joshua S.

    2016-08-01

    One difficult problem in the analysis of peptide modifications is quantifying isomeric modifications that differ by the position of the amino acid modified. HPLC separation using C18 reverse phase chromatography coupled with electron transfer dissociation (ETD) in tandem mass spectrometry has recently been shown to be able to relatively quantify how much of a given modification occurs at each amino acid position for isomeric mixtures; however, the resolution of reverse phase chromatography greatly complicates quantification of isomeric modifications by ETD because of the chromatographic separation of peptides with identical modifications at different sequence positions. Using peptide oxidation as a model system, we investigated the use of size exclusion chromatography coupled with ETD fragmentation to separate peptide sequences. This approach allows for the benefits of chromatographic separation of peptide sequences while ensuring co-elution of modification isomers for accurate relative quantification of modifications using standard data-dependent acquisitions. Using this method, the relative amount of modification at each amino acid can be accurately measured from single ETD MS/MS spectra in a standard data-dependent acquisition experiment.

  13. Relative Quantification of Sites of Peptide and Protein Modification Using Size Exclusion Chromatography Coupled with Electron Transfer Dissociation.

    Science.gov (United States)

    Xie, Boer; Sharp, Joshua S

    2016-08-01

    One difficult problem in the analysis of peptide modifications is quantifying isomeric modifications that differ by the position of the amino acid modified. HPLC separation using C18 reverse phase chromatography coupled with electron transfer dissociation (ETD) in tandem mass spectrometry has recently been shown to be able to relatively quantify how much of a given modification occurs at each amino acid position for isomeric mixtures; however, the resolution of reverse phase chromatography greatly complicates quantification of isomeric modifications by ETD because of the chromatographic separation of peptides with identical modifications at different sequence positions. Using peptide oxidation as a model system, we investigated the use of size exclusion chromatography coupled with ETD fragmentation to separate peptide sequences. This approach allows for the benefits of chromatographic separation of peptide sequences while ensuring co-elution of modification isomers for accurate relative quantification of modifications using standard data-dependent acquisitions. Using this method, the relative amount of modification at each amino acid can be accurately measured from single ETD MS/MS spectra in a standard data-dependent acquisition experiment. Graphical Abstract ᅟ. PMID:27075875

  14. Analysis of Naturally Occurring Phenolic Compounds in Aromatic Plants by RP-HPLC Coupled to Diode Array Detector (DAD and GC-MS after Silylation

    Directory of Open Access Journals (Sweden)

    Charalampos Proestos

    2013-03-01

    Full Text Available The following aromatic plants of Greek origin, Origanum dictamnus (dictamus, Eucalyptus globulus (eucalyptus, Origanum vulgare L. (oregano, Mellisa officinalis L. (balm mint and Sideritis cretica (mountain tea, were examined for the content of phenolic substances. Reversed phase HPLC coupled to diode array detector (DAD was used for the analysis of the plant extracts. The gas chromatography-mass spectrometry method (GC-MS was also used for identification of phenolic compounds after silylation. The most abundant phenolic acids were: gallic acid (1.5–2.6 mg/100 g dry sample, ferulic acid (0.34–6.9 mg/100 g dry sample and caffeic acid (1.0–13.8 mg/100 g dry sample. (+-Catechin and (−-epicatechin were the main flavonoids identified in oregano and mountain tea. Quercetin was detected only in eucalyptus and mountain tea.

  15. Multidimensional chromatography coupled to mass spectrometry in analysing complex proteomics samples

    NARCIS (Netherlands)

    Horvatovich, Peter; Hoekman, Berend; Govorukhina, Natalia; Bischoff, Rainer

    2010-01-01

    Multidimensional chromatography coupled to mass spectrometry (LC(n)-MS) provides more separation power and an extended measured dynamic concentration range to analyse complex proteomics samples than one dimensional liquid chromatography coupled to mass spectrometry (1D-LC-MS). This review gives an o

  16. HPLC-Orbitrap analysis for identification of organic molecules in complex material

    Science.gov (United States)

    Gautier, T.; Schmitz-Afonso, I.; Carrasco, N.; Touboul, D.; Szopa, C.; Buch, A.; Pernot, P.

    2015-10-01

    We performed High Performance Liquid Chromatography (HPLC) coupled to Orbitrap High Resolution Mass Spectrometry (OHR MS) analysis of Titan's tholins. This analysis allowed us to determine the exact composition and structure of some of the major components of tholins.

  17. MALDI-TOF mass spectrometry and reversed-phase HPLC-ELSD chromatography for structural and quantitative studies of major steroid saponins in commercial extracts of Yucca schidigera Roezl.

    Science.gov (United States)

    Sastre, F; Ferreira, F; Pedreschi, F

    2016-02-20

    This paper describes a new, improved systematic qualitative analysis of yucca saponins in commercial products by combined use of high-pressure liquid chromatography (HPLC) coupled to an evaporative light scattering detector (ELSD) and matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry (MS). Three groups with four saponins in each were completely resolved by HPLC-ELSD under C18 reversed-phase conditions using a linear gradient composed of methanol and water. The selectivity of the described HPLC-ELSD method is given by the sapogenin differences at C12 (carbonyl group) and at C2 (hydroxyl group), followed by the presence or absence of an exomethylene group at C25, and the composition and length of the oligosaccharidic chain at C3 in the sapogenins. The saponins were identified by chemical and spectroscopic methods including MALDI-TOF MS(1) and MS(2), high resolution MS, and one and bi-dimensional nuclear magnetic resonance (NMR) experiments. Among the twelve saponins identified, eleven were previously reported, and one is reported for the first time in Yucca schidigera. An identification flowchart procedure based on the analysis of the sodium adducts of intact saponins [M+Na](+) and the oligosaccharidic chain ions obtained in the MALDI-TOF MS(1) and the MS(2) spectrums, was developed for the analysis of Y. schidigera saponins. Two intact isomeric saponins were differentiated by this method, which could also be applied to the structural assignment of other steroid and triterpenic saponins. Using the four-major saponins as reference standards, a C18 reversed-phase HPLC-ELSD method was validated for their specific analysis in commercial extracts of Y. schidigera. Finally, the applicability of the HPLC-ELSD method for the relative quantification of yucca saponins is discussed. PMID:26760245

  18. Qualitative and quantitative analysis of glucosinolates and nucleosides in Radix Isatidis by HPLC and liquid chromatography tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    Xiuming Wang

    2013-09-01

    Full Text Available Multi-component fingerprinting and quantitation of the glucosinolates and nucleosides in samples of Radix Isatidis have been carried out using high-performance liquid chromatography with diode-array detection and electrospray ionization tandem mass spectrometry (HPLC–DAD–ESI/MS. Five nucleosides together with one glucosinolate were identified by comparing retention times, ultraviolet spectra, mass spectra and/or empirical molecular formulae of reference compounds. Quantitation of these six compounds was carried out simultaneously by HPLC on a Phenomenex Luna C18 column using gradient elution with methanol and water and detection at 254 nm. All calibration curves were linear (r>0.9994 within test ranges. Limits of detection and quantitation were 0.33 ng and 2.50 ng on column, respectively. Intra- and inter-day precision (as relative standard deviation for all analytes was <2.19% with recoveries in the range 99.6%–101.8% at three concentration levels. The validated method was successfully applied to fingerprinting and assay of 25 batches of Radix Isatidis sourced from different geographical regions of China. The method is simple and reliable and has potential value in the quality control of Radix Isatidis.

  19. Preparative separation and purification of bufadienolides from ChanSu by high-speed counter-current chromatography combined with preparative HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Li, Jialian; Zhang, Yongqing, E-mail: fleiv@163.com [College of Pharmacy, Shandong University of Traditional Chinese Medicine, Jinan, Shandong (China); Lin, Yunliang; Wang, Xiao; Fang, Lei; Geng, Yanling [Shandong Analysis and Test Center, Shandong Academy of Sciences, Jinan, Shandong (China); Zhang, Qinde [Shandong College of Traditional Chinese Medicine, Laiyang, Shandong (China)

    2013-09-01

    Eight bufadienolides were successfully isolated and purified from ChanSu by high-speed counter-current chromatography (HSCCC) combined with preparative HPLC (prep-HPLC). First, a stepwise elution mode of HSCCC with the solvent system composed of petroleum ether-ethyl acetate-methanol-water (4:6:4:6, 4:6:5:5, v/v) was employed and four bufadienolides, two partially purified fractions were obtained from 200 mg of crude extract. The partially purified fractions III and VI were then further separated by prepHPLC, respectively, and another four bufadienolides were recovered. Their structures were confirmed by ESI-MS and {sup 1}H-NMR spectra. (author)

  20. Preparative separation and purification of bufadienolides from ChanSu by high-speed counter-current chromatography combined with preparative HPLC

    Directory of Open Access Journals (Sweden)

    Jialian Li

    2013-01-01

    Full Text Available Eight bufadienolides were successfully isolated and purified from ChanSu by high-speed counter-current chromatography (HSCCC combined with preparative HPLC (prep-HPLC. First, a stepwise elution mode of HSCCC with the solvent system composed of petroleum ether - ethyl acetate - methanol - water (4:6:4:6, 4:6:5:5, v/v was employed and four bufadienolides, two partially purified fractions were obtained from 200 mg of crude extract. The partially purified fractions III and VI were then further separated by prep-HPLC, respectively, and another four bufadienolides were recovered. Their structures were confirmed by ESI-MS and ¹H-NMR spectra.

  1. Method optimization and quality assurance in speciation analysis using high performance liquid chromatography with detection by inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Larsen, Erik H.

    1998-02-01

    Achievement of optimum selectivity, sensitivity and robustness in speciation analysis using high performance liquid chromatography (HPLC) with inductively coupled mass spectrometry (ICP-MS) detection requires that each instrumental component is selected and optimized with a view to the ideal operating characteristics of the entire hyphenated system. An isocratic HPLC system, which employs an aqueous mobile phase with organic buffer constituents, is well suited for introduction into the ICP-MS because of the stability of the detector response and high degree of analyte sensitivity attained. Anion and cation exchange HPLC systems, which meet these requirements, were used for the seperation of selenium and arsenic species in crude extracts of biological samples. Furthermore, the signal-to-noise ratios obtained for these incompletely ionized elements in the argon ICP were further enhanced by a factor of four by continously introducing carbon as methanol via the mobile phase into the ICP. Sources of error in the HPLC system (column overload), in the sample introduction system (memory by organic solvents) and in the ICP-MS (spectroscopic interferences) and their prevention are also discussed. The optimized anion and cation exchange HPLC-ICP-MS systems were used for arsenic speciation in contaminated ground water and in an in-house shrimp reference sample. For the purpose of verification, HPLC coupled with tandem mass spectrometry with electrospray ionization was additionally used for arsenic speciation in the shrimp sample. With this analytical technique the HPLC retention time in combination with mass analysis of the molecular ions and their collision-induced fragments provide almost conclusive evidence of the identity of the analyte species. The speciation methods are validated by establishing a mass balance of the analytes in each fraction of the extraction procedure, by recovery of spikes and by employing and comparing independent techniques. The urgent need for

  2. Determination of the Antibiotic Oxytetracycline in Commercial Milk by Solid-Phase Extraction: A High-Performance Liquid Chromatography (HPLC) Experiment for Quantitative Instrumental Analysis

    Science.gov (United States)

    Mei-Ratliff, Yuan

    2012-01-01

    Trace levels of oxytetracylcine spiked into commercial milk samples are extracted, cleaned up, and preconcentrated using a C[subscript 18] solid-phase extraction column. The extract is then analyzed by a high-performance liquid chromatography (HPLC) instrument equipped with a UV detector and a C[subscript 18] column (150 mm x 4.6 mm x 3.5 [mu]m).…

  3. Exploring bitterness of traditional Chinese medicine samples by potentiometric electronic tongue and by capillary electrophoresis and liquid chromatography coupled to UV detection.

    Science.gov (United States)

    Yaroshenko, Irina; Kirsanov, Dmitry; Kartsova, Lyudmila; Sidorova, Alla; Sun, Qiyong; Wan, Haitong; He, Yu; Wang, Ping; Legin, Andrey

    2016-05-15

    Instrumental bitterness assessment of traditional Chinese herbal medicine (TCM) preparations was addressed in this study. Three different approaches were evaluated, high-performance liquid chromatography coupled to UV detector (HPLC), capillary electrophoresis coupled to UV detector (CE) and a potentiometric multisensor system - electronic tongue (ET). Most studies involving HPLC and CE separations use these as selective instruments for quantification of individual substances. However we employed these techniques to provide chromatographic or electrophoretic sample profiles. These profiles are somewhat analogous to the profiles produced by the ET. Profiles from all instruments were then related to professional sensory panel evaluations using projections on latent structures (PLS) regression. It was found that all three methods allow for bitterness assessment in TCM samples in terms of human sensory panel with root mean squared errors of prediction ca. 0.9 within bitterness scale from 0 (no bitterness) to 6 (maximal bitterness). PMID:26992500

  4. Estimation of the quantification uncertainty from flow injection and liquid chromatography transient signals in inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    The quality of the quantitative results obtained from transient signals in high-performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICPMS) and flow injection-inductively coupled plasma mass spectrometry (FI-ICPMS) was investigated under multielement conditions. Quantification methods were based on multiple-point calibration by simple and weighted linear regression, and double-point calibration (measurement of the baseline and one standard). An uncertainty model, which includes the main sources of uncertainty from FI-ICPMS and HPLC-ICPMS (signal measurement, sample flow rate and injection volume), was developed to estimate peak area uncertainties and statistical weights used in weighted linear regression. The behaviour of the ICPMS instrument was characterized in order to be considered in the model, concluding that the instrument works as a concentration detector when it is used to monitorize transient signals from flow injection or chromatographic separations. Proper quantification by the three calibration methods was achieved when compared to reference materials, although the double-point calibration allowed to obtain results of the same quality as the multiple-point calibration, shortening the calibration time. Relative expanded uncertainties ranged from 10-20% for concentrations around the LOQ to 5% for concentrations higher than 100 times the LOQ

  5. Arsenic speciation by liquid chromatography coupled with ionspray tandem mass spectrometry

    DEFF Research Database (Denmark)

    Corr, J. J.; Larsen, Erik Huusfeldt

    1996-01-01

    Ionspray mass spectrometry, a well established organic analysis technique, has been coupled to high-performance liquid chromatography for speciation of organic arsenic compounds, The ionspray source and differentially pumped interface of the mass spectrometer were operated in dual modes for...... fragmentation patterns showing molecular dissociation through an expected common product ion were obtained for the four arsenosugars, Molecular mode detection was utilized for qualitative verification of speciation analysis by high-performance liquid chromatography coupled to inductively coupled plasma mass...

  6. Capabilities of mixed-mode liquid chromatography coupled to inductively coupled plasma mass spectrometry for the simultaneous speciation analysis of inorganic and organically-bound selenium.

    Science.gov (United States)

    Peachey, Emma; Cook, Ken; Castles, Adrian; Hopley, Christopher; Goenaga-Infante, Heidi

    2009-10-16

    This work investigates for the first time the potential of mixed-mode (anion-exchange with reversed-phase) high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry (ICP-MS) for the simultaneous retention and selective separation of a range of inorganic and organically-bound selenium (Se) species. Baseline separation and detection of selenocystine (SeCys(2)), Se-methyl-selenocysteine (SeMC), selenomethionine (SeMet), methylseleninic acid (MSA), selenite, gamma-glutamyl-methyl-selenocysteine (gamma-glutamyl-SeMC), and selenate in a Se standard mixture by mixed-mode HPLC-ICP-MS was achieved by switching between two citrate mobile phases of different pH and ionic strength within a single chromatographic run of 20 min. Limits of detection obtained for these Se species ranged from 80 ng kg(-1) (for SeMC) to 123 ng kg(-1) (for selenate). Using this approach as developed for selenium speciation, an adequate separation of inorganic and organic As compounds was also achieved. These include arsenite, arsenate, arsenobetaine (AsB) and dimethylarsenic acid (DMA), which may coexist with Se species in biological samples. Application of the newly proposed methodology to the investigation of the elemental species distribution in watercress (used as the model sample) after enzymatic hydrolysis or leaching in water by accelerated solvent extraction (ASE) was addressed. Only SeMet, SeMC and selenate could be tentatively identified in watercress extracts by mixed-mode HPLC-ICP-MS and retention time matching with standards. Recoveries (n=3) of these Se species from samples spiked with standards averaged 102% (for SeMC), 94.9% (for SeMet) and 98.3% (for selenate). Verification of the presence of SeMet and SeMC in an enzymatic watercress extract was achieved by on-line HPLC-ESI MS/MS in selected reaction monitoring (SRM) mode. PMID:19758595

  7. Hydride generation, electrothermal vaporization and liquid chromatography as sample introduction techniques for inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Olson, Lisa K.; Vela, Nohora P.; Caruso, Joseph A.

    1995-06-01

    Although the most common method of sample introduction for inductively coupled plasma-mass spectrometry (ICP-MS) used is pneumatic nebulization, it suffers from limitations particularly with respect to the transport efficiency. In an effort to improve the analyte transport to the plasma, many alternative techniques have been studied, including electrothermal vaporization (ETV) and hydride generation, among others. Flow injection and liquid chromatography, although they employ pneumatic nebulization, have also been studied as sample introduction techniques due to the ability to analyze small volume samples and obtain speciation information. Here, some advances in sample introduction for ICP-MS will be discussed including hydride generation and ETV techniques. In addition, recent studies in HPLC-ICP-MS will also be described. Advantages and disadvantages of each method will be reviewed together with the application to some representative samples.

  8. High performance liquid chromatography coupled with radioactivity detection: a powerful tool for determining drug metabolite profiles in biological fluids.

    Science.gov (United States)

    Vollmer, K O; Klemisch, W; von Hodenberg, A

    1986-01-01

    High performance liquid chromatography coupled with continuous radioactivity detection represents an advancement in drug metabolism research. Using radioactive substances labelled in biologically stable positions, all metabolites can be specifically detected by radioactivity measurement. Thus no clean-up of biological fluids is required prior to HPLC. This can prevent artefact formation from unstable metabolites, reduces recovery problems and facilitates quantitation. Separation of highly polar and unpolar metabolites is possible in a single chromatographic run using gradient elution and reversed phase materials. This technique is also well-suited for preparative isolation and purification of metabolites for subsequent structure elucidation. Various metabolite profiles of drugs labelled with carbon-14 or tritium are shown. Metabolites of the following drugs are presented: norfenefrine, etozolin, thymoxamine, naloxone, and levobunolol. We review the general methodology and report our experience with this technique. In principle, this technique may be useful for all biological systems in which tracer techniques are applied. PMID:2939640

  9. High performance liquid chromatography (HPLC) applied to determination of oligosaccharides in irradiated beans (Vigna unguiculata (L.) Walp)

    Energy Technology Data Exchange (ETDEWEB)

    Lima, Keila S. Cople; Souza, Luciana B.; Coelho, Maysa J.; Lima, Antonio L. Santos; Vital, Helio C. [Instituto Militar de Engenharia IME, Rio de Janeiro, RJ (Brazil). Secao de Engenharia Nuclear]. E-mail: keila@ime.eb.br; maysa@ime.eb.br; santoslima@ime.eb.br; Godoy, Ronoel L.O. [EMBRAPA Agroindustria de Alimentos, Rio de Janeiro, RJ (Brazil)]. E-mail: ronoel@ctaa.embrapa.br

    2007-07-01

    Beans are important components of Brazilian diet, especially for less affordable people. They have in their composition proteins, vitamins, carbohydrates, minerals and fibers. Despite of their high nutritional value, nonnutritive elements from natural origin are present in leguminous plants, such as raffinose and stachyose. The oligosaccharides are flatulence agents due to bacterial anaerobic fermentation at the intestines. The aim of this study is to evaluate the effect of combined boiling and gamma irradiation treatments on fradinho-beans (Vigna unguiculata (L.) Walp) with respect to oligosaccharide contents. The irradiation process was performed at the Nuclear Defense Section of Brazilian Army, using a cavity type research irradiator, which has a Cs-137 radiation source and maximum dose rate of 1.8 kGy/h. The oligosaccharides were evaluated by HPLC technique, at 'EMBRAPA Agroindustria de Alimentos', using a SHIMADZU liquid chromatography system, with a refraction index detector Waters 2421. The mobile phase was acetonitrile 70% in water for raffinose and stachyose and 80% for saccharose. The flux and the running time were 1 mL/min and 18 minutes for raffinose and stachyose, and 1.3 mL/min and 20 minutes for saccharose. The injection volume was 20 {mu}L and the column used (Waters 250 x 4,6 mm; 4 mm) was kept at room temperature. The evaluation of unboiled irradiated beans showed that there was no significant difference between the different irradiation doses and control sample, keeping the oligosaccharide contents. However, the combination of the boiling and the irradiation processes turned out to reduce of non-nutritive factors that may cause flatulence, meaning a real benefit to the consumers. (author)

  10. High performance liquid chromatography (HPLC) applied to determination of oligosaccharides in irradiated beans (Vigna unguiculata (L.) Walp)

    International Nuclear Information System (INIS)

    Beans are important components of Brazilian diet, especially for less affordable people. They have in their composition proteins, vitamins, carbohydrates, minerals and fibers. Despite of their high nutritional value, nonnutritive elements from natural origin are present in leguminous plants, such as raffinose and stachyose. The oligosaccharides are flatulence agents due to bacterial anaerobic fermentation at the intestines. The aim of this study is to evaluate the effect of combined boiling and gamma irradiation treatments on fradinho-beans (Vigna unguiculata (L.) Walp) with respect to oligosaccharide contents. The irradiation process was performed at the Nuclear Defense Section of Brazilian Army, using a cavity type research irradiator, which has a Cs-137 radiation source and maximum dose rate of 1.8 kGy/h. The oligosaccharides were evaluated by HPLC technique, at 'EMBRAPA Agroindustria de Alimentos', using a SHIMADZU liquid chromatography system, with a refraction index detector Waters 2421. The mobile phase was acetonitrile 70% in water for raffinose and stachyose and 80% for saccharose. The flux and the running time were 1 mL/min and 18 minutes for raffinose and stachyose, and 1.3 mL/min and 20 minutes for saccharose. The injection volume was 20 μL and the column used (Waters 250 x 4,6 mm; 4 mm) was kept at room temperature. The evaluation of unboiled irradiated beans showed that there was no significant difference between the different irradiation doses and control sample, keeping the oligosaccharide contents. However, the combination of the boiling and the irradiation processes turned out to reduce of non-nutritive factors that may cause flatulence, meaning a real benefit to the consumers. (author)

  11. HPLC-UV Analysis Coupled with Chemometry to Identify Phenolic Biomarkers from Medicinal Plants, used as Ingredients in Two Food Supplement Formulas

    Directory of Open Access Journals (Sweden)

    Raluca Maria Pop

    2013-11-01

    Full Text Available . High performance liquid chromatography (HPLC with UV detection is nowadays the reference method to identify and quantify the biomarkers of quality and authenticity of plants and food supplements. Seven medicinal plants were collected from wild flora: Taraxacum officinalis (1, Cynara scolimus (2, Silybum marianum (3, Hypericum perforatum (4,  Chelidonium majus (5, Lycopodium clavatum (6 and  Hippophae rhamnoides (7  leaves and fruits.  Two products (A and B were obtained by mixing individual plant powders. Therefore product A was obtained by mixing dandelion, artichoke and milk thistle, 1:1:1 while product B by mixing St John’s wort, Celandine and Wolf’s claw, 1:1:1. The methanolic extracts of individual plants as well as three different extracts of products A and B (using acidulated water, neutral water and acidulated methanol were analyzed using HPLC-UV for their phenolics’ fingerprint and composition. The qualitative (untargeted analysis and quantitative (targeted analysis results were further compared using Principal Component Analysis (PCA in order to identify their specific biomarkers. Thus, quantitative evaluation of individual phenolics in case of individual plants and products A and B extracts, showed specific and significant differences of composition. Both products A and B contained elagic acid as major compound. For product A, good biomarkers were trans-cinnamic, chlorogenic, caffeic and p-coumaric acids, as well silymarin and silibine originating from milk thistle. For product B, good biomarkers were quercetin and kaempherol, gallic and protocatecuic acids, this product being rich in flavonoids. In conclusion, HPLC-UV coupled with PCA analysis proved to be a rapid and useful way to identify the main biomarkers of plants’ authentication, as well of final products’ quality and safety.

  12. Trace analysis of acrylamide by high-performance thin-layer chromatography coupled to mass spectrometry

    OpenAIRE

    Alpmann, Alexander

    2011-01-01

    Planar-chromatography (High-Performance Thin-Layer Chromatography, HPTLC) is a rapid and cost-effective offline separation method. Through advances in the automatization of each step the system reproducibility, from application and development to detection, has been improved. This makes planar-chromatography a highly reliable technique. HPTLC shows a couple of features that make it unique. There is great flexibility concerning application, development and detection that distinguishes HPTLC fr...

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

    Science.gov (United States)

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

  14. HPLC-MS/MS法测定曲霉菌代谢物中黄曲霉毒素及同系物%Determination of Aflatoxin and Aflatoxin-like Compounds in Aspergilli Metabolites by High Performance Liquid Chromatography Coupled with Tandem Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    郭礼强; 宫小明; 孙军; 张金玲; 丁葵英; 李凯

    2016-01-01

    建立了同时检测曲霉菌代谢物中黄曲霉毒素和同系物的高效液相色谱-线性离子阱质谱测定方法。产黄曲霉毒素B1(AFB1)寄生曲霉(菌株3.124)经PDA固体培养基培养,提取净化后经线性离子阱(QTrap)质量分析器分析(正离子模式,多反应检测),以AFB1二级碎片(MS2)信息和其同系物分子式信息预测代谢物MRM方法,检出3.124代谢物中黄曲霉毒素B2(AFB2)、黄曲霉毒素G1(AFG1)、黄曲霉毒素G2(AFG2)、O-甲基杂色曲霉素(MST)、杂色曲霉素(ST)5种真菌毒素,并用标准品进行了确证。结果表明,AFB2和AFG2在0.5μg/L~40μg/L,其它4种代谢物在0.2μg/L~40μg/L范围内线型关系良好,相关系数均大于0.99。本方法6种代谢物日内回收率81.3%~92.3%,相对标准偏差(RSD)为3.4%~6.2%;日间回收率82.1%~91.7%, RSD为3.8%~7.7%。该方法为快速检测霉菌代谢物中的同系物提供新的方法。%A stimulate method for determination of aflatoxin and aflatoxin-like compounds in Aspergilli metabolite was developed by high performance liquid chromatography-linear ion trap mass spectrometry. A. parasiticus (strain 3.124) which produce AFB1 was cultivated by PDA solid medium, then the metabolites of strain 3.124 was analyzed by mass analyzer of QTrap(positive ion mode, multiple reaction monitoring(MRM)) after extraction and purification, and found five mycotoxins of AFB2、AFG1、AFG2、MST and ST through the MRM methods predicted by MS2 of AFB1 and structural formula of aflatoxin-like compounds, and was confirmed by standard. The linear range of AFB2 and AFG2 was 0.5μg/L-40μg/L, the other 4 metabolites showed good linearity in the range of 0.2μg/L-40μg/L with the correlation coefficients more than 0.99. The recoveries of in-ter-day ranged from 81.3%to 92.3%with the relative standard deviations of 3.4%-6.2%, The recoveries of intra-day ranged from 82.1%to 91.7%with

  15. Comparative oxidation state specific analysis of arsenic species by high-performance liquid chromatography- inductively coupled plasma-mass spectrometry and hydride generation-cryotrapping-atomic absorption spectrometry

    OpenAIRE

    Currier, J. M.; Saunders, R J; Ding, L.; Bodnar, W.; Cable, P.; Matoušek, T. (Tomáš); Creed, J. T.; Stýblo, M.

    2013-01-01

    The formation of methylarsonous acid (MAsIII) and dimethylarsinous acid (DMAsIII) in the course of inorganic arsenic (iAs) metabolism plays an important role in the adverse effects of chronic exposure to iAs. High-performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) and hydride generation-cryotrapping-atomic absorption spectrometry (HG-CT-AAS) have been frequently used for the analysis of MAsIII and DMAsIII in biological samples. While HG-CT-AAS has con...

  16. High performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry for V and Ni quantification as tetrapyrroles

    Science.gov (United States)

    Duyck, Christiane Béatrice; Saint'Pierre, Tatiana Dillenburg; Miekeley, Norbert; da Fonseca, Teresa Cristina Oliveira; Szatmari, Peter

    2011-05-01

    A method was developed for the determination of V and Ni as tetrapyrroles by High Performance Liquid Chromatography hyphenated to Inductively Coupled Plasma Mass Spectrometry (HPLC-ICP-MS) using reversed phase and elution gradient. Chlorinated solvents and tetrahydrofuran were investigated as regard to separation time and ICP-MS detection efficiencies. The final elution gradient program started from pure methanol to a mixture of 20:80 (v/v) chloroform:methanol. External quantification of V and Ni with inorganic standards by flow injection ICP-MS, used online with HPLC, resulted in 95% of recoveries. The Limits of Detection for V during methanol elution and for Ni during the 20% chloroform gradient elution were evaluated by their minimum detectable concentrations, which were, respectively, 5 μg L - 1 and 8 μg L - 1 . The methodology was applied to polar and resin fractions separated from a Brazilian crude oil and a sediment extract from an oil-polluted area in the Guanabara Bay, Rio de Janeiro, Brazil. Vanadium as tetrapyrroles represented the totality of V content in the polar fraction, whereas Ni was in different polar forms in the resin and sediment extract.

  17. High performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry for V and Ni quantification as tetrapyrroles

    International Nuclear Information System (INIS)

    A method was developed for the determination of V and Ni as tetrapyrroles by High Performance Liquid Chromatography hyphenated to Inductively Coupled Plasma Mass Spectrometry (HPLC-ICP-MS) using reversed phase and elution gradient. Chlorinated solvents and tetrahydrofuran were investigated as regard to separation time and ICP-MS detection efficiencies. The final elution gradient program started from pure methanol to a mixture of 20:80 (v/v) chloroform:methanol. External quantification of V and Ni with inorganic standards by flow injection ICP-MS, used online with HPLC, resulted in 95% of recoveries. The Limits of Detection for V during methanol elution and for Ni during the 20% chloroform gradient elution were evaluated by their minimum detectable concentrations, which were, respectively, 5 μg L-1 and 8 μg L-1. The methodology was applied to polar and resin fractions separated from a Brazilian crude oil and a sediment extract from an oil-polluted area in the Guanabara Bay, Rio de Janeiro, Brazil. Vanadium as tetrapyrroles represented the totality of V content in the polar fraction, whereas Ni was in different polar forms in the resin and sediment extract.

  18. High performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry for V and Ni quantification as tetrapyrroles

    Energy Technology Data Exchange (ETDEWEB)

    Duyck, Christiane Beatrice, E-mail: cbduyck@vm.uff.br [Pontificia Universidade Catolica do Rio de Janeiro (PUC-Rio), R. Marques de Sao Vicente, 225, Gavea, Rio de Janeiro, RJ, 22451-900 (Brazil); Universidade Federal Fluminense (UFF), Campus do Valonguinho, Outeiro de Sao Joao Batista, s/no, 24020-150, Niteroi, RJ (Brazil); Saint' Pierre, Tatiana Dillenburg; Miekeley, Norbert [Pontificia Universidade Catolica do Rio de Janeiro (PUC-Rio), R. Marques de Sao Vicente, 225, Gavea, Rio de Janeiro, RJ, 22451-900 (Brazil); Oliveira da Fonseca, Teresa Cristina; Szatmari, Peter [Centro de Pesquisas Leopoldo A. Miguez de Mello da Petrobras (CENPES), Av. Horacio Macedo, 950, Cidade Universitaria, Rio de Janeiro, RJ, 21941-915 (Brazil)

    2011-05-15

    A method was developed for the determination of V and Ni as tetrapyrroles by High Performance Liquid Chromatography hyphenated to Inductively Coupled Plasma Mass Spectrometry (HPLC-ICP-MS) using reversed phase and elution gradient. Chlorinated solvents and tetrahydrofuran were investigated as regard to separation time and ICP-MS detection efficiencies. The final elution gradient program started from pure methanol to a mixture of 20:80 (v/v) chloroform:methanol. External quantification of V and Ni with inorganic standards by flow injection ICP-MS, used online with HPLC, resulted in 95% of recoveries. The Limits of Detection for V during methanol elution and for Ni during the 20% chloroform gradient elution were evaluated by their minimum detectable concentrations, which were, respectively, 5 {mu}g L{sup -1} and 8 {mu}g L{sup -1}. The methodology was applied to polar and resin fractions separated from a Brazilian crude oil and a sediment extract from an oil-polluted area in the Guanabara Bay, Rio de Janeiro, Brazil. Vanadium as tetrapyrroles represented the totality of V content in the polar fraction, whereas Ni was in different polar forms in the resin and sediment extract.

  19. Determination of Flavonoids and Anthocyanins in Nitraria tangutorum by High Performance Liquid Chromatography Coupled with Tandem Mass Spectrometry.

    Science.gov (United States)

    Zhe, Gao; Ying-Chun, Wang; Yan-Xu, Chang

    2016-01-01

    Using high-performance liquid chromatography coupled with diode array detection and electrospray ionization tandem mass spectrometry (HPLC-DAD-MSn) method, qualitative and quantitative analysis of flavonoids of stems, leaves, fruits and seeds, and anthocyanidin of fresh fruits in Nitraria tangutorum were performed. A total of 14 flavonoid components were identified from the seeds of N. tangutorum including three quercetin derivatives, three kaempferol derivatives, and eight isorhamnetin derivatives. A total of 12, 10, and 7 flavonoid components were identified from leaves, stems, and fruits of N. tangutorum, respectively; all were present in seeds also. The total content of flavonoids in leaves was the highest, up to 42.43 mg/g·dry weight. A total of 12 anthocyanidin components were identified from the fresh fruits of N. tangutorum, belonging to five anthocyanidin. The total content of anthocyanidin in fresh fruits was up to 45.83 mg/100 g· fresh weight, of which the acylated anthocyanidin accounted for 65.7%. The HPLC-DAD-MS(n) method can be operated easily, rapidly, and accurately, and is feasible for qualitative and quantitative analysis of flavone glycosides in N. tangutorum. PMID:26972973

  20. Analysis of Flavonoids in Lotus (Nelumbo nucifera Leaves and Their Antioxidant Activity Using Macroporous Resin Chromatography Coupled with LC-MS/MS and Antioxidant Biochemical Assays

    Directory of Open Access Journals (Sweden)

    Ming-Zhi Zhu

    2015-06-01

    Full Text Available Lotus (Nelumbo nucifera leaves, a traditional Chinese medicinal herb, are rich in flavonoids. In an effort to thoroughly analyze their flavonoid components, macroporous resin chromatography coupled with HPLC-MS/MS was employed to simultaneously enrich and identify flavonoids from lotus leaves. Flavonoids extracted from lotus leaves were selectively enriched in the macroporous resin column, eluted subsequently as fraction II, and successively subjected to analysis with the HPLC-MS/MS and bioactivity assays. Altogether, fourteen flavonoids were identified, four of which were identified from lotus leaves for the first time, including quercetin 3-O-rhamnopyranosyl-(1→2-glucopyranoside, quercetin 3-O-arabinoside, diosmetin 7-O-hexose, and isorhamnetin 3-O-arabino- pyranosyl-(1→2-glucopyranoside. Further bioactivity assays revealed that these flavonoids from lotus leaves possess strong antioxidant activity, and demonstrate very good potential to be explored as food supplements or even pharmaceutical products to improve human health.

  1. Determination of multiple human arsenic metabolites employing high performance liquid chromatography inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Stice, Szabina; Liu, Guangliang; Matulis, Shannon; Boise, Lawrence H; Cai, Yong

    2016-01-15

    During the metabolism of different arsenic-containing compounds in human, a variety of metabolites are produced with significantly varying toxicities. Currently available analytical methods can only detect a limited number of human metabolites in biological samples during one run due to their diverse characteristics. In addition, co-elution of species is often unnoticeable with most detection techniques leading to inaccurate metabolic profiles and assessment of toxicity. A high performance liquid chromatography inductively coupled mass spectrometry (HPLC-ICP-MS) method was developed that can identify thirteen common arsenic metabolites possibly present in human with special attention dedicated to thiolated or thiol conjugated arsenicals. The thirteen species included in this study are arsenite (As(III)), arsino-glutathione (As(GS)3), arsenate (As(V)), monomethylarsonous acid (MMA(III)), monomethylarsino-glutathione (MMA(III)(GS) 2), monomethylarsonic acid (MMA(V)), dimethylarsinous acid (DMA(III) (from DMA(III)I)), S-(dimethylarsinic)cysteine (DMA(III) (Cys)), dimethylarsino-glutathione (DMA(III)(GS)), dimethylarsinic acid (DMA(V)), dimethylmonothioarsinic acid (DMMTA(V)), dimethyldithioarsinic acid (DMDTA(V)), dimethylarsinothioyl glutathione (DMMTA(V)(GS)). The developed method was applied for the analysis of cancer cells that were incubated with darinaparsin (DMA(III)(GS)), a novel chemotherapeutic agent for refractory malignancies, and the arsenic metabolic profile obtained was compared to results using a previously developed method. This method provides a useful analytical tool which is much needed in unequivocally identifying the arsenicals formed during the metabolism of environmental arsenic exposure or therapeutic arsenic administration. PMID:26708625

  2. Report on three aliphatic dimethylarsinoyl compounds as common minor constituents in marine samples. An investigation using high-performance liquid chromatography inductively coupled plasma mass spectrometry and electrospray ionisation tandem mass spectrometry

    DEFF Research Database (Denmark)

    Sloth, Jens Jørgen; Larsen, Erik Huusfeldt; Julshamn, K.

    2005-01-01

    chromatography/inductively coupled plasma mass spectrometry (HPLC/ICPMS). Eluate fractions from the HPLC/ICPMS analyses containing the compounds in question were collected and subjected to analysis by electrospray ionisation tandem mass spectrometry (ESI-MS/MS), which provided supportive evidence for the...... of the 37 samples analysed, respectively. The limits of detection were 2-3 mug kg(-1) dry mass. The data illustrate that the three compounds are common minor constituents in marine samples. This is the first report on DMAE and DMAP as naturally occurring species in marine samples. The presence of...

  3. Determination of cyproheptadine in feeds using molecularly imprinted solid-phase extraction coupled with HPLC.

    Science.gov (United States)

    Yang, Jianwen; Wang, Zongnan; Zhou, Tong; Song, Xuqin; Liu, Qingyong; Zhang, Yuman; He, Limin

    2015-05-15

    A novel method was developed for the determination of cyproheptadine in feeds using molecularly imprinted solid-phase extraction coupled with high-performance liquid chromatography. The polymers were prepared using cyproheptadine as a template molecule, methacrylic acid as a functional monomer, ethylene glycol dimethacrylate as a cross-linking agent, and dichloromethane as a solvent by bulk polymerization. Under the optimum solid-phase extraction conditions, the molecular imprinting cartridge can selectively extract and enrich cyproheptadine from a variety of feeds. Mean recoveries of cyproheptadine from four kinds of feeds spiked at 0.1, 1.0 and 10mgkg(-1) ranged from 85.5% to 96.2%, with intra-day and inter-day relative standard deviation less than 10%. The calibration curve of cyproheptadine was good linear relationship (r>0.9993) within the range of 0.1-50μgmL(-1). The limit of detection (LOD) and the limit of quantification (LOQ) were 0.04 and 0.1mgkg(-1), respectively. PMID:25855316

  4. Method for the quantification of vanadyl porphyrins in fractions of crude oils by High Performance Liquid Chromatography-Flow Injection-Inductively Coupled Plasma Mass Spectrometry

    Science.gov (United States)

    Wandekoken, Flávia G.; Duyck, Christiane B.; Fonseca, Teresa C. O.; Saint'Pierre, Tatiana D.

    2016-05-01

    High performance liquid chromatography hyphenated by flow injection to inductively coupled plasma mass spectrometry (HPLC-FI-ICP-MS) was used to investigate V linked to porphyrins present in fractions of crude oil. First, the crude oil sample was submitted to fractionation by preparative liquid chromatography with UV detection, at the porphyrin Soret band wavelength (400 nm). The obtained porphyrin fractions were then separated in a 250 mm single column, in the HPLC, and eluted with different mobile phases (methanol or methanol:toluene (80:20; v:v)). The quantification of V-porphyrins in the fractions eluted from HPLC was carried out by online measuring the 51V isotope in the ICP-MS, against vanadyl octaethylporphine standard solutions (VO-OEP), prepared in the same solvent as the mobile phase, and injected post-column directly into the plasma. A 20 μg L- 1 Ge in methanol was used as internal standard for minimizing non-spectral interference, such as short-term variations due to injection. The mathematical treatment of the signal based on Fast Fourier Transform smoothing algorithm was employed to improve the precision. The concentrations of V as V-porphyrins were between 2.7 and 11 mg kg- 1 in the fractions, which were close to the total concentration of V in the porphyrin fractions of the studied crude oil.

  5. Coupling of hplc and NMR. 2. Analysis of flowing liquid chromatographic fractions by proton magnetic resonance in the presence of hydrogen-containing eluting solvents

    Science.gov (United States)

    Buddrus, Joachim; Herzog, Helmut; Cooper, James W.

    1H NMR spectra of flowing high-pressure liquid chromatography (hplc) fractions of barbituric acids dissolved in hydrogen-chloroform were obtained. Two techniques have been used to prevent overflow in the computer linked with the Fourier transform NMR spectrometer: (1) extension of the computer word length from the standard 16 to 32 bits, and (2) selective presaturation of the solvent protons.

  6. Separation of silver ions and starch modified silver nanoparticles using high performance liquid chromatography with ultraviolet and inductively coupled mass spectrometric detection

    Science.gov (United States)

    Hanley, Traci A.; Saadawi, Ryan; Zhang, Peng; Caruso, Joseph A.; Landero-Figueroa, Julio

    2014-10-01

    The production of commercially available products marketed to contain silver nanoparticles is rapidly increasing. Species-specific toxicity is a phenomenon associated with many elements, including silver, making it imperative to develop a method to identify and quantify the various forms of silver (namely, silver ions vs. silver nanoparticles) possibly present in these products. In this study a method was developed using high performance liquid chromatography (HPLC) with ultraviolet (UV-VIS) and inductively coupled mass spectrometric (ICP-MS) detection to separate starch stabilized silver nanoparticles (AgNPs) and silver ions (Ag+) by cation exchange chromatography with 0.5 M nitric acid mobile phase. The silver nanoparticles and ions were baseline resolved with an ICP-MS response linear over four orders of magnitude, 0.04 mg kg- 1 detection limit, and 90% chromatographic recovery for silver solutions containing ions and starch stabilized silver nanoparticles smaller than 100 nm.

  7. Separation of silver ions and starch modified silver nanoparticles using high performance liquid chromatography with ultraviolet and inductively coupled mass spectrometric detection

    International Nuclear Information System (INIS)

    The production of commercially available products marketed to contain silver nanoparticles is rapidly increasing. Species-specific toxicity is a phenomenon associated with many elements, including silver, making it imperative to develop a method to identify and quantify the various forms of silver (namely, silver ions vs. silver nanoparticles) possibly present in these products. In this study a method was developed using high performance liquid chromatography (HPLC) with ultraviolet (UV–VIS) and inductively coupled mass spectrometric (ICP-MS) detection to separate starch stabilized silver nanoparticles (AgNPs) and silver ions (Ag+) by cation exchange chromatography with 0.5 M nitric acid mobile phase. The silver nanoparticles and ions were baseline resolved with an ICP-MS response linear over four orders of magnitude, 0.04 mg kg−1 detection limit, and 90% chromatographic recovery for silver solutions containing ions and starch stabilized silver nanoparticles smaller than 100 nm

  8. Bamboo charcoal as adsorbent for SPE coupled with monolithic column-HPLC for rapid determination of 16 polycyclic aromatic hydrocarbons in water samples.

    Science.gov (United States)

    Ma, Jiping; Li, Mo; Li, Jinhua; Rui, Cuijie; Xin, Yanping; Xue, Qinzhao; Chen, Lingxin

    2011-10-01

    The coupling of solid-phase extraction (SPE) using bamboo charcoal (BC) as an adsorbent with a monolithic column-high performance liquid chromatography (MC-HPLC) method was developed for the high-efficiency enrichment and rapid determination of 16 polycyclic aromatic hydrocarbons (PAHs) in water. Key influence factors, such as the type and the volume of the elution solvent, and the flow rate and the volume of the sample loading, were optimized to obtain a high SPE recovery and extraction efficiency. BC as an SPE adsorbent presented a high extraction efficiency due to its large specific surface area and high adsorption capacity; MC as an HPLC column accelerated the separation within 8 min because of its high porosity, fast mass transfer, and low-pressure resistance. The calibration curves for the PAHs extracted were linear in the range of 0.2-15 µg/L, with the correlation coefficients (r(2)) between 0.9970-0.9999. This method attained good precisions (relative standard deviation, RSD) from 3.5 to 10.9% for the standard PAHs I aqueous solutions at 5 µg/L; the method recoveries ranged in 52.6-121.6% for real spiked river water samples with 0.4 and 4 µg/L. The limits of detection (LODs, S/N = 3) of the method were determined from 11 and 87 ng/L. The developed method was demonstrated to be applicable for the rapid and sensitive determination of 16 PAHs in real environmental water samples. PMID:22586244

  9. Fast Determination of Toxic Arsenic Species in Food Samples Using Narrow-bore High-Performance Liquid-Chromatography Inductively Coupled Plasma Mass Spectrometry.

    Science.gov (United States)

    Terol, Amanda; Marcinkowska, Monika; Ardini, Francisco; Grotti, Marco

    2016-01-01

    A new method for the speciation analysis of arsenic in food using narrow-bore high-performance liquid-chromatography inductively coupled plasma mass spectrometry (HPLC-ICP-MS) has been developed. Fast separation of arsenite, arsenate, monomethylarsonic acid and dimethylarsinic acid was carried out in 7 min using an anion-exchange narrow-bore Nucleosil 100 SB column and 12 mM ammonium dihydrogen phosphate of pH 5.2 as the mobile phase, at a flow rate of 0.3 mL min(-1). A PFA-ST micronebulizer jointed to a cyclonic spray chamber was used for HPLC-ICP-MS coupling. Compared with standard-bore HPLC-ICP-MS, the new method has provided higher sensitivity, reduced mobile-phase consumption, a lower matrix plasma load and a shorter analysis time. The achieved instrumental limits of detection were in the 0.3 - 0.4 ng As mL(-1) range, and the precision was better than 3%. The arsenic compounds were efficiently (>80%) extracted from various food samples using a 1:5 methanol/water solution, with additional ultrasonic treatment for rice products. The applicability of this method was demonstrated by the analysis of several samples, such as seafood (fish, mussels, shrimps, edible algae) and rice-based products (Jasmine and Arborio rice, spaghetti, flour, crackers), including three certified reference materials. PMID:27506720

  10. Environmental application of elemental speciation analysis based on liquid or gas chromatography hyphenated to inductively coupled plasma mass spectrometry-A review

    International Nuclear Information System (INIS)

    In recent years the number of environmental applications of elemental speciation analysis using inductively coupled plasma mass spectrometry (ICP-MS) as detector has increased significantly. The analytical characteristics, such as extremely low detection limits (LOD) for almost all elements, the wide linear range, the possibility for multi-elemental analysis and the possibility to apply isotope dilution mass spectrometry (IDMS) make ICP-MS an attractive tool for elemental speciation analysis. Two methodological approaches, i.e. the combination of ICP-MS with high performance liquid chromatography (HPLC) and gas chromatography (GC), dominate the field. Besides the investigation of metals and metalloids and their species (e.g. Sn, Hg, As), representing 'classic' elements in environmental science, more recently other elements (e.g. P, S, Br, I) amenable to ICP-MS determination were addressed. In addition, the introduction of isotope dilution analysis and the development of isotopically labeled species-specific standards have contributed to the success of ICP-MS in the field. The aim of this review is to summarize these developments and to highlight recent trends in the environmental application of ICP-MS coupled to GC and HPLC.

  11. HPLC/Hydride Generation AAS Coupling for the Speciation of Sb(III) and Sb(V) in Wastewaters

    OpenAIRE

    ŞATIROĞLU, Nuray; GENÇ, Sema BEKTAŞ and Ömer

    2000-01-01

    A comparative study was made with two HPLC columns of different lengths (PRP-X 100, 250 mm \\( \\times \\) 4.1 mm id and PRP-X 100, 100 mm \\( \\times \\) 4.1 mm id) coupled to HGAAS for the speciation of inorganic Sb(III) and Sb(V) species. The effects of eluent concentration and pH on the retention times of Sb species in both columns were investigated. The separation of Sb species was realized by using 50 mmol/L citrate solution at pH 4.0 as the eluent. The retention times were 2.0 min and 10.0 m...

  12. Determination of Oxidized Phosphatidylcholines by Hydrophilic Interaction Liquid Chromatography Coupled to Fourier Transform Mass Spectrometry

    OpenAIRE

    Pia Sala; Sandra Pötz; Martina Brunner; Martin Trötzmüller; Alexander Fauland; Alexander Triebl; Jürgen Hartler; Ernst Lankmayr; Köfeler, Harald C

    2015-01-01

    A novel liquid chromatography-mass spectrometry (LC-MS) approach for analysis of oxidized phosphatidylcholines by an Orbitrap Fourier Transform mass spectrometer in positive electrospray ionization (ESI) coupled to hydrophilic interaction liquid chromatography (HILIC) was developed. This method depends on three selectivity criteria for separation and identification: retention time, exact mass at a resolution of 100,000 and collision induced dissociation (CID) fragment spectra in a linear ion ...

  13. Solid-phase microextraction coupled with high performance liquid chromatography: a complementary technique to solid-phase microextraction-gas chromatography for the analysis of pesticide residues in strawberries.

    Science.gov (United States)

    Wang, Z; Hennion, B; Urruty, L; Montury, M

    2000-11-01

    Solid-phase microextraction coupled with high performance liquid chromatography has been studied for the analysis of methiocarb, napropamide, fenoxycarb and bupirimate in strawberries. The strawberries were blended and centrifuged. Then, an aliquot of the resulting extracting solution was subjected to solid-phase microextraction (SPME) on a 60 microns polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibre for 45 min at room temperature. The extracted pesticides on the SPME fibre were desorbed into SPME/high performance liquid chromatography (HPLC) interface for HPLC analysis with diode-array detection (DAD). The method is organic solvent-free for the whole extraction process and is simple and easy to manipulate. The detection limits were shown to be at low microgram kg-1 level and the linear response covered the range from 0.05 to 2 mg kg-1 of pesticides in strawberries with a regression coefficient larger than 0.99. A good repeatability with RSDs between 2.92 and 9.25% was obtained, depending on compounds. PMID:11271705

  14. Molecular assessment of the membrane menaquinones of irradiated micrococcus on disposable medical devices with high performance liquid chromatography (HPLC)

    International Nuclear Information System (INIS)

    The genus of micrococcus and its main species like; M. Roseus, M. nishinomiyans consist of up to 10% of microbial contamination of disposal medical devices. Chemical alteration of menoquinones mainly [MK-7-(H2), MK-8(H2),.....] from some irradiated species of the micrococcus at different doses (500 Gy to 25 kGy) the sterilization dose, are quantitatively evaluated by HPLC. (author)

  15. Molecular assessment of the membrane menaquinones of irradiated micrococcus on disposable medical devices with high performance liquid chromatography (HPLC)

    Science.gov (United States)

    Ghojaie, M.

    1993-10-01

    The genus of micrococcus and its main species like; M. Roseus, M. Nishinomiyansis consist of upto 10% of microbial contamination of disposable medical devices. Chemical alteration of Menuquinones Mainly [MK-7-(H2), MK-8(H2),…] from some Irradiated species of the micrococcus at different doses (500 Gy to 25 kGy; the sterilization dose) are quantitatively evaluated by HPLC.

  16. Efficient generation of arsanes coupled with HPLC or with cryotrapping for speciation analysis of arsenic

    Czech Academy of Sciences Publication Activity Database

    Marschner, Karel; Musil, Stanislav; Rychlovský, P.; Dědina, Jiří

    Prague: Charles University in Prague, Faculty of Science, 2015 - (Nesměrák, K.), s. 123-129 ISBN 978-80-7444-036-6. [International Students Conference "Modern Analytical Chemistry" /11./. Prague (CZ), 22.09.2015-23.09.2015] R&D Projects: GA ČR GA14-23532S Institutional support: RVO:68081715 Keywords : arsenic speciation analysis * hydride generation * HPLC Subject RIV: CB - Analytical Chemistry, Separation

  17. Automated on-line solid phase extraction coupled to HPLC-APCI-MS detection as a versatile tool for the analysis of phenols in water samples

    International Nuclear Information System (INIS)

    In this work a liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry (HPLC-APCI-MS) technique was developed for the determination of phenols and anilines in waste water samples. All relevant parameters were optimized for liquid chromatographic (LC) separation and mass spectrometric (MS) detection. Mass spectrometric detection was used in either negative ionization (NI) or positive ionization (PI) mode, which was depending on the physicochemical properties of the analyte. For screening analysis, full scan mode (SCAN) was used, while selected ion monitoring (SIM) mode of acquisition was used for maximum sensitivity. The optimal interface parameters and solvent compositions were evaluated, which mainly determined the ionization of analytes thus strongly influencing the sensitivity. The quasi-molecular ions were the most abundant signals both for phenols ([M-H]- in NI) and for anilines ([M+H]+ in PI). In general, fragmentation was hardly observed for one-ring phenols. Only fragmentation due to neutral losses of NO, HCl, NH3, CO2, CHO or CO from the functional groups were obtained via collision induced dissociation (CID) in a single quadrupole mass spectrometer. A further source of structural information was the relative intensity of positive and negative ions for one analyte: Only in the case of para-methyl substituted phenols, detection was also possible in positive ionization mode with reasonable sensitivity. In contrast to the phenols, anilines offered somewhat higher structural information due to increased fragmentation through CID, when detected in the positive ionization mode. The main goal of this work was the development of a method for the determination of US EPA priority phenols in different environmental matrices. As highest sensitivity and selectivity was required for this task, a preconcentrating step was necessary, and consequently solid phase extraction (SPE) was coupled on-line to HPLC-APCI-MS. The optimized method allowed the

  18. On the reliability of methods for the speciation of mercury based on chromatographic separation coupled to atomic spectrometric detection

    OpenAIRE

    Qvarnström, Johanna

    2003-01-01

    This thesis deals with the reliability of methods for the speciation of mercury in environmental and biological samples. Problems with speciation methods that couple chromatography to atomic spectrometric detection and how to overcome the problems are discussed. Analytical techniques primarily studied and evaluated are high performance liquid chromatography-cold vapour-atomic absorption spectrometry (HPLC-CV-AAS), HPLC-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS), capillary elec...

  19. Strategy of accelerated method development for high-throughput bioanalytical assays using ultra high-performance liquid chromatography coupled with mass spectrometry.

    Science.gov (United States)

    Liu, Guowen; Snapp, Heidi M; Ji, Qin C; Arnold, Mark E

    2009-11-15

    Here we report a strategy for rapid method development of high-throughput bioanalytical assays using ultra high-performance liquid chromatography coupled with tandem mass spectrometry (uHPLC-MS/MS). First, a data set was established for the removal of representative phospholipids under different sample treatments to guide subsequent method development for various compounds. The recovery information of the analyte(s) of interest under different extraction conditions was then obtained during method development. With the recovery profiles and the pre-established knowledge of phospholipids removal in place, an optimal extraction condition was identified to give not only a satisfactory recovery but also a good cleanup of the sample. A rapid LC or uHPLC method was developed without the need of extensive column wash after the elution of the analyte. This strategy was demonstrated through the method development of a uHPLC-MS/MS bioanalytical assay for the quantitation of ketoconazole in human plasma with liquid-liquid extraction using a hexane and ethyl acetate solvent system. The retention time for ketoconazole through an isocratic elution was 18 s. Good accuracy and precision were obtained. Assay ruggedness was demonstrated by consistent internal standard responses and retention time for 500 sequential injections. In addition, consistent results were obtained for incurred sample reanalysis. PMID:19856950

  20. An optimized high-performance liquid chromatography (HPLC method for benzoylmesaconine determination in Radix Aconiti Lateralis Preparata (Fuzi, aconite roots and its products

    Directory of Open Access Journals (Sweden)

    Xu Hongxi

    2008-05-01

    Full Text Available Abstract Background Benzoylmesaconine (BMA is the main Aconitum alkaloid in Radix Aconiti Lateralis Preparata (Fuzi, aconite roots with potent pharmacological activities, such as analgesia and anti-inflammation. The present study developed a simple and reliable method using BMA as a marker compound for the quality control of processed aconite roots and their products. Methods After extraction, a high-performance liquid chromatography (HPLC determination of BMA was conducted on a RP-C18 column by gradient elution with acetonitrile and aqueous phase, containing 0.1% phosphoric acid adjusted with triethylamine to pH 3.0. Results A distinct peak profile was obtained and separation of BMA was achieved. Method validation showed that the relative standard deviations (RSDs of the precision of BMA in all intra-day and inter-day assays were less than 1.36%, and that the average recovery rate was 96.95%. Quantitative analysis of BMA showed that the content of BMA varied significantly in processed aconite roots and their products. Conclusion This HPLC method using BMA as a marker compound is applicable to the quality control of processed aconite roots and their products.

  1. Arsenic speciation by liquid chromatography coupled with ionspray tandem mass spectrometry

    DEFF Research Database (Denmark)

    Corr, J. J.; Larsen, Erik Huusfeldt

    1996-01-01

    Ionspray mass spectrometry, a well established organic analysis technique, has been coupled to high-performance liquid chromatography for speciation of organic arsenic compounds, The ionspray source and differentially pumped interface of the mass spectrometer were operated in dual modes for...

  2. HPLC-UV Analysis Coupled with Chemometry to Identify Phenolic Biomarkers from Medicinal Plants, used as Ingredients in Two Food Supplement Formulas

    OpenAIRE

    Raluca Maria Pop; Florina Csernatoni; Floricuta Ranga; Florinela Fetea; Carmen Socaciu

    2013-01-01

    . High performance liquid chromatography (HPLC) with UV detection is nowadays the reference method to identify and quantify the biomarkers of quality and authenticity of plants and food supplements. Seven medicinal plants were collected from wild flora: Taraxacum officinalis (1), Cynara scolimus (2), Silybum marianum (3), Hypericum perforatum (4),  Chelidonium majus (5), Lycopodium clavatum (6) and  Hippophae rhamnoides (7)  leaves and fruits.  Two products (A and B) were obtained by mixing i...

  3. Simultaneous speciation and preconcentration of ultra trace concentrations of mercury and selenium species in environmental and biological samples by hollow fiber liquid phase microextraction prior to high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Moreno, F; García-Barrera, T; Gómez-Ariza, J L

    2013-07-26

    Nowadays, hollow fiber membrane extraction techniques are widely used due to the high enrichment factors obtained with many different types of analytes and samples. In this paper, we propose a new analytical method that allows the simultaneous extraction of methylmercury, inorganic mercury and Se(4+) and determination by high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry (HPLC-ICP-MS). The detection limits obtained are very low (110-230ng/L) with relative standard deviations below 15% for all the analytes and averaged recoveries in fortified samples in the range of 71-99%. The precision of the analytical method is very good which overcomes one of the most important shortcomings of membrane extraction techniques. Several variables were studied to get optimal extraction conditions for the analytes. This method has been validated with real world samples such as water (tap, river and estuarine) and human blood plasma. PMID:23541655

  4. Constructing a LabVIEW-Controlled High-Performance Liquid Chromatography (HPLC) System: An Undergraduate Instrumental Methods Exercise

    Science.gov (United States)

    Smith, Eugene T.; Hill, Marc

    2011-01-01

    In this laboratory exercise, students develop a LabVIEW-controlled high-performance liquid chromatography system utilizing a data acquisition device, two pumps, a detector, and fraction collector. The programming experience involves a variety of methods for interface communication, including serial control, analog-to-digital conversion, and…

  5. Simultaneous Determination of Caffeine and Vitamin B6 in Energy Drinks by High-Performance Liquid Chromatography (HPLC)

    Science.gov (United States)

    Leacock, Rachel E.; Stankus, John J.; Davis, Julian M.

    2011-01-01

    A high-performance liquid chromatography experiment to determine the concentration of caffeine and vitamin B6 in sports energy drinks has been developed. This laboratory activity, which is appropriate for an upper-level instrumental analysis course, illustrates the standard addition method and simultaneous determination of two species. (Contains 1…

  6. Rapid Isolation and Determination of Flavones in Biological Samples Using Zinc Complexation Coupled with High-Performance Liquid Chromatography.

    Science.gov (United States)

    Sun, Chenghe; Wang, Hecheng; Wang, Yingping; Xiao, Shengyuan

    2016-01-01

    Chlorophyll-type contaminants are commonly encountered in the isolation and determination of flavones of plant aerial plant parts. Heme is also a difficult background substance in whole blood analysis. Both chlorophyll and heme are porphyrin type compounds. In this study, a rapid method for isolating flavones with 5-hydroxyl or ortho-hydroxyl groups from biological samples was developed based on the different solubilities of porphyrin-metal and flavone-metal complexes. It is important that other background substances, e.g., proteins and lipids, are also removed from flavones without an additional processing. The recoveries of scutellarin, baicalin, baicalein, wogonoside and wogonin, which are the primary constituents of Scutellaria baicalensis (skullcaps) were 99.65% ± 1.02%, 98.98% ± 0.73%, 99.65% ± 0.03%, 97.59% ± 0.09% and 95.19% ± 0.47%, respectively. As a sample pretreatment procedure, this method was coupled to high-performance liquid chromatography (HPLC) with good separation, sensitivity and linearity and was applied to determine the flavone content in different aerial parts of S. baicalensis and in dried blood spot samples. PMID:27537870

  7. Rapid Isolation and Determination of Flavones in Biological Samples Using Zinc Complexation Coupled with High-Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Chenghe Sun

    2016-08-01

    Full Text Available Chlorophyll-type contaminants are commonly encountered in the isolation and determination of flavones of plant aerial plant parts. Heme is also a difficult background substance in whole blood analysis. Both chlorophyll and heme are porphyrin type compounds. In this study, a rapid method for isolating flavones with 5-hydroxyl or ortho-hydroxyl groups from biological samples was developed based on the different solubilities of porphyrin-metal and flavone-metal complexes. It is important that other background substances, e.g., proteins and lipids, are also removed from flavones without an additional processing. The recoveries of scutellarin, baicalin, baicalein, wogonoside and wogonin, which are the primary constituents of Scutellaria baicalensis (skullcaps were 99.65% ± 1.02%, 98.98% ± 0.73%, 99.65% ± 0.03%, 97.59% ± 0.09% and 95.19% ± 0.47%, respectively. As a sample pretreatment procedure, this method was coupled to high-performance liquid chromatography (HPLC with good separation, sensitivity and linearity and was applied to determine the flavone content in different aerial parts of S. baicalensis and in dried blood spot samples.

  8. Novel approaches in analysis of Fusarium mycotoxins in cereals employing ultra performance liquid chromatography coupled with high resolution mass spectrometry

    International Nuclear Information System (INIS)

    Rapid, simple and cost-effective analytical methods with performance characteristics matching regulatory requirements are needed for effective control of occurrence of Fusarium toxins in cereals and cereal-based products to which they might be transferred during processing. Within this study, two alternative approaches enabling retrospective data analysis and identification of unknown signals in sample extracts have been implemented and validated for determination of 11 major Fusarium toxins. In both cases, ultra-high performance liquid chromatography (U-HPLC) coupled with high resolution mass spectrometry (HR MS) was employed. 13C isotopically labeled surrogates as well as matrix-matched standards were employed for quantification. As far as time of flight mass analyzer (TOF-MS) was a detection tool, the use of modified QuEChERS (quick easy cheap effective rugged and safe) sample preparation procedure, widely employed in multi-pesticides residue analysis, was shown as an optimal approach to obtain low detection limits. The second challenging alternative, enabling direct analysis of crude extract, was the use of mass analyzer based on Orbitrap technology. In addition to demonstration of full compliance of the new methods with Commission Regulation (EC) No. 401/2006, also their potential to be used for confirmatory purposes according to Commission Decision 2002/657/EC has been critically assessed.

  9. High performance liquid chromatography coupled to mass spectrometry for profiling and quantitative analysis of folate monoglutamates in tomato.

    Science.gov (United States)

    Tyagi, Kamal; Upadhyaya, Pallawi; Sarma, Supriya; Tamboli, Vajir; Sreelakshmi, Yellamaraju; Sharma, Rameshwar

    2015-07-15

    Folates are essential micronutrients for animals as they play a major role in one carbon metabolism. Animals are unable to synthesize folates and obtain them from plant derived food. In the present study, a high performance liquid chromatography coupled to mass spectrometric (HPLC-MS/MS) method was developed for the high throughput screening and quantitative analysis of folate monoglutamates in tomato fruits. For folate extraction, several parameters were optimized including extraction conditions, pH range, amount of tri-enzyme and boiling time. After processing the extract was purified using ultra-filtration with 10 kDa membrane filter. The ultra-filtered extract was chromatographed on a RP Luna C18 column using gradient elution program. The method was validated by determining linearity, sensitivity and recovery. This method was successfully applied to folate estimation in spinach, capsicum, and garden pea and demonstrated that this method offers a versatile approach for accurate and fast determination of different folate monoglutamates in vegetables. PMID:25722141

  10. Speciation of vanadium in oilsand coke and bacterial culture by high performance liquid chromatography inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Li, X Sherry; Glasauer, Susan; Le, X Chris

    2007-10-17

    A simple and sensitive method for the speciation of vanadium(III), (IV), and (V) was developed by using high performance liquid chromatography and inductively coupled plasma mass spectrometry (HPLC-ICPMS). The EDTA-complexed vanadium species were separated on a strong anion exchange column with an eluent containing 2 mM EDTA, 3% acetonitrile, and 80 mM ammonium bicarbonate at pH 6. Each analysis was complete in 5 min. The detection limits were 0.6, 0.7 and 1.0 microg L(-1) for V(III), V(IV), and V(V), respectively. The method was applied to coke pore water samples from an oilsand processing/upgrading site in Fort McMurray, Alberta, Canada and to Shewanella putrefaciens CN32 bacterial cultures incubated with V(V). In the coke pore water samples, V(IV) and V(V) were found to be the major species. For the first time, V(III) was detected in the bacterial cultures incubated with V(V). PMID:17936102

  11. Speciation of vanadium in oilsand coke and bacterial culture by high performance liquid chromatography inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Li, X. Sherry [Department of Chemistry, University of Alberta, Edmonton, Alberta T6G 2G2 (Canada); Le, X. Chris [Department of Chemistry, University of Alberta, Edmonton, Alberta T6G 2G2 (Canada); Analytical and Environmental Toxicology, Department of Laboratory Medicine and Pathology, University of Alberta, Edmonton, Alberta T6G 2G3 (Canada)], E-mail: xc.le@ualberta.ca

    2007-10-17

    A simple and sensitive method for the speciation of vanadium(III), (IV), and (V) was developed by using high performance liquid chromatography and inductively coupled plasma mass spectrometry (HPLC-ICPMS). The EDTA-complexed vanadium species were separated on a strong anion exchange column with an eluent containing 2 mM EDTA, 3% acetonitrile, and 80 mM ammonium bicarbonate at pH 6. Each analysis was complete in 5 min. The detection limits were 0.6, 0.7 and 1.0 {mu}g L{sup -1} for V(III), V(IV), and V(V), respectively. The method was applied to coke pore water samples from an oilsand processing/upgrading site in Fort McMurray, Alberta, Canada and to Shewanella putrefaciens CN32 bacterial cultures incubated with V(V). In the coke pore water samples, V(IV) and V(V) were found to be the major species. For the first time, V(III) was detected in the bacterial cultures incubated with V(V)

  12. Speciation of vanadium in oilsand coke and bacterial culture by high performance liquid chromatography inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    A simple and sensitive method for the speciation of vanadium(III), (IV), and (V) was developed by using high performance liquid chromatography and inductively coupled plasma mass spectrometry (HPLC-ICPMS). The EDTA-complexed vanadium species were separated on a strong anion exchange column with an eluent containing 2 mM EDTA, 3% acetonitrile, and 80 mM ammonium bicarbonate at pH 6. Each analysis was complete in 5 min. The detection limits were 0.6, 0.7 and 1.0 μg L-1 for V(III), V(IV), and V(V), respectively. The method was applied to coke pore water samples from an oilsand processing/upgrading site in Fort McMurray, Alberta, Canada and to Shewanella putrefaciens CN32 bacterial cultures incubated with V(V). In the coke pore water samples, V(IV) and V(V) were found to be the major species. For the first time, V(III) was detected in the bacterial cultures incubated with V(V)

  13. Novel approaches in analysis of Fusarium mycotoxins in cereals employing ultra performance liquid chromatography coupled with high resolution mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zachariasova, M.; Lacina, O.; Malachova, A.; Kostelanska, M.; Poustka, J. [Institute of Chemical Technology, Faculty of Food and Biochemical Technology, Department of Food Chemistry and Analysis, Technicka 3, 166 28 Prague 6 (Czech Republic); Godula, M. [Thermo Fisher Scientific, Czech Republic, Slunecna 27, 100 00 Prague 10 (Czech Republic); Hajslova, J., E-mail: jana.hajslova@vscht.cz [Institute of Chemical Technology, Faculty of Food and Biochemical Technology, Department of Food Chemistry and Analysis, Technicka 3, 166 28 Prague 6 (Czech Republic)

    2010-03-03

    Rapid, simple and cost-effective analytical methods with performance characteristics matching regulatory requirements are needed for effective control of occurrence of Fusarium toxins in cereals and cereal-based products to which they might be transferred during processing. Within this study, two alternative approaches enabling retrospective data analysis and identification of unknown signals in sample extracts have been implemented and validated for determination of 11 major Fusarium toxins. In both cases, ultra-high performance liquid chromatography (U-HPLC) coupled with high resolution mass spectrometry (HR MS) was employed. {sup 13}C isotopically labeled surrogates as well as matrix-matched standards were employed for quantification. As far as time of flight mass analyzer (TOF-MS) was a detection tool, the use of modified QuEChERS (quick easy cheap effective rugged and safe) sample preparation procedure, widely employed in multi-pesticides residue analysis, was shown as an optimal approach to obtain low detection limits. The second challenging alternative, enabling direct analysis of crude extract, was the use of mass analyzer based on Orbitrap technology. In addition to demonstration of full compliance of the new methods with Commission Regulation (EC) No. 401/2006, also their potential to be used for confirmatory purposes according to Commission Decision 2002/657/EC has been critically assessed.

  14. Determination of ethylenediaminetetraacetic acid in nuclear waste by high-performance liquid chromatography coupled with electro-spray mass spectrometry

    International Nuclear Information System (INIS)

    EDTA is a chelating agent that has been used in decontamination processes. Its quantification is required for nuclear waste management because it affects the mobility of radionuclides and metals in environment and, thus, can harm the safety of the storage. Ion-pair chromatography coupled with electro-spray mass spectrometry detection is a convenient method for quantitative analysis of EDTA but EDTA should be present as a single anionic chelate form. However, radioactive liquid wastes contain high concentrations of heavy metals and salts and consequently, EDTA is present as several chelates. Speciation studies were carried out to choose a metal cation to be added in excess to the solution to obtain a major chelate form. Fe is the predominant cation and Fe(III)-EDTA is thermodynamically favored but these speciation studies showed that ferric hydroxide precipitated above pH 2. Consequently, it was not possible to quantify EDTA as Fe(III)-EDTA complex. Therefore, Ni2+ was chosen but its use implied pretreatment with a base of the solution to eliminate Fe. Deuterated EDTA was used as tracer in order to validate the whole procedure, from the treatment with a base to the final analysis by HPLC-ESI-MS. This analytical method was successfully applied for EDTA quantification in two real effluents resulting from a nuclear liquid waste process. A recovery rate between 60 and 80% was obtained. The limit of detection of this method was determined at 34 * 10-9 mol L-1. (authors)

  15. Determination of ethylenediaminetetraacetic acid in nuclear waste by high-performance liquid chromatography coupled with electrospray mass spectrometry.

    Science.gov (United States)

    du Bois de Maquillé, Laurence; Renaudin, Laetitia; Goutelard, Florence; Jardy, Alain; Vial, Jérôme; Thiébaut, Didier

    2013-02-01

    EDTA is a chelating agent that has been used in decontamination processes. Its quantification is required for nuclear waste management because it affects the mobility of radionuclides and metals in environment and, thus, can harm the safety of the storage. Ion-pair chromatography coupled with electrospray mass spectrometry detection is a convenient method for quantitative analysis of EDTA but EDTA should be present as a single anionic chelate form. However, radioactive liquid wastes contain high concentrations of heavy metals and salts and consequently, EDTA is present as several chelates. Speciation studies were carried out to choose a metal cation to be added in excess to the solution to obtain a major chelate form. Fe is the predominant cation and Fe(III)-EDTA is thermodynamically favored but these speciation studies showed that ferric hydroxide precipitated above pH 2. Consequently, it was not possible to quantify EDTA as Fe(III)-EDTA complex. Therefore, Ni(2+) was chosen but its use implied pretreatment with a base of the solution to eliminate Fe. Deuterated EDTA was used as tracer in order to validate the whole procedure, from the treatment with a base to the final analysis by HPLC-ESI-MS. This analytical method was successfully applied for EDTA quantification in two real effluents resulting from a nuclear liquid waste process. A recovery rate between 60 and 80% was obtained. The limit of detection of this method was determined at 34×10(-9)mol L(-1). PMID:23312862

  16. Monitoring the chemical and physical stability for tromethamine excipient in a lipid based formulation by HPLC coupled with ELSD.

    Science.gov (United States)

    Rodríguez, Shirley A; Qiu, Fenghe; Mulcey, Michael; Weigandt, Karen; Tamblyn, Toby

    2015-11-10

    Tromethamine, a UV-transparent amine base excipient, was used in the liquid phase of a self-emulsifying drug delivery system-soft gelatin capsule (SEDDS-SGC) formulation as an emulsification agent and to improve solubilization of the active drug. The level of this excipient was found to be decreasing in aged and stressed drug product capsules. The decrease could potentially affect oral bioavailability of the drug; should the amount of solubilizer decrease enough to lead to precipitation of the active drug from the formulation. Therefore, further investigation was warranted. HPLC coupled with evaporative light scattering detection (ELSD) was used to monitor the physical and chemical stability of tromethamine in the SEDDS-SGC formulation. Confirmation of the tromethamine interaction products was done by LC-MS. PMID:26254033

  17. Speciation of Selenium in Selenium-Enriched Sunflower Oil by High-Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry/Electrospray-Orbitrap Tandem Mass Spectrometry.

    Science.gov (United States)

    Bierla, Katarzyna; Flis-Borsuk, Anna; Suchocki, Piotr; Szpunar, Joanna; Lobinski, Ryszard

    2016-06-22

    The reaction of sunflower oil with selenite produces a complex mixture of selenitriglycerides with antioxidant and anticancer properties. To obtain insight into the identity and characteristics of the species formed, an analytical approach based on the combination of high-performance liquid chromatography (HPLC) with (78)Se-specific selenium detection by inductively coupled plasma mass spectrometry (ICP MS) and high-resolution (100 000), high mass accuracy (oil dissolved in isopropanol and methanol extract of the oil containing 65% selenium. HPLC-ICP MS showed 14 peaks, 11 of which could also be detected in the methanol extract. Isotopic patterns corresponding to molecules with one or two selenium atoms could be attributed by Orbitrap MS at the retention times corresponding to the HPLC-ICP MS peak apexes. Structural data for these species were acquired by MS(2) and MS(3) fragmentation of protonated or sodiated ions using high-energy collisional dissociation (HCD). A total of 11 selenium-containing triglycerol derivatives resulting from the oxidation of one or two double bonds of linoleic acid and analogous derivatives of glycerol-mixed linoleate(s)/oleinate(s) have been identified for the first time. The presence of these species was confirmed by the targeted analysis in the total oil isopropanol solution. Their identification corroborated the predicted elution order in reversed-phase chromatography: LLL (glycerol trilinoleate), LLO (glycerol dilinoleate-oleinate), LOO (glycerol linoleate-dioleinate), OOO (glycerol trioleinate), of which the extrapolation allowed for the prediction of the identity [glycerol dioleinate-stearate (OOS) and glycerol oleinate-distearate (OSS)] of the nonpolar species detected by ICP MS in the oil but not detected by electrospray MS. PMID:27214173

  18. Determination of the total drug-related chlorine and bromine contents in human blood plasma using high performance liquid chromatography-tandem ICP-mass spectrometry (HPLC-ICP-MS/MS).

    Science.gov (United States)

    Klencsár, Balázs; Bolea-Fernandez, Eduardo; Flórez, María R; Balcaen, Lieve; Cuyckens, Filip; Lynen, Frederic; Vanhaecke, Frank

    2016-05-30

    A fast, accurate and precise method for the separation and determination of the total contents of drug-related Cl and Br in human blood plasma, based on high performance liquid chromatography - inductively coupled plasma - tandem mass spectrometry (HPLC-ICP-MS/MS), has been developed. The novel approach was proved to be a suitable alternative to the presently used standard methodology (i.e. based on a radiolabelled version of the drug molecule and radiodetection), while eliminating the disadvantages of the latter. Interference-free determination of (35)Cl has been accomplished via ICP-MS/MS using H2 as reaction gas and monitoring the (35)ClH2(+) reaction product at mass-to-charge ratio of 37. Br could be measured "on mass" at a mass-to-charge of 79. HPLC was relied on for the separation of the drug-related entities from the substantial amount of inorganic Cl. The method developed was found to be sufficiently precise (repeatability 0.990) from the limit of quantification (0.05 and 0.01 mg/L for Cl and Br in blood plasma, respectively) to at least 5 and 1mg/L for Cl and Br, respectively. Quantification via either external or internal standard calibration provides reliable results for both elements. As a proof-of-concept, human blood plasma samples from a clinical study involving a newly developed Cl- and Br-containing active pharmaceutical ingredient were analysed and the total drug exposure was successfully described. Cross-validation was achieved by comparing the results obtained on Cl- and on Br-basis. PMID:26942335

  19. Plasma mitomycin C concentrations determined by HPLC coupled to solid-phase extraction.

    Science.gov (United States)

    Paroni, R; Arcelloni, C; De Vecchi, E; Fermo, I; Mauri, D; Colombo, R

    1997-04-01

    The aim of this study was to set up a method for quantification of plasma mitomycin C (MMC) concentrations during intravesical chemotherapy delivered in the presence of local bladder hyperthermia (HT). In comparison with existing methods, this assay, characterized by relative simplicity and efficiency, resulted in the facilitation of performance with nondedicated instrumentation or nonspecialized staff. Purification from plasma matrix was carried out by solid-phase extraction under vaccuum. The purified drug was then collected directly into the vials of the HPLC autosampler. Chromatographic analysis was performed on a reversed-phase C18 column with water:acetonitrile (85:15 by vol) as the mobile phase and the UV detector set at 365 nm. The use of porfiromycin as internal standard provided a method with good within-day precision (CV 6.0% at 5 micrograms/L, n = 6), linearity (0.5-50 micrograms/L), and specificity. The lower limit of detection (< or = 0.5 microgram/L) proved to be suitable for plasma pharmacokinetics monitoring in two tested patients treated with MMC + HT for superficial bladder cancer. PMID:9105262

  20. Characterization of the fermentation process by gas chromatography Lasiodiplodia theobromae and gas chromatography coupled with mass spectrometry

    International Nuclear Information System (INIS)

    Lasiodiplodia theobromae is a fungus, which has been reported by some authors as a high yield producer of the phytohormone jasmonic acid (JA). An indigenous strain of this fungus has been used for producing a fermentation broth with a high JA concentration by the Cuban Research Institute for Sugar Cane Derivatives (ICIDCA), registered as BIOJAS. The broth has been applied to some agricultural crops and demonstrated its economic feasibility as plant growth regulator and biological control of various phytopathogenic microorganisms and pests. Both fermentation broth and biomass from this fungus contain some other metabolites having bioactive properties, for instance, fatty acids. This paper shows the composition and quantification of fatty acids in the biomass using Gas Chromatography (GC) and the identification of substances profile in fermentation broth by Gas Chromatography coupled to Mass Spectrometry (GC-MS). The most fatty acids in the biomass are palmitic, stearic, oleic, linoleic and linolenic acids, being oleic acid the major component. On the other hand, 2,32 % of fatty acid esters; 2,47 % of alkenes; 14,40 % of alcohols; 30,15 % of aldehydes and 21,73 % of paraffins were detected in the composition of fermentation broth

  1. Simultaneous determination of dyes in wines by HPLC coupled to quadrupole orbitrap mass spectrometry.

    Science.gov (United States)

    Jia, Wei; Chu, Xiaogang; Ling, Yun; Huang, Junrong; Lin, Yuanhui; Chang, James

    2014-04-01

    A new method combining the QuEChERS (quick, easy, cheap, effective, rugged, and safe) method with ultra high performance liquid chromatography and ESI quadrupole Orbitrap high-resolution MS was developed for the highly accurate and sensitive screening of 69 dyes in wines. Response surface methodology was employed to optimize the QuEChERS sample preparation method for the determination of 69 different analytes in wines for the first time. After optimization, the maximum predicted recovery was 99.48% rate for canacert indigo carmine under the optimized conditions of 10 mL acetonitrile, 1.45 g sodium acetate, 107 mg primary secondary amine, and 96 mg C18 . For the matrices studied, the recovery rates of the other 68 compounds ranged from 87.2-107.4%, with coefficient of variation fast screening of different food additives. PMID:24478185

  2. Separation and Purification of Flavonoids from Black Currant Leaves by High-Speed Countercurrent Chromatography and Preparative HPLC

    OpenAIRE

    He, Dajun; Huang, Yun; Ayupbek, Amatjan; Gu, Dongyu; Yi YANG; Aisa, Haji Akber; Ito, Yoichiro

    2010-01-01

    High-speed countercurrent chromatography (HSCCC) has been successfully used for the preparative isolation of flavonoids from the ethyl acetate extracts of black currant leaves. The HSCCC separation was performed with a two-phase solvent system composed of n-hexane/EtOAc/MeOH/H2O (1:10:1:10, v/v) at a flow rate of 1.5 mL/min. When the flow rate was increased from 1.0 to 3.0 mL/min, the retention of stationary phase decreased from 60.3% to 39.7% resulting in loss of peak resolution, while the s...

  3. Determination of organoarsenic species in marine samples using gradient elution cation exchange HPLC-ICP-MS

    DEFF Research Database (Denmark)

    Sloth, Jens Jørgen; Larsen, Erik Huusfeldt; Julshamn, Kåre

    2003-01-01

    A method for the determination of arsenic species in marine samples using high performance liquid chromatography coupled to inductively coupled mass spectrometry (HPLC-ICP-MS) has been developed. Cation exchange HPLC with gradient elution using pyridine formate as the mobile phase was employed for...... the separation of a large number of arsenicals that occurred in the samples. The arsenic species were extracted using a 50% (v/v) methanol-water mixture and mechanical agitation overnight. The effect of the sample matrix on HPLC retention time was investigated and showed a dramatic effect for...

  4. Determination of Oxidized Phosphatidylcholines by Hydrophilic Interaction Liquid Chromatography Coupled to Fourier Transform Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Pia Sala

    2015-04-01

    Full Text Available A novel liquid chromatography-mass spectrometry (LC-MS approach for analysis of oxidized phosphatidylcholines by an Orbitrap Fourier Transform mass spectrometer in positive electrospray ionization (ESI coupled to hydrophilic interaction liquid chromatography (HILIC was developed. This method depends on three selectivity criteria for separation and identification: retention time, exact mass at a resolution of 100,000 and collision induced dissociation (CID fragment spectra in a linear ion trap. The process of chromatography development showed the best separation properties with a silica-based Kinetex column. This type of chromatography was able to separate all major lipid classes expected in mammalian samples, yielding increased sensitivity of oxidized phosphatidylcholines over reversed phase chromatography. Identification of molecular species was achieved by exact mass on intact molecular ions and CID tandem mass spectra containing characteristic fragments. Due to a lack of commercially available standards, method development was performed with copper induced oxidation products of palmitoyl-arachidonoyl-phosphatidylcholine, which resulted in a plethora of lipid species oxidized at the arachidonoyl moiety. Validation of the method was done with copper oxidized human low-density lipoprotein (LDL prepared by ultracentrifugation. In these LDL samples we could identify 46 oxidized molecular phosphatidylcholine species out of 99 possible candidates.

  5. Ultra-Sensitive Elemental Analysis Using Plasmas 5.Speciation of Arsenic Compounds in Biological Samples by High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry System

    Science.gov (United States)

    Kaise, Toshikazu

    Arsenic originating from the lithosphere is widely distributed in the environment. Many arsenicals in the environment are in organic and methylated species. These arsenic compounds in drinking water or food products of marine origin are absorbed in human digestive tracts, metabolized in the human body, and excreted viatheurine. Because arsenic shows varying biological a spects depending on its chemical species, the biological characteristics of arsenic must be determined. It is thought that some metabolic pathways for arsenic and some arsenic circulation exist in aqueous ecosystems. In this paper, the current status of the speciation analysis of arsenic by HPLC/ICP-MS (High Performance Liquid Chromatography-Inductively Coupled Plasma Mass spectrometry) in environmental and biological samples is summarized using recent data.

  6. Stir bar sorptive extraction combined with high performance liquid chromatography-ultraviolet/inductively coupled plasma mass spectrometry for analysis of thyroxine in urine samples.

    Science.gov (United States)

    Fan, Wenying; Mao, Xiangju; He, Man; Chen, Beibei; Hu, Bin

    2013-11-29

    tIn this work, polyethyleneglycol (PEG)/hydroxyl polydimethylsiloxane (OH-PDMS)/γ -mercaptopropyltrimethoxysilane (γ -MPTS) coated stir bar was prepared by sol–gel process and its extraction performance for the extraction of amphoteric thyroxines (3,3',5,5'-tetraiodothyronin, T(4); 3,3',5-triiodothyronine, T(3); reversed-3,3',5-triiodothyronine, rT(3)) and their metabolite (3,5-diiodothyronine,T2) was studied. The preparation reproducibility of PEG/OH-PDMS/γ -MPTS coated stir bar was investigated, and the relative standard deviations (RSDs) in the same batch and among different batches were 3.3–14.3% (n = 5) and 7.7–16.6% (n = 3), respectively. The prepared PEG/OH-PDMS/γ -MPTS coated stir bar could be reused for more than 20 times. Based on this fact, a novel method of stir bar sorptive extraction (SBSE) combined with high performance liquid chromatography (HPLC)-ultraviolet (UV)and HPLC-inductively coupled plasma mass spectrometry (ICP-MS) for the analysis of target thyroxinesin human urine samples was developed. The influencing factors of SBSE, such as sample pH, extraction time, stirring rate, salt effect, desorption solution and desorption time, were studied in detail, and the analytical performance of the proposed method was evaluated under the optimized conditions. The enrichment factors (EFs) of the developed method for four target thyroxines were in the range of 14.9–70.4(theoretical enrichment factor was 100). The RSDs were ranging from 4.0% to 13.8% for SBSE-HPLC-UV (c = 25 μg/L, n = 6) and from 3.7% to 6.1% for SBSE-HPLC-ICP-MS (c = 0.5 μg/L, n = 5). The linear range obtained by SBSE-HPLC-UV was 2–500 μg/L for T(2)and 5–500 μg/L for rT3, T(3)and T(4), with correlation coefficients (r) ranging from 0.9957 to 0.9998, respectively, while the linear range obtained by SBSE-HPLC-ICP-MS was 0.05–500 μg/L for T(2) and rT(3), 0.10–200 μg/L for T(3) and 0.05–200 μg/L for T(4)with r ranging from 0.9979 to 0.9998, respectively. The

  7. Comparative assessment of irradiated proteins in potato tuber with untreated control by high performance liquid chromatography (HPLC) and gel electrophoresis

    International Nuclear Information System (INIS)

    About 2% of the weight of potato tuber is composed of proteins. In spite of their low quantity the proteins play a key role in the physiological activities leading to the break of the dormancy period and start of the cell division. This causes sprouting and also greening due to chlorophyll formation. This in turn is always accompanied by the production of the glycoalkaloid solanine in the flesh of tuber. For evaluation of radiation effect (dose range 50-250 Gy) and probable structural changes (amino acid release), analysis of selected proteins (molecular range 5 x 104 - 2 x 105 Dalton) of potato tuber in both irradiated and control type by HPLC showed no considerable changes in retention times, but qualitative assessment of amino acids by Pico-TagTM Pre-derivatizing method had some changes in quantity of amino acids like lysine which was increased 1 month after irradiation while Glutamic acid had considerable decreasment after the same time of irradiation. (Author)

  8. Imidacloprid Extraction from Citrus Leaves and Analysis by Liquid Chromatography-Mass Spectrometry (HPLC-MS/MS).

    Science.gov (United States)

    Leiva, Jorge A; Nkedi-Kizza, Peter; Borejsza-Wysocki, Wlodzimierz S; Bauder, Victor S; Morgan, Kelly T

    2016-05-01

    A procedure was developed to extract Imidacloprid (IMD) from newly-flushed and fully-expanded citrus leaves. The extraction was conducted in a bullet blender, using a small sample mass (0.5 g of fresh tissue), stainless-steel beads (24 g), and methanol as extractant (10 mL). The extracts did not require further clean-up before analysis by HPLC-MS/MS. The method was validated with control samples from IMD-untreated Hamlin orange trees. The method limit of detection and limit of quantitation were 0.04 and 0.12 μg g(-1), respectively. IMD recoveries from fortified leaf tissue were between 92 % and 102 %, with relative standard deviations of <8 %. The method was further evaluated by extracting leaves from Hamlin orange trees treated with IMD. The treated trees showed maximum concentrations of 10.8 and 21.8 µg g(-1), observed at 20 days after applying two soil-drenching rates (0.51 and 1.02 kg IMD ha(-1)), respectively. This extraction technique will generate useful data on IMD plant uptake, foliar concentration, and correlations with Asian citrus psyllid (ACP) mortality or control. The method could be used to generate baseline data to improve IMD soil-drenching applications as the main management practice to control the ACP. PMID:26988226

  9. Ultrasound-assisted enzymatic hydrolysis for iodinated amino acid extraction from edible seaweed before reversed-phase high performance liquid chromatography-inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Romarís-Hortas, Vanessa; Bermejo-Barrera, Pilar; Moreda-Piñeiro, Antonio

    2013-09-27

    The combination of reverse phase high performance liquid chromatography (RP-HPLC) with inductively coupled plasma mass spectrometry (ICP-MS) was used for the determination of monoiodotyrosine (MIT) and diiodotyrosine (DIT) in edible seaweed. A sample pre-treatment based on ultrasound assisted enzymatic hydrolysis was optimized for the extraction of these iodinated amino acids. Pancreatin was selected as the most adequate type of enzyme, and parameters affecting the extraction efficiency (pH, temperature, mass of enzyme and extraction time) were evaluated by univariate approaches. In addition, extractable inorganic iodine (iodide) was also quantified by anion exchange high performance liquid chromatography (AE-HPLC) coupled with ICP-MS. The proposed procedure offered limits of detection of 1.1 and 4.3ngg(-1) for MIT and DIT, respectively. Total iodine contents in seaweed, as well as total iodine in enzymatic digests were measured by ICP-MS after microwave assisted alkaline digestion with tetramethylamonium hydroxide (TMAH) for total iodine assessment, and also by treating the pancreatin extracts (extractable total iodine assessment). The optimized procedure was successfully applied to five different types of edible seaweed. The highest total iodine content, and also the highest iodide levels, was found in the brown seaweed Kombu (6646±45μgg(-1)). Regarding iodinated amino acids, Nori (a red seaweed) was by far the one with the highest amount of both species (42±3 and 0.41±0.024μgg(-1) for MIT and DIT, respectively). In general, MIT concentrations were much higher than the amounts of DIT, which suggests that iodine from iodinated proteins in seaweed is most likely bound in the form of MIT residues. PMID:23972456

  10. 局所麻酔薬8種のHPLC-MSによる分離分析法とSSI及びAPCI法の感度比較

    OpenAIRE

    有信, 哲哉; 服部, 秀樹; 岩井, 雅枝; 妹尾, 洋; 石井, 晃; 熊澤, 武志; 鈴木, 修

    2002-01-01

    We have developed a rapid determination method for local anesthetics of tetracaine, procaine, benzoxinate, dibucaine, lidocaine, bupivacaine and mepivacaine by high-performance liquid chromatography (HPLC)-mass spectrometry (MS) coupled with a diol-bonded silica gel HPLC column that enabled direct injection of biological samples. We have also compared the sensitivities for the drags by sonic spray ionization (SSI) and atmospheric pressure chemical ionization (APCI). Those by HPLC-SSI-MS for t...

  11. Investigation of mercury-containing proteins by enriched stable isotopic tracer and size-exclusion chromatography hyphenated to inductively coupled plasma-isotope dilution mass spectrometry

    International Nuclear Information System (INIS)

    In order to investigate trace mercury-containing proteins in maternal rat and their offspring, a method of enriched stable isotopic tracer (196Hg and 198Hg) combined with size-exclusion chromatography (SEC) coupled to inductively coupled plasma-isotope dilution mass spectrometry (ICP-IDMS) was developed. Prior to the analysis, 196Hg- and 198Hg-enriched methylmercury was administrated to the pregnant rats. Then the mercury-containing proteins in serum and brain cytosol of the dam and pup rats were separated by size-exclusion columns and the mercury was detected by ICP-MS. The ICP-MS spectrogram of the tracing samples showed significantly elevated 196Hg and 198Hg isotopic signals compared with the natural ones, indicating that the detection sensitivity could be increased by the tracer method. The contents of mercury in chromatographic fractions of the dam and pup rat brain cytosol were quantitatively estimated by post-column reverse ID-ICP-MS. The quantitative speciation differences of mercury in brain cytosol between the dam and pup rats were observed, indicating that such studies could be useful for toxicological estimation. Additionally, the isotopic ratio measurement of 198Hg/202Hg in the tracing samples could be used to identify the artifact mercury species caused in the analytical procedure. The study demonstrates that the tracer method combined with high-performance liquid chromatography (HPLC)-ICP-IDMS could provide reliably qualitative and quantitative information on mercury-containing proteins in organisms

  12. Increasing Protein Identifications Using a Novel HPLC-Chip Coupled to a Q-TOF Mass Spectrometer

    OpenAIRE

    Buckenmaier, Stephan; Miller, Christine; Perkins, Pat; Staples, Greg; Yin, Honfeng; Greiner, Martin; Van de Goor, Tom; Potter, Oscar

    2013-01-01

    Since its introduction in 2005, HPLC-Chip/MS technology has proven to be a powerful solution to the challenges associated with Nano-HPLC-MS, simplifying set-up and maintenance whilst overcoming conventional limitations in robustness and reproducibility. Integration of connections, lines, valves and an electrospray tip onto HPLC-Chips provides simplicity of use and robustness at nanoflow scale separations. This allows for enhanced productivity plus generation of consistent results obtained fro...

  13. Determination of taxonomic status of chinese species of the genus clematis by using high performance liquid chromatography-mass spectrometry (HPLC-MS) technique

    International Nuclear Information System (INIS)

    A comparative taxonomic study using chemometric and numerical taxonomic approaches on 15 populations of 12 species of major taxa of the genus Clematis, belonging to sections, Rectae, Clematis, Meclatis, Tubulosae and Viorna were analyzed by HPLC coupled with diode array detector and ESI-MS. The chemo diversity profile of saponins proved to be useful taxonomic markers for the genus and results are presented in pheno grams. The compound 'Huzhangoside D' was the most abundant in analyzed species of the genus. Numerical taxonomic study was also conducted based on phylogenetically informative characters which corroborated with chemical fingerprinting findings. The significance of chemical markers in taxonomic study as well as their correlation between morphology and chemical compound profile is also debated with its significant role in botanic drugs identification. (author)

  14. On-line DACC-HPLC analysis of polycyclic aromatic hydrocarbons in edible oils

    OpenAIRE

    Neđeral, Sandra; Pukec, Dragutin; Škevin, Dubravka; Kraljić, Klara; Obranović, Marko; Zrinjan, Petra

    2014-01-01

    In this work an HPLC method for determination of polycyclic aromatic hydrocarbons (PAH) in edible oils on a DACC (donor-acceptor complex chromatography) column coupled with an on-line HPLC system with fluorescent detection. Method was used to determine the content of individual PAHs in the refined sunflower oil, virgin olive oil, cold pressed pumpkin seed oil, dark sesame oil and pumpkin seed oil produced with roasting obtained from domestic market. Calibration and validation were conducted f...

  15. Polyphenolic profile characterization of Agrimonia eupatoria L. by HPLC with different detection devices

    OpenAIRE

    Correia, Helena; González-Paramás, Ana; Amaral, Maria Teresa; Santos-Buelga, Celestino; Batista, Maria Teresa

    2006-01-01

    Liquid chromatography coupled to diode array and electrospray ionization mass spectrometry detection was used to establish the polyphenolic profile of an ethyl acetate fraction from Agrimonia eupatoria L. aqueous-alcoholic extract. Additionally, an HPLC technique with post-column derivatization by p-dimethylaminocinnamaldehyde was employed for the selective detection and quantification of flavan-3-ols. Important information was obtained by combining the data of these two HPLC techniques. Flav...

  16. Purification and identification of endogenous antioxidant and ACE-inhibitory peptides from donkey milk by multidimensional liquid chromatography and nanoHPLC-high resolution mass spectrometry.

    Science.gov (United States)

    Zenezini Chiozzi, Riccardo; Capriotti, Anna Laura; Cavaliere, Chiara; La Barbera, Giorgia; Piovesana, Susy; Samperi, Roberto; Laganà, Aldo

    2016-08-01

    Donkey milk is a valuable product for the food industry due to its nutraceutical, nutritional, and functional properties. In this work, the endogenous peptides from donkey milk were investigated for their antioxidant and ACE-inhibitory activities, combining a two-dimensional peptide fractionation strategy with high-resolution mass spectrometry, bioinformatics analysis, and in vitro assays. After extraction, the endogenous peptides were fractionated twice, first by polymeric reversed phase and then by hydrophilic interaction chromatography. Fractions were screened for the investigated bioactivities and only the most active ones were finally analyzed by nanoRP-HPLC-MS/MS; this approach allowed to reduce the total number of possible bioactive sequences. Results were further mined by in silico analysis using PeptideRanker, BioPep, and PepBank, which provided a bioactivity score to the identified peptides and matched sequences to known bioactive peptides, in order to select candidates for chemical synthesis. Thus, five peptides were prepared and then compared to the natural occurring ones, checking their retention times and fragmentation patterns in donkey milk alone and in spiked donkey milk samples. Pure peptide standards were finally in vitro tested for the specific bioactivity. In this way, two novel endogenous antioxidant peptides, namely EWFTFLKEAGQGAKDMWR and GQGAKDMWR, and two ACE-inhibitory peptides, namely REWFTFLK and MPFLKSPIVPF, were successfully validated from donkey milk. Graphical Abstract Analytical workflow for purification and identification of bioactive peptides from donkey milk sample. PMID:27325462

  17. DETERMINATION AND COMPARISON OF MAJOR POLYPHENOL OF FOUR RED FRUITS USING HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC WITH DIODE-ARRAY DETECTION

    Directory of Open Access Journals (Sweden)

    Khatereh Khorsandi

    2013-12-01

    Full Text Available Polyphenols are ubiquitous compounds in plants which are abundant micronutrients in our diet. They got more attention in recent years due to their bioactive functions and health effects on many diseases such as cancer. These components are secondary plant metabolites that function as antimicrobial, antiviral and anti-inflammatory compounds. Extraction of these compounds from plants and fruits and in vitro and in vivo study of their various health effects has been subject of many researches. The objective of this study was to investigate the profiles of polyphenolic compounds in apple, red grape, sour cherry and pomegranate fruit juices and comparison of the phenolic contents of various juices. Major polyphenolic compounds of four different concentrated fruit juices from various industries were analyzed and characterized by liquid chromatography. RP-HPLC-DAD was used in our study as powerful and accurate method. The total and individual polyphenolic compounds differed significantly among the four selected red fruit juices. Among the tested juices, sour cherry and apple juices had the highest and the lowest contents of phenolic compounds, respectively.

  18. QUANTITATIVE DETERMINATION OF ETORICOXIB AND PARACETAMOL IN PHARMACEUTICAL DOSAGE FORM AND IN-VITRO COMPARISON BY REVERSED-PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHY (RP-HPLC

    Directory of Open Access Journals (Sweden)

    MAITREYI ZAVERI, AMIT KHANDHAR

    2013-10-01

    Full Text Available The objective of this present work was todevelop and validate analytical method for quantitativedetermination of Paracetamol and Etoricoxib in a tabletformulation and also the comparison of invitro data withreference dosage form. Chromatographic separations of thetwo drugs were analyzed on a Kromasil C18 column (25cmX 4.6mm, 5 m. The mobile phase constituted of Buffer:Acetonitirile with gradient program was delivered at theflow rate 1.0 mL/min. Detection was performed at 220 nm.Separation was completed within 20 min. Calibrationcurves were linear with coefficient correlation between0.99 to 1.0 over a concentration range of 48 to 146 g/mLof Paracetamol and 6 to 19 g/mL for Etoricoxibrespectively. The relative standard deviation (R.S.D wasfound to be less than 2.0%. Analysis for dissolution studywas also performed by Reversed-Phase High PerformanceLiquid Chromatography (RP-HPLC method. Differencefactor (f1 were found to be 2.85 and 3.83 and similarityfactor (f2 were found to be 73.514 and 68.961 forParacetamol and Etoricoxib respectively.

  19. Speciation of arsenic in environmental samples of the Nha Trang Harbor, Vietnam, using HPLC coupled HG-AAS.

    Science.gov (United States)

    Le, Lan Anh; Trinh, Anh Duc; Nguyen, Dinh Thuat; Bui, Minh Ly

    2011-04-01

    A coupled high performance liquid chromatography-hydride generation-atomic absorption spectroscopy system was used to determine the speciation of arsenic in samples from the Nha Trang Harbor, Vietnam. Concentrations of arsenic in seawater, pore water, suspended solid, and sediment were 4.12-9.81 μg/L, 13.10-24.32 μg/L, 1.87-6.42 μg/g, and 3.37-9.06 μg/g, respectively. Extraction using H(3)PO(4) + NH(2)OH·HCl and ultrasonic digestion was optimized to yield a 76-85% of total arsenic. Arsenic (III) was the most abundant species in suspended solids and sediments whereas arsenic (V) represented for 30-50% of arsenic (III) concentration. Monomethylarsonic acid and dimethylarsinic acid species were undetectable. PMID:21365299

  20. Simultaneous determination of ten underivatized biogenic amines in meat by liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).

    Science.gov (United States)

    Sirocchi, Veronica; Caprioli, Giovanni; Ricciutelli, Massimo; Vittori, Sauro; Sagratini, Gianni

    2014-09-01

    Biogenic amines (BAs) are considered to be important indicators of freshness and quality in food. In this work, an analytical method for analyzing ten underivatized BAs in meat by performance liquid chromatography-tandem mass spectrometry has been developed. Comparison between ion trap and triple quadrupole as mass analyzers indicated that the latter provides greater sensitivity and selectivity. The range of the correlation coefficients of the calibration curves of the analyzed compounds was 0.987-0.999, and the limits of detection and limits of quantification were in the range of 0.002-0.1 mg l(-1) and 0.008-0.5 mg l(-1), respectively. Once validated, the method was used to analyze the concentrations of BAs in 16 commercial meat samples, for evaluating the freshness of food through the study of BA indices, i.e. biogenic amine index (BAI) and the ratio spermidine/spermine (SPD/SPE). The results indicated that all the samples were fresh, with a BAI lower than 1.49 mg kg(-1) and a SPD/SPE ratio lower than 0.41 in each case. This methodology for testing the freshness of meat has potential for quality control applications along the entire production chain of meat products. PMID:25230178

  1. Separation and identification of polyphenols in apple pomace by high-speed counter-current chromatography and high-performance liquid chromatography coupled with mass spectrometry.

    Science.gov (United States)

    Cao, Xueli; Wang, Cong; Pei, Hairun; Sun, Baoguo

    2009-05-01

    Apple pomace, a by-product in the processing of apple juice, was investigated as a potential source of polyphenols. Two methods of separation and purification of polyphenols from apple pomace extract were established by combination of gel chromatography with high-speed counter-current chromatography (HSCCC) and solvent extraction with HSCCC, respectively. The optimal separation was performed on a Sephadex LH-20 column using gradient aqueous ethanol as eluting solvent from 0% to 100% in increments of 10%. HPLC analysis indicated that main polyphenols existed in fractions eluted between 40% and 50% aqueous ethanol. The fractions of interest from column were separated by HSCCC with the solvent system hexane-ethyl acetate-1% aqueous acetic acid (0.5:9.5:10, v/v/v). Ethyl acetate fractionation of the apple pomace extract followed by direct HSCCC separation by the same solvent system in the volume ratio of 1:9:10 also produced a good separation of the main polyphenols of interest. Six high-purity polyphenols were achieved tentatively and identified by HPLC/MS: chlorogenic acid (1, m/z 354), quercetin-3-glucoside/quercetin-3-glacaside (2, m/z 464), quercetin-3-xyloside (3, m/z 434), phloridzin (4, m/z 436), quercetin-3-arabinoside (5, m/z 434), and quercetin-3-rhamnoside (6, m/z 448). These results provided a preliminary foundation for further development and exploration of apple pomace. PMID:19203755

  2. Stationary phase modulation in liquid chromatography through the serial coupling of columns: A review.

    Science.gov (United States)

    Alvarez-Segura, T; Torres-Lapasió, J R; Ortiz-Bolsico, C; García-Alvarez-Coque, M C

    2016-06-01

    Liquid chromatography with single columns often does not succeed in the analysis of complex samples, in terms of resolution and analysis time. A relatively simple solution to enhance chromatographic resolution is the modulation of the stationary phase through the serial coupling of columns. This can be implemented with any type of column using compatible elution conditions and conventional instruments. This review describes the key features of column coupling and published procedures, where two or more columns were coupled in series to solve separation problems. In all reports, the authors could not resolve their samples with single columns, whereas significant enhancement in chromatographic performance was obtained when the columns were combined. Particularly interesting is the reduction in the analysis time in the isocratic mode, which alleviates the "general elution problem" of liquid chromatography, and may represent a stimulus for the proposal of new procedures, especially in combination with mass spectrometric, electrochemical and refractometric detection. Developments proposed to make the serial coupling of columns useful in routine and research laboratories are outlined, including optimisation strategies that facilitate the selection of the appropriate column combination and elution conditions (solvent content, flow rate or temperature) in both isocratic and gradient modes. The availability of zero dead volume couplers, able to connect standard columns, and the commercialisation of short columns with multiple lengths, have expanded the possibilities of success. PMID:27155298

  3. Direct and sensitive determination of glyphosate and aminomethylphosphonic acid in environmental water samples by high performance liquid chromatography coupled to electrospray tandem mass spectrometry.

    Science.gov (United States)

    Guo, Hongyue; Riter, Leah S; Wujcik, Chad E; Armstrong, Daniel W

    2016-04-22

    A novel method based on high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) was developed for the sensitive determination of glyphosate and its major degradation product, AMPA in environmental water samples. The method involves the use of MS compatible mobile phases (0.1% formic acid in water and acetonitrile) for HPLC and direct analysis of water samples without sample derivatization. The method has been validated in different types of water matrices (drinking, surface and groundwater) by accuracy and precision studies with samples spiked at 0.1, 7.5 and 90 ppb. All mean accuracy values ranged from 85% to 112% for glyphosate and AMPA using both primary and secondary quantitative ion transitions (RSD ≤ 10%). Moreover, both primary and secondary ion transitions for glyphosate and AMPA can achieve the quantitation limits at 0.1 ppb. The linear dynamic range of the calibration curves were from 0.1 to 100 ppb for each analyte at each ion transitions with correlation coefficient higher than 0.997. PMID:26993781

  4. Determination of Polymer Additives-Antioxidants, Ultraviolet Stabilizers, Plasticizers and Photoinitiators in Plastic Food Package by Accelerated Solvent Extraction Coupled with High-Performance Liquid Chromatography.

    Science.gov (United States)

    Li, Bo; Wang, Zhi-Wei; Lin, Qin-Bao; Hu, Chang-Ying; Su, Qi-Zhi; Wu, Yu-Mei

    2015-07-01

    An analytical method for the quantitative determination of 4 antioxidants, 9 ultraviolet (UV) stabilizers, 12 phthalate plasticizers and 2 photoinitiators in plastic food package using accelerated solvent extraction (ASE) coupled with high-performance liquid chromatography-photodiode array detector (HPLC-PDA) has been developed. Parameters affecting the efficiency in the process such as extraction and chromatographic conditions were studied in order to determine operating conditions. The analytical method of ASE-HPLC showed good linearity with good correlation coefficients (R ≥ 0.9833). The limits of detection and quantification were between 0.03 and 0.30 µg mL(-1) and between 0.10 and 1.00 µg mL(-1) for 27 analytes. Average spiked recoveries for most analytes in samples were >70.4% at 10, 20 and 40 µg g(-1) spiked levels, except UV-9 and Irganox 1010 (58.6 and 64.0% spiked at 10 µg g(-1), respectively), the relative standard deviations were in the range from 0.4 to 15.4%. The methodology has been proposed for the analysis of 27 polymer additives in plastic food package. PMID:25472804

  5. Molecularly imprinted polymer cartridges coupled on-line with high performance liquid chromatography for simple and rapid analysis of human insulin in plasma and pharmaceutical formulations.

    Science.gov (United States)

    Moein, Mohammad Mahdi; Javanbakht, Mehran; Akbari-adergani, Behrouz

    2014-04-01

    In this paper, a novel method is described for automated determination of human insulin in biological fluids using principle of sequential injection on a molecularly imprinted solid-phase extraction (MISPE) cartridge as a sample clean-up technique combined with high performance liquid chromatography (HPLC). The water-compatible molecularly imprinted polymers (MIPs) were prepared using methacrylic acid as a functional monomer, ethylene glycol dimethacrylate as a cross-linker, chloroform as a porogen and insulin as a template molecule. The imprinted polymers were then employed as the solid-phase extraction sorbent for on-line extraction of insulin from human plasma samples. To achieve the best condition, influential parameters on the extraction efficiency were thoroughly investigated. Rapid and simple analysis of the hormone was successfully accomplished through the good selectivity of the prepared sorbent coupled with HPLC. Limits of detection (LOD) and quantification (LOQ) of 0.2 ng mL(-1), 0.7 ng mL(-1), and 0.03 ng mL(-1), 0.1 ng mL(-1) were obtained in plasma and urine respectively. The obtained data exhibited the great recoveries for extraction of insulin from human plasma and pharmaceutical samples, higher than 87%. PMID:24607106

  6. Quantitative coupling of supercritical fluid extraction and high-performance liquid chromatography by means of a coated open-tubular interface.

    Science.gov (United States)

    Stone, M A; Taylor, L T

    2001-10-01

    Supercritical fluid extraction was coupled on-line with reversed-phase high-performance liquid chromatography (HPLC). An open-tubular column with a 95% methyl-5% phenyl stationary phase was utilized as an interface between the two systems. This phase allowed for good analyte focusing onto the packed analytical column and exhibited low reactivity. Due to the non-polar nature of this phase there was a low tendency for analytes to be prematurely rinsed off the interface by condensed modifier. Using this approach, it was possible to transfer the extracted analytes quantitatively to the HPLC column in the presence of as much as 10% (v/v) methanol. By placing a 10 m guard column at the head of the interface, the same could be accomplished with ethanol as the modifier: allowing the extraction to be conducted entirely with non-toxic fluids. The method also allowed the use of very practical extraction parameters in terms of amount extracted, extraction flow-rate, extraction vessel volume, and extraction time. PMID:11695521

  7. Identification and Characterization of the Major Chemical Constituents in Fructus Akebiae by High-Performance Liquid Chromatography Coupled with Electrospray Ionization-Quadrupole-Time-of-Flight Mass Spectrometry.

    Science.gov (United States)

    Ling, Yun; Zhang, Qing; Zhu, Dan-dan; Chen, Fei; Kong, Xiu-hua; Liao, Liang

    2016-02-01

    Fructus Akebiae (FA), the dry fruit of Akebia quinata (THUNB.) DECNE., possesses potent antidepressant properties. Owing to the structural complexity, high polarity and thermal lability in plants, it is difficult and time-consuming to analyze the major chemical constituents by traditional strategies that involve extraction, isolation, purification and identification by chemical manipulations and spectroscopic methods. In this study, a high-performance liquid chromatography coupled with electrospray ionization-quadrupole-time-of-flight mass spectrometry (HPLC-ESI-Q-TOF-MS-MS) method was established for quickly identifying the chemical constituents in the extract of Fructus Akebiae. The main saponin components in the extract of Fructus Akebiae were detected with the HPLC-ESI-Q-TOF-MS-MS in negative-ion mode. These components were further analyzed by MS(2) spectra, and compared with the corresponding reference substances and literature data. Nineteen saponins in the extract of Fructus Akebiae were well separated in one run. The new method is accurate and rapid. It can be used to identify the main chemical constituents in the extract of Fructus Akebiae and can be suitable for the quality control of Fructus Akebiae. PMID:26311648

  8. Vortex-assisted liquid-liquid microextraction coupled with high performance liquid chromatography for the determination of furfurals and patulin in fruit juices.

    Science.gov (United States)

    Abu-Bakar, Nur-Bahiyah; Makahleh, Ahmad; Saad, Bahruddin

    2014-03-01

    A fast and simple solvent microextraction technique using salting out-vortex-assisted liquid-liquid microextraction (salting out-VALLME) was developed for the extraction of furfurals (2-furfural (2-F), 3-furfural (3-F), 5-methylfurfural (5-MF) and 5-hydroxymethylfurfural (5-HMF)) and patulin (PAT) in fruit juice samples. The optimum extraction conditions for 5 mL sample were: extraction solvent, 1-hexanol; volume of extractant, 200 µL; vortex time, 45 s; salt addition, 20%. The simultaneous determination of the furfurals and PAT were investigated using high performance liquid chromatography coupled with diode array detector (HPLC-DAD). The separation was performed using ODS Hypersil C18 column (4.6 mm i.d × 250 mm, 5 μm) under gradient elution. The detection wavelengths used for all compounds were 280 nm except for 3-F (210 nm). The furfurals and PAT were successfully separated in less than 9 min. Good linearities (r(2)>0.99) were obtained within the range 1-5000 μg L(-1) for all compounds except for 3-F (10-5000 µg L(-1)) and PAT (0.5-100 μg L(-1)). The limits of detection (0.28-3.2 µg L(-1)) were estimated at S/N ratio of 3. The validated salting out-VALLME-HPLC method was applied for the analysis of furfurals and PAT in fruit juice samples (apple, mango and grape). PMID:24468341

  9. Determination of phthalates in fruit jellies by dispersive SPE coupled with HPLC-MS.

    Science.gov (United States)

    Ma, Yuwei; Hashi, Yuki; Ji, Feng; Lin, Jin-Ming

    2010-02-01

    In this study, a simple, rapid and sensitive method for the determination of five phthalates including dimethyl phthalate, diethyl phthalate, dipropyl phthalate, benzyl butyl phthalate, and dicyclohexyl phthalate in fruit jellies by LC coupled with MS has been developed. Samples were pretreated by a dispersive SPE method, termed QuEChERS, which is an acronym for quick, easy, cheap, effective, rugged, and safe. The standard calibration curves were linear for all the analytes over the concentration range of 10-250 ng/mL, and the correlation coefficients ranged from 0.9976 to 0.9991. The LODs and LOQs were in the ranges of 0.09-3.68 ng/mL and 0.28-11.25 ng/mL, respectively. The accuracy of this method was evaluated by measuring the recovery from spiked samples. The recoveries of all five phthalates from samples spiked at three different concentrations (0.01, 0.03, and 0.05 mg/kg), were in the ranges of 83.5-103.9%, 86.7-95.8%, and 87.1-95.2%, respectively. The RSD values for the samples spiked at 0.01, 0.03, and 0.05 mg/kg ranged from 2.0-7.6%, 1.4-6.4%, and 1.2-3.8%, respectively. The method has been used for the analysis of real samples and BBP and DEP were found in real samples. PMID:19998379

  10. Enantioselective determination of acylamino acid fungicides in vegetables and fruits by chiral liquid chromatography coupled with tandem mass spectrometry.

    Science.gov (United States)

    Zhang, Hu; Wang, Xinquan; Jin, Lixia; Qian, Mingrong; Wang, Xiangyun; Xu, Hao; Qi, Peipei; Wang, Qiang; Wang, Minghua

    2012-08-01

    An efficient and sensitive enantioselective method for simultaneous determination of three acylamino acid fungicides in vegetables and fruits was presented by high-performance liquid chromatography (HPLC) coupled with tandem mass spectrometry. The three fungicides (benalaxyl, furalaxyl, and metalaxyl) residues in samples were extracted with acetonitrile containing 1% acetic acid and an aliquot was cleaned up with Si-(CH(2))(3)-NH-(CH(2))(2)-NH(2) and C(18) sorbent. Complete enantioseparation of three acylamino acid fungicides enantiomers was obtained under reversed-phase conditions on a cellulose tris (4-chloro-3-methylphenylcarbamate) column at 25°C using acetonitrile-0.1% formic acid solution (45:55, v/v) as a mobile phase. The elution orders of the eluted enantiomers were determined by a circular dichroism (CD) detector. The linearity, matrix effect, recovery, and precision were evaluated. Good linearity was obtained over the concentration range of 0.5-250 μg/L for each enantiomer in the standard solution and sample matrix calibration curves. There was no significant matrix effect for three fungicides determination based on the method. The inter-day mean recoveries, intra-day repeatability, and inter-day reproducibility varied from 81.3 to 95.7%, 2.2 to 9.4%, and 2.3 to 9.6%, respectively. The method provided high selectivity and sensitivity, and limits of quantification for enantiomers of three fungicides in vegetables and fruits were both 1 μg/kg. PMID:22753298

  11. Comprehensive analytical strategy for biomarker identification based on liquid chromatography coupled to mass spectrometry and new candidate confirmation tools.

    Science.gov (United States)

    Mohamed, Rayane; Varesio, Emmanuel; Ivosev, Gordana; Burton, Lyle; Bonner, Ron; Hopfgartner, Gérard

    2009-09-15

    A comprehensive analytical LC-MS(/MS) platform for low weight biomarkers molecule in biological fluids is described. Two complementary retention mechanisms were used in HPLC by optimizing the chromatographic conditions for a reversed-phase column and a hydrophilic interaction chromatography column. LC separation was coupled to mass spectrometry by using an electrospray ionization operating in positive polarity mode. This strategy enables us to correctly retain and separate hydrophobic as well as polar analytes. For that purpose artificial model study samples were generated with a mixture of 38 well characterized compounds likely to be present in biofluids. The set of compounds was used as a standard aqueous mixture or was spiked into urine at different concentration levels to investigate the capability of the LC-MS(/MS) platform to detect variations across biological samples. Unsupervised data analysis by principal component analysis was performed and followed by principal component variable grouping to find correlated variables. This tool allows us to distinguish three main groups whose variables belong to (a) background ions (found in all type of samples), (b) ions distinguishing urine samples from aqueous standard and blank samples, (c) ions related to the spiked compounds. Interpretation of these groups allows us to identify and eliminate isotopes, adducts, fragments, etc. and to generate a reduced list of m/z candidates. This list is then submitted to the prototype MZSearcher software tool which simultaneously searches several lists of potential metabolites extracted from metabolomics databases (e.g., KEGG, HMDB, etc) to propose biomarker candidates. Structural confirmation of these candidates was done off-line by fraction collection followed by nanoelectrospray infusion to provide high quality MS/MS data for spectral database queries. PMID:19702294

  12. Assessment of pesticide residues in some fruits using gas chromatography coupled with micro electron capture detector

    International Nuclear Information System (INIS)

    A very sensitive analytical method for the determination of 26 pesticides in some fruits based on solid phase extraction (SPE) cleanup was developed using gas chromatography (GC) coupled with micro electron capture detector (mu ECD). The identity of the pesticides was confirmed by gas chromatography mass spectroscopy (GC-MS) using selected ion monitoring (SIM) mode. Ethyl acetate was used as a solvent for the extraction of pesticide residues with assistance of sonication. For cleanup an octadecyl, C18 SPE column was used. A linear response of mu ECD was observed for all pesticides with good correlation coefficients (>0.9992). Proposed method was successfully applied for the determination of pesticide residues in the orange, apple, and grape fruits. Average recoveries achieved for all of the pesticides at fortification levels of 0.05, 1.0 and 2.0 mu g g/sup -1/ in analyzed fruits were above 90% with relative standard deviations (RSD) less than 6%. (author)

  13. HPLC: Early and Recent Perspectives.

    Science.gov (United States)

    Karger, Barry L.

    1997-01-01

    Provides a perspective on what it was like in the early days of high-performance liquid chromatography (HPLC) and several of the key developments. Focuses on the advances in HPLC generally, and more specifically for the biological sciences, that were necessary for the method to reach the preeminent stage of today. Contains 20 references. (JRH)

  14. Direct determination of chlorophenols in water samples through ultrasound-assisted hollow fiber liquid-liquid-liquid microextraction on-line coupled with high-performance liquid chromatography.

    Science.gov (United States)

    Chao, Yu-Ying; Tu, Yi-Ming; Jian, Zhi-Xuan; Wang, Hsaio-Wen; Huang, Yeou-Lih

    2013-01-01

    In this study we on-line coupled hollow fiber liquid-liquid-liquid microextraction (HF-LLLME), assisted by an ultrasonic probe, with high-performance liquid chromatography (HPLC). In this approach, the target analytes - 2-chlorophenol (2-CP), 3-chlorophenol (3-CP), 2,6-dichlorophenol (2,6-DCP), and 3,4-dichlorophenol (3,4-DCP) - were extracted into a hollow fiber (HF) supported liquid membrane (SLM) and then back-extracted into the acceptor solution in the lumen of the HF. Next, the acceptor solution was withdrawn on-line into the HPLC sample loop connected to the HF and then injected directly into the HPLC system for analysis. We found that the chlorophenols (CPs) could diffuse quickly through two sequential extraction interfaces - the donor phase - SLM and the SLM - acceptor phase - under the assistance of an ultrasonic probe. Ultrasonication provided effective mixing of the extracted boundary layers with the bulk of the sample and it increased the driving forces for mass transfer, thereby enhancing the extraction kinetics and leading to rapid enrichment of the target analytes. We studied the effects of various parameters on the extraction efficiency, viz. the nature of the SLM and acceptor phase, the compositions of the donor and acceptor phases, the fiber length, the stirring rate, the ion strength, the sample temperature, the sonication conditions, and the perfusion flow rate. This on-line extraction method exhibited linearity (r(2)≥0.998), sensitivity (limits of detection: 0.03-0.05 μg L(-1)), and precision (RSD%≤4.8), allowing the sensitive, simple, and rapid determination of CPs in aqueous solutions and water samples with a sampling time of just 2 min. PMID:23237709

  15. Speciation of four selenium compounds using high performance liquid chromatography with on-line detection by inductively coupled plasma mass spectrometry or flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Pedersen, G.A. [National Food Agency of Denmark, Institute of Food Chemistry and Nutrition, Moerkhoej Bygade 19, DK-2860 Soeborg (Denmark); Larsen, E.H. [National Food Agency of Denmark, Institute of Food Chemistry and Nutrition, Moerkhoej Bygade 19, DK-2860 Soeborg (Denmark)

    1997-07-01

    An analytical method for the speciation of selenomethionine, selenocystine, selenite and selenate by high performance liquid chromatography (HPLC) with atomic spectrometric detection is presented. An organic polymeric strong anion exchange column was used as the stationary phase in combination with an aqueous solution of 6 mmol L{sup -1} of salicylate ion at pH 8.5 as the mobile phase which allowed the isocratic separation of the four selenium analytes within 8 minutes. The separated selenium species were detected on-line by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma mass spectrometry (ICP-MS). The signal-to-noise ratio of the FAAS detector was optimized using a hydrogen-argon entrained-air flame and a slotted-tube atom trap (STAT) in the flame. The limit of detection (3 {sigma}) achieved by the HPLC-FAAS system was 1 mg L{sup -1} of selenium (100 {mu}L injections) for each of the four selenium species. More powerful selenium detection was achieved using an ELAN 5000 ICP-MS instrument. Selenium was measured at m/z = 82. The ICP-MS signal intensity was enhanced by a factor of 3-4 after addition of 3% methanol to the chromatographic mobile phase and by using an increased plasma power input of 1300 W. The limit of detection achieved under these conditions was 1 {mu}g L{sup -1} (100 {mu}L injections). The HPLC-ICP-MS system was used for selenium speciation of selenite and selenate in aqueous solutions during a BCR certification exercise and for selenium speciation in the certified reference material, BCR No. 402 White Clover. Extraction experiments revealed that the selenium species in the biological material were extractable only in the presence of water in the extraction medium. The results indicated that selenate and a compound of unknown identity U were present in the plant sample. (orig.). With 5 figs., 5 tabs.

  16. Antimicrobial activity of Marcetia DC species (Melastomataceae and analysis of its flavonoids by reverse phase-high performance liquid chromatography coupled-diode array detector

    Directory of Open Access Journals (Sweden)

    Tonny Cley Campos Leite

    2012-01-01

    Full Text Available Background: Marcetia genera currently comprises 29 species, with approximately 90% inhabiting Bahia (Brazil, and most are endemic to the highlands of the Chapada Diamantina (Bahia. Among the species, only M. taxifolia (A.St.-Hil. DC. populates Brazil (state of Roraima to Paranα and also Venezuela, Colombia, and Guyana. Objective: This work evaluated the antimicrobial activity of hexane, ethyl acetate, and methanol extracts of three species of Marcetia (Marcetia canescens Naud., M. macrophylla Wurdack, and M. taxifolia A.StHil against several microorganism. In addition, the flavonoids were analyzed in extracts by HPLC-DAD. Materials and methods: The tests were made using Gram-positive (three strains of Staphylococcus aureus and Gram-negative (two strains of Escherichia coli, a strain of Pseudomonas aeruginosa and another of Salmonella choleraesius bacteria resistant and nonresistant to antibiotics and yeasts (two strains of Candida albicans and one of C. parapsilosis by the disk diffusion method. Solid-phase extraction (SPE was performed on the above extracts to isolate flavonoids, which were subsequently analyzed by high performance liquid chromatography coupled diode array detector (HPLC-DAD. Results: Results showed that extracts inhibited the Gram-positive bacteria and yeast. The hexane extracts possessed the lowest activity, while the ethyl acetate and methanolic extracts were more active. Conclusion: Marcetia taxifolia was more effective (active against 10 microorganisms studied, and only its methanol extract inhibited Gram-negative bacteria (P. aeruginosa and S. choleraesius. SPE and HPLC-DAD analysis showed that M. canescens and M. macrophylla contain glycosylated flavonoids, while the majority of extracts from M. taxifolia were aglycone flavonoids.

  17. Determination of eight artificial sweeteners and common Stevia rebaudiana glycosides in non-alcoholic and alcoholic beverages by reversed-phase liquid chromatography coupled with tandem mass spectrometry

    OpenAIRE

    Kubica, Paweł; Namieśnik, Jacek; Wasik, Andrzej

    2014-01-01

    The method for the determination of acesulfame-K, saccharine, cyclamate, aspartame, sucralose, alitame, neohesperidin dihydrochalcone, neotame and five common steviol glycosides (rebaudioside A, rebaudioside C, steviol, steviolbioside and stevioside) in soft and alcoholic beverages was developed using high-performance liquid chromatography and tandem mass spectrometry with electrospray ionisation (HPLC-ESI-MS/MS). To the best of our knowledge, this is the first work that presents an HPLC-ESI-...

  18. HPLC Neurotransmitter Analysis.

    Science.gov (United States)

    Holm, Thomas Hellesøe; Isaksen, Toke Jost; Lykke-Hartmann, Karin

    2016-01-01

    High performance liquid chromatography (HPLC) is a powerful tool to measure neurotransmitter levels in specific tissue samples and dialysates from patients and animals. In this chapter, we list the current protocols used to measure neurotransmitters in the form of biogenic amines from murine brain samples. PMID:26695044

  19. Systematic evaluation of matrix effects in hydrophilic interaction chromatography versus reversed phase liquid chromatography coupled to mass spectrometry.

    Science.gov (United States)

    Periat, Aurélie; Kohler, Isabelle; Thomas, Aurélien; Nicoli, Raul; Boccard, Julien; Veuthey, Jean-Luc; Schappler, Julie; Guillarme, Davy

    2016-03-25

    Reversed phase liquid chromatography (RPLC) coupled to mass spectrometry (MS) is the gold standard technique in bioanalysis. However, hydrophilic interaction chromatography (HILIC) could represent a viable alternative to RPLC for the analysis of polar and/or ionizable compounds, as it often provides higher MS sensitivity and alternative selectivity. Nevertheless, this technique can be also prone to matrix effects (ME). ME are one of the major issues in quantitative LC-MS bioanalysis. To ensure acceptable method performance (i.e., trueness and precision), a careful evaluation and minimization of ME is required. In the present study, the incidence of ME in HILIC-MS/MS and RPLC-MS/MS was compared for plasma and urine samples using two representative sets of 38 pharmaceutical compounds and 40 doping agents, respectively. The optimal generic chromatographic conditions in terms of selectivity with respect to interfering compounds were established in both chromatographic modes by testing three different stationary phases in each mode with different mobile phase pH. A second step involved the assessment of ME in RPLC and HILIC under the best generic conditions, using the post-extraction addition method. Biological samples were prepared using two different sample pre-treatments, i.e., a non-selective sample clean-up procedure (protein precipitation and simple dilution for plasma and urine samples, respectively) and a selective sample preparation, i.e., solid phase extraction for both matrices. The non-selective pretreatments led to significantly less ME in RPLC vs. HILIC conditions regardless of the matrix. On the contrary, HILIC appeared as a valuable alternative to RPLC for plasma and urine samples treated by a selective sample preparation. Indeed, in the case of selective sample preparation, the compounds influenced by ME were different in HILIC and RPLC, and lower and similar ME occurrence was generally observed in RPLC vs. HILIC for urine and plasma samples

  20. Cell-based bioreporter assay coupled to HPLC micro-fractionation in the evaluation of antimicrobial properties of the basidiomycete fungus Pycnoporus cinnabarinus.

    Science.gov (United States)

    Järvinen, Päivi; Nybond, Susanna; Marcourt, Laurence; Ferreira Queiroz, Emerson; Wolfender, Jean-Luc; Mettälä, Aila; Karp, Matti; Vuorela, Heikki; Vuorela, Pia; Hatakka, Annele; Tammela, Päivi

    2016-06-01

    Context Identification of bioactive components from complex natural product extracts can be a tedious process that aggravates the use of natural products in drug discovery campaigns. Objective This study presents a new approach for screening antimicrobial potential of natural product extracts by employing a bioreporter assay amenable to HPLC-based activity profiling. Materials and methods A library of 116 crude extracts was prepared from fungal culture filtrates by liquid-liquid extraction with ethyl acetate, lyophilised, and screened against Escherichia coli using TLC bioautography. Active extracts were studied further with a broth microdilution assay, which was, however, too insensitive for identifying the active microfractions after HPLC separation. Therefore, an assay based on bioluminescent E. coli K-12 (pTetLux1) strain was coupled with HPLC micro-fractionation. Results Preliminary screening yielded six fungal extracts with potential antimicrobial activity. A crude extract from a culture filtrate of the wood-rotting fungus, Pycnoporus cinnabarinus (Jacq.) P. Karst. (Polyporaceae), was selected for evaluating the functionality of the bioreporter assay in HPLC-based activity profiling. In the bioreporter assay, the IC50 value for the crude extract was 0.10 mg/mL. By integrating the bioreporter assay with HPLC micro-fractionation, the antimicrobial activity was linked to LC-UV peak of a compound in the chromatogram of the extract. This compound was isolated and identified as a fungal pigment phlebiarubrone. Discussion and conclusion HPLC-based activity profiling using the bioreporter-based approach is a valuable tool for identifying antimicrobial compound(s) from complex crude extracts, and offers improved sensitivity and speed compared with traditional antimicrobial assays, such as the turbidimetric measurement. PMID:26808592

  1. Quality control and identification of steroid saponins in crude extracts from Dioscorea zingiberensis C. H. Wright by fingerprint with HPLC-ELSD and HPLC-ESI-Quadrupole/Time-of-fight tandem mass spectrometry

    OpenAIRE

    Zhang, Xinxin; Liang, Jinru; Liu, Jianli; Zhao, Ye; Gao, Juan; Sun, Wenji; Ito, Yoichiro

    2013-01-01

    In this study, a fingerprint of steroid saponins, the major bioactive constituents in the crude extracts from Dioscorea zingiberensis C. H. Wright (DZW), has been established for the first time by high-performance liquid chromatography coupled with evaporative light scattering detector (HPLC-ELSD) and the simultaneous characterization of the steroid saponins by high-performance liquid chromatography coupled with electrospray ionization-mass spectrometry and quadrupole tandem...

  2. Qualitative and Quantitative Analysis of Lignan Constituents in Caulis Trachelospermi by HPLC-QTOF-MS and HPLC-UV

    OpenAIRE

    Xiao-Ting Liu; Xu-Guang Wang; Rui Xu; Fan-Hua Meng; Neng-Jiang Yu; Yi-Min Zhao

    2015-01-01

    A high-performance liquid chromatography coupled with quadrupole tandem time-of-flight mass (HPLC-QTOF-MS) and ultraviolet spectrometry (HPLC-UV) was established for simultaneous qualitative and quantitative analysis of the major chemical constituents in Caulis Trachelospermi, respectively. The analysis was performed on an Agilent Zorbax Eclipse Plus C18 column (4.6 mm × 150 mm, 5 μm) using a binary gradient system of water and methanol, with ultraviolet absorption at 230 nm. Based on high-re...

  3. Rapid analysis of components in Rhizoma Anemarrhenae by HPLC-DAD-MS and HPLC-DAD-TOFMS

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    A global quality control method based on high performance liquid chromatography(HPLC)coupled with diode array detection(DAD),single quadrupole mass spectrometry(MS)and time-of-flight mass spectrometry(TOFMS)was developed for simultaneous determination of seven major components(mangiferin,neomangiferin,timosaponin E1,timosaponin E,timosaponin BⅡ,timosaponin BⅢ,and timosaponin AⅢ)and identification of most components in extracts of Rhizoma Anemarrhenae(RA).HPLC analysis was performed on an Agilent SB-C18 colu...

  4. Immobilized Metal Affinity Chromatography Coupled to Multiple Reaction Monitoring Enables Reproducible Quantification of Phospho-signaling.

    Science.gov (United States)

    Kennedy, Jacob J; Yan, Ping; Zhao, Lei; Ivey, Richard G; Voytovich, Uliana J; Moore, Heather D; Lin, Chenwei; Pogosova-Agadjanyan, Era L; Stirewalt, Derek L; Reding, Kerryn W; Whiteaker, Jeffrey R; Paulovich, Amanda G

    2016-02-01

    A major goal in cell signaling research is the quantification of phosphorylation pharmacodynamics following perturbations. Traditional methods of studying cellular phospho-signaling measure one analyte at a time with poor standardization, rendering them inadequate for interrogating network biology and contributing to the irreproducibility of preclinical research. In this study, we test the feasibility of circumventing these issues by coupling immobilized metal affinity chromatography (IMAC)-based enrichment of phosphopeptides with targeted, multiple reaction monitoring (MRM) mass spectrometry to achieve precise, specific, standardized, multiplex quantification of phospho-signaling responses. A multiplex immobilized metal affinity chromatography- multiple reaction monitoring assay targeting phospho-analytes responsive to DNA damage was configured, analytically characterized, and deployed to generate phospho-pharmacodynamic curves from primary and immortalized human cells experiencing genotoxic stress. The multiplexed assays demonstrated linear ranges of ≥3 orders of magnitude, median lower limit of quantification of 0.64 fmol on column, median intra-assay variability of 9.3%, median inter-assay variability of 12.7%, and median total CV of 16.0%. The multiplex immobilized metal affinity chromatography- multiple reaction monitoring assay enabled robust quantification of 107 DNA damage-responsive phosphosites from human cells following DNA damage. The assays have been made publicly available as a resource to the community. The approach is generally applicable, enabling wide interrogation of signaling networks. PMID:26621847

  5. Thin layer chromatography coupled to paper spray ionization mass spectrometry for cocaine and its adulterants analysis.

    Science.gov (United States)

    De Carvalho, Thays C; Tosato, Flavia; Souza, Lindamara M; Santos, Heloa; Merlo, Bianca B; Ortiz, Rafael S; Rodrigues, Rayza R T; Filgueiras, Paulo R; França, Hildegardo S; Augusti, Rodinei; Romão, Wanderson; Vaz, Boniek G

    2016-05-01

    Thin layer chromatography (TLC) is a simple and inexpensive type of chromatography that is extensively used in forensic laboratories for drugs of abuse analysis. In this work, TLC is optimized to analyze cocaine and its adulterants (caffeine, benzocaine, lidocaine and phenacetin) in which the sensitivity (visual determination of LOD from 0.5 to 14mgmL(-1)) and the selectivity (from the study of three different eluents: CHCl3:CH3OH:HCOOHglacial (75:20:5v%), (C2H5)2O:CHCl3 (50:50v%) and CH3OH:NH4OH (100:1.5v%)) were evaluated. Aiming to improve these figures of merit, the TLC spots were identified and quantified (linearity with R(2)>0.98) by the paper spray ionization mass spectrometry (PS-MS), reaching now lower LOD values (>1.0μgmL(-1)). The method developed in this work open up perspective of enhancing the reliability of traditional and routine TLC analysis employed in the criminal expertise units. Higher sensitivity, selectivity and rapidity can be provided in forensic reports, besides the possibility of quantitative analysis. Due to the great simplicity, the PS(+)-MS technique can also be coupled directly to other separation techniques such as the paper chromatography and can still be used in analyses of LSD blotter, documents and synthetic drugs. PMID:26970868

  6. Speciation of arsenic in water, sediment, and plants of the Moira watershed, Canada, using HPLC coupled to high resolution ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Zheng, Jian; Hintelmann, Holger; Dimock, Brian; Dzurko, Mark Stephen [Department of Chemistry, Trent University, 1600 West Bank Drive, K9J 7B8, Peterborough, Ontario (Canada)

    2003-09-01

    High-performance liquid chromatography (HPLC) coupled with high-resolution sector field ICP-MS was applied to the speciation of arsenic in environmental samples collected from the Moira watershed, Ontario, Canada. Arsenic contamination in Moira River and Moira Lake from historic gold mine operations is of increasing environmental concern to the local community. In this study, the current arsenic contamination status in water, sediment, and plants was investigated. Elevated levels of arsenic in the surface water of up to 75 ng mL{sup -1} in Moira River and 50 ng mL{sup -1} in Moira Lake were detected, 98% of which was present as arsenate. High concentrations of arsenic (>300 ng mL{sup -1}), mainly present as arsenite, were detected in sediment porewaters. A sediment profile of As from the West basin of Moira Lake showed lower As concentrations compared with data from the 1990s. An optimized extraction procedure using a phosphoric acid-ascorbic acid mixture demonstrated that an unknown ''As-complex'' which may consist of As, sulfide and organic matter is potentially responsible for the release of arsenite from the sediment to the overlying water column. Arsenic concentrations in plant samples ranged from 2.6 to 117 mg kg{sup -1}, dry weight. Accumulation of arsenic was observed in submerged plants collected from Moira River and Moira Lake. Only a small part of the arsenic (6.3-16.1%) in the plants was extractable with methanol-water (9:1), and most of this arsenic (70-93%) was inorganic arsenic. A variety of organic arsenic compounds, including simple methylated compounds (methylarsonic acid and dimethylarsinic acid), trimethylarsine oxide, and tetramethylarsonium cation were detected at trace levels. No arsenobetaine and arsenocholine was found in any plant sample. An unknown compound, most probably an arsenosugar was detected in the two submerged plants, coontail (Ceratophyllum demersum) and long-stemmed waterwort (Elatine triandra). These

  7. Indirect hydrogen analysis by gas chromatography coupled to mass spectrometry (GC-MS).

    Science.gov (United States)

    Varlet, V; Smith, F; Augsburger, M

    2013-08-01

    Gas chromatography (GC) is an analytical tool very useful to investigate the composition of gaseous mixtures. The different gases are separated by specific columns but, if hydrogen (H2 ) is present in the sample, its detection can be performed by a thermal conductivity detector or a helium ionization detector. Indeed, coupled to GC, no other detector can perform this detection except the expensive atomic emission detector. Based on the detection and analysis of H2 isotopes by low-pressure chemical ionization mass spectrometry (MS), a new method for H2 detection by GC coupled to MS with an electron ionization ion source and a quadrupole analyser is presented. The presence of H2 in a gaseous mixture could easily be put in evidence by the monitoring of the molecular ion of the protonated carrier gas. PMID:23893637

  8. Novel applications of high performance ion chromatography - inductively coupled plasma mass spectrometry (HPIC-ICP-MS)

    International Nuclear Information System (INIS)

    This work demonstrates the development of highly sensitive and selective analytical methods, which make use of the hyphenation of high performance ion chromatography (HPIC) to inductively coupled plasma sector field mass spectrometry (ICP-SFMS). On-line coupling a chromatographic separation method with an elemental detection method provides two advantages: (1) The components of a possibly interfering matrix can be separated allowing accurate and precise ultra trace analysis of the element of interest and (2) elemental species of an element can be separated and quantified. In this work, matrix separation methods for interference free determination of 232Th, 234U, 235U and 238U in geological matrices were developed and employed. Furthermore HPIC-ICP-SFMS was applied for ultra trace analysis of Pd in environmental and geological matrices. The usefulness of HPIC-ICP-SFMS for speciation studies was demonstrated by investigating the interaction of an anti-cancer drug (cisplatin) with guanosine monophosphates. (author)

  9. HPLC-Orbitrap analysis for identification of organic molecules in complex material

    OpenAIRE

    Gautier, Thomas; Schmitz-Afonso, Isabelle; Carrasco, Nathalie; Touboul, D.; Szopa, Cyril; Buch, Arnaud; Pernot, Pascal

    2015-01-01

    International audience We performed High Performance Liquid Chromatography (HPLC) coupled to Orbitrap High Resolution Mass Spectrometry (OHR MS) analysis of Titan’s tholins. This analysis allowed us to determine the exact composition and structure of some of the major components of tholins.

  10. HPLC-Profiles of Tocopherols, Sugars, and Organic Acids in Three Medicinal Plants Consumed as Infusions

    OpenAIRE

    Custódio Lobo Roriz; Lillian Barros; Ana Maria Carvalho; Ferreira, Isabel C. F. R.

    2014-01-01

    Pterospartum tridentatum (L.) Willk., Gomphrena globosa L. and Cymbopogon citratus (DC) Stapf. are medicinal plants that require a more detailed chemical characterization, given the importance of their consumption as infusions. Therefore, the individual profiles in tocopherols, free sugars and organic acids were obtained by high performance liquid chromatography (HPLC) coupled to different detectors (fluorescence, refraction index and photodiode array, respectively). C. citratus revealed th...

  11. Using HPLC-Mass Spectrometry to Teach Proteomics Concepts with Problem-Based Techniques

    Science.gov (United States)

    Short, Michael; Short, Anne; Vankempen, Rachel; Seymour, Michael; Burnatowska-Hledin, Maria

    2010-01-01

    Practical instruction of proteomics concepts was provided using high-performance liquid chromatography coupled with a mass selective detection system (HPLC-MS) for the analysis of simulated protein digests. The samples were prepared from selected dipeptides in order to facilitate the mass spectral identification. As part of the prelaboratory…

  12. Speciation of arsenic of liquid and gaseous emissions from soil in a microcosmos experiment by liquid and gas chromatography with inductively coupled plasma mass spectrometer (ICP-MS) detection

    Energy Technology Data Exchange (ETDEWEB)

    Prohaska, T.; Stingeder, G. [University of Agricultural Sciences - BOKU Wien (Austria). Inst. of Chemistry; Pfeffer, M.; Tulipan, M.; Mentler, A.; Wenzel, W.W. [Vienna University of Agricultural Sciences - BOKU Wien (Austria). Inst. of Soil Science

    1999-07-01

    Gas chromatography and high-performance liquid chromatography coupled to a double focusing sectorfield ICP-MS as sensitive element specific detector are used for the speciation of arsenic of liquid and gaseous emissions from soil samples, which were equilibrated in a microcosmos experiment. Speciation of liquid samples was performed by HPLC and hydride generation was used as introduction system to ICP-MS. An online prereduction step was introduced to enhance the sensitivity for As(V). A home-built and laboratory-ready transfer line from GC to ICP-MS is presented and quantification of As in gaseous emissions was performed by external calibration via hydride generation. The microcosmos experiment revealed only low production rates of organoarsenic compounds and reflected a limited capability of the biovolatilization experiment for the simulation of natural systems. (orig.) With 5 figs., 5 tabs., 29 refs.

  13. Serum/plasma methylmercury determination by isotope dilution gas chromatography-inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Highlights: · We determine methylmercury in serum and plasma using isotope dilution calibration. · Separation by gas chromatography and detection by inductively coupled plasma mass spectrometry. · Data for 50 specimens provides first reference range for methylmercury in serum. · Serum samples shown to be stable for 11 months in refrigerator. - Abstract: A method for the determination of methylmercury in plasma and serum samples was developed. The method uses isotope dilution with 198Hg-labeled methylmercury, extraction into dichloromethane, back-extraction into water, aqueous-phase ethylation, purge and trap collection, thermal desorption, separation by gas chromatography, and mercury isotope specific detection by inductively coupled plasma mass spectrometry. By spiking 2 mL sample with 1.2 ng tracer, measurements in a concentration interval of (0.007-2.9) μg L-1 could be performed with uncertainty amplification factors -1 was estimated at 10 times the standard deviation of concentrations measured in preparation blanks. Within- and between-run relative standard deviations were -1, 0.35 μg L-1 and 2.8 μg L-1, with recoveries in the range 82-110%. Application of the method to 50 plasma/serum samples yielded a median (mean; range) concentration of methylmercury of 0.081 (0.091; -1. This is the first time methylmercury has been directly measured in this kind of specimen, and is therefore the first estimate of a reference range.

  14. Development and application of liquid chromatography coupled to isotope ratio mass spectrometry

    International Nuclear Information System (INIS)

    Stable isotope analysis has found widespread applications in various disciplines such as archaeology, geochemistry, biology, food authenticity, and forensic science. Coupling chromatography to isotope ratio mass spectrometry for compound-specific isotope analysis (CSIA) is a trend, as it provides several advantages over bulk isotope analysis, e.g., relatively simple sample preparation, the ability to measure individual compounds in a complex mixture in one run, and the reduced sample size required for precise isotope analysis. Gas chromatography coupled to isotope ratio mass spectrometry (GC/IRMS) has been well-established for compound-specific isotope analysis of volatile organic compounds within the last two decades. However, an interface combining liquid chromatography with isotope ratio mass spectrometry (LC/IRMS) was not commercially available until 2004. The current design of the interface requires using a carbon-free eluent in chromatographic separation. This requirement limits the application of the most frequently used reversed-phase liquid chromatography in CSIA, because the elution strength of water at room temperature is too low to serve as mobile phase in reversed-phase separations. In order to increase the elution strength of water, we propose using high temperature water for chromatographic elution. The polarity of water decreases with an increase of temperature, yielding increased elution strength in reversed-phase columns. Therefore, high temperature water can be used as eluent instead of organic solvent for combining reversed-phase liquid chromatography with isotope ratio mass spectrometry (RPLC/IRMS). Additionally, temperature gradients can replace organic solvent gradients to increase chromatographic resolution. This is very important for LC/IRMS analysis, as precise isotope analysis requires baseline separation of analytes. In this thesis, high-temperature reversed-phase liquid chromatography was coupled to, and for the first time carefully

  15. Development and application of liquid chromatography coupled to isotope ratio mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Lijun

    2014-02-19

    Stable isotope analysis has found widespread applications in various disciplines such as archaeology, geochemistry, biology, food authenticity, and forensic science. Coupling chromatography to isotope ratio mass spectrometry for compound-specific isotope analysis (CSIA) is a trend, as it provides several advantages over bulk isotope analysis, e.g., relatively simple sample preparation, the ability to measure individual compounds in a complex mixture in one run, and the reduced sample size required for precise isotope analysis. Gas chromatography coupled to isotope ratio mass spectrometry (GC/IRMS) has been well-established for compound-specific isotope analysis of volatile organic compounds within the last two decades. However, an interface combining liquid chromatography with isotope ratio mass spectrometry (LC/IRMS) was not commercially available until 2004. The current design of the interface requires using a carbon-free eluent in chromatographic separation. This requirement limits the application of the most frequently used reversed-phase liquid chromatography in CSIA, because the elution strength of water at room temperature is too low to serve as mobile phase in reversed-phase separations. In order to increase the elution strength of water, we propose using high temperature water for chromatographic elution. The polarity of water decreases with an increase of temperature, yielding increased elution strength in reversed-phase columns. Therefore, high temperature water can be used as eluent instead of organic solvent for combining reversed-phase liquid chromatography with isotope ratio mass spectrometry (RPLC/IRMS). Additionally, temperature gradients can replace organic solvent gradients to increase chromatographic resolution. This is very important for LC/IRMS analysis, as precise isotope analysis requires baseline separation of analytes. In this thesis, high-temperature reversed-phase liquid chromatography was coupled to, and for the first time carefully

  16. Direct Determination of Total Arsenic and Arsenic Species by Ion Chromatography Coupled with Inductively Coupled Plasma Mass Spectrometry

    International Nuclear Information System (INIS)

    The simultaneous determination of As(III), As(V), and DMA has been performed by ion chromatography (IC) coupled with inductively coupled plasma-mass spectrometry (ICP-MS). The separation of the three arsenic species was achieved by an anionic separator column (AS 7) with an isocratic elution system. The separated species were directly detected by ICP-MS as an element-selective detection method. The IC-ICP-MS technique was applied for the determination of arsenic species in a NIST SRM 1643d water sample. An As(III) only was detected in the sample. The detection limits of As(III), As(V) and DMA were 0.31, 0.45, and 2.09 ng/mL, respectively. It was also applied for the determination of arsenic species in a human urine obtained by a volunteer, and three arsenic species were identified. The determination of total As in human urines that were obtained from 25 volunteers at the different age was also carried out by ICP-MS

  17. Coupling Charge Reduction Mass Spectrometry to Liquid Chromatography for Complex Mixture Analysis.

    Science.gov (United States)

    Stutzman, John R; Crowe, Matthew C; Alexander, James N; Bell, Bruce M; Dunkle, Melissa N

    2016-04-01

    Electrospray ionization (ESI) of solution mixtures often generates complex mass spectra, even following liquid chromatography (LC), due to analyte multiple charging. Multiple charge state distributions can lead to isobaric interferences, mass spectral congestion, and ambiguous ion identification. As a consequence, data interpretation increases in complexity. Several charge reduction mass spectrometry (MS) approaches have been previously developed to reduce the average charge state of gaseous ions; however, all of these techniques have been restricted to direct infusion MS. In this study, synthetic polyols and surfactants separated by liquid chromatography and ionized by positive mode ESI have been subjected to polonium-210 α-particle radiation to reduce the average charge state to singly charged cations prior to mass analysis. LC/MS analysis of 5000 molecular weight poly(ethylene glycol) (PEG5000) generated an average charge state of 5.88+; whereupon, liquid chromatography/electrospray ionization/charge reduction/mass spectrometry (LC/CR/MS) analysis of PEG 5000 generated an average charge state of 1.00+. The PEG5000 results demonstrated a decrease in spectral complexity and enabled facile interpretation. Other complex solution mixtures representing specific MS challenges (i.e., competitive ionization and isobaric ion overlap) were explored and analyzed with LC/CR/MS to demonstrate the benefits of coupling LC to CR/MS. For example, polyol information related to initiator, identity/relative amount of monomer, and estimated molecular weight was characterized in random and triblock ethylene oxide/propylene oxide polyols using LC/CR/MS. LC/CR/MS is a new analytical technique for the analysis of complex mixtures. PMID:26971559

  18. Assessment of Pesticide Residues in Some Fruits Using Gas Chromatography Coupled with Micro Electron Capture Detector

    Directory of Open Access Journals (Sweden)

    M. I. Bhanger

    2011-12-01

    Full Text Available A very sensitive analytical method for the determination of 26 pesticides in some fruits based on solid phase extraction (SPE cleanup was developed using gas chromatography (GC coupled with micro electron capture detector (μECD. The identity of the pesticides was confirmed by gas chromatography mass spectroscopy (GC-MS using selected ion monitoring (SIM mode. Ethyl acetate was used as a solvent for the extraction of pesticide residues with assistance of sonication. For cleanup an octadecyl, C18 SPE column was used. A linear response of μECD was observed for all pesticides with good correlation coefficients (>0.9992. Proposed method was successfully applied for the determination of pesticide residues in the orange, apple, and grape fruits. Average recoveries achieved for all of the pesticides at fortification levels of 0.05, 1.0 and 2.0 μg g-1 in analyzed fruits were above 90% with relative standard deviations (RSD less than 6

  19. Fast separation of triterpenoid saponins using supercritical fluid chromatography coupled with single quadrupole mass spectrometry.

    Science.gov (United States)

    Huang, Yang; Zhang, Tingting; Zhou, Haibo; Feng, Ying; Fan, Chunlin; Chen, Weijia; Crommen, Jacques; Jiang, Zhengjin

    2016-03-20

    Triterpenoid saponins (TSs) are the most important components of some traditional Chinese medicines (TCMs) and have exhibited valuable pharmacological properties. In this study, a rapid and efficient method was developed for the separation of kudinosides, stauntosides and ginsenosides using supercritical fluid chromatography coupled with single quadrupole mass spectrometry (SFC-MS). The separation conditions for the selected TSs were carefully optimized after the initial screening of eight stationary phases. The best compromise for all compounds in terms of chromatographic performance and MS sensitivity was obtained when water (5-10%) and formic acid (0.05%) were added to the supercritical carbon dioxide/MeOH mobile phase. Beside the composition of the mobile phase, the nature of the make-up solvent for interfacing SFC with MS was also evaluated. Compared to reversed phase liquid chromatography, the SFC approach showed higher resolution and shorter running time. The developed SFC-MS methods were successfully applied to the separation and identification of TSs present in Ilex latifolia Thunb., Panax quinquefolius L. and Panax ginseng C.A. Meyer. These results suggest that this SFC-MS approach could be employed as a useful tool for the quality assessment of natural products containing TSs as active components. PMID:26773536

  20. Speciation of metals in soil extracts by size exclusion chromatography/inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Metal ion speciation influences the mobility of metals in the environment and their bioavailability. Dissolved humic substances (HS) and low molecular weight organic acids greatly influence the speciation of metals in soil and other natural environment. This study was conducted to identify HS bound metal in citric acid extracts from soil by size exclusion chromatography/inductively coupled plasma mass spectrometry (SEC/ICP-MS). The size exclusion column, which has optimal separation range from 3000-7000, was used. Absorption was monitored at 280 nm using an UV/VIS absorption detector. The eluate from the detector was directly introduced to the ICP-MS through a nebulizer. The size exclusion chromatography could separate HS and citric acid used for extraction. This was confirmed by the results obtained using a multi-channel diode array detector. HS was evidenced by broad absorption from UV to VIS range while organic acid was by narrow UV absorption. Analysis showed that most of iron was bound to HS, while part of aluminium was bound HS. Other metals were not bound to HS and some transitional metals except manganese made complex with citric acid. Most of silicon was not bound to HS and probably existed in the form of silicic acid. (author)

  1. ANALYSIS OF PENTACHLOROPHENOL IN WATER BY PURGE AND TRAP CONCENTRATOR COUPLED TO GAS CHROMATOGRAPHY

    Institute of Scientific and Technical Information of China (English)

    HuixiaLan; YuancaiChen; ZhonghaoChen

    2004-01-01

    It is convenient and time saving to analyze pentachlorophenol (PCP) in water by purge and trap concentrator coupled to gas chromatography that avoids employing a great deal of organic solvent. In this paper, the appropriate purge and trap conditions of PCP are determined: the trapped sorbent is TenaxGC; the purge gas is pure nitrogen and purge flow is 40ml/min; the purge time is 30min. A series of standard PCP water samples 5, 10, 50, 100, 200, 400, 800, 1000ppb are analyzed in order to obtain standard curve, and the linear regressive equation obtained is Y=109.65X-687.72, which correlation coefficient r is 0.9949. The precision of the method is determined with 0.5ppb PCP water sample, and the standard deviation measured is 3%. The detection limit for PCP is 0.2ppb.

  2. ANALYSIS OF PENTACHLOROPHENOL IN WATER BY PURGE AND TRAP CONCENTRATOR COUPLED TOGAS CHROMATOGRAPHY

    Institute of Scientific and Technical Information of China (English)

    Huixia Lan; Yuancai Chen; Zhonghao Chen

    2004-01-01

    It is convenient and time saving to analyze pentachlorophenol (PCP) in water by purge and trap concentrator coupled to gas chromatography that avoids employing a great deal of organic solvent: In this paper, the appropriate purge and trap conditions of PCP are determined: the trapped sorbent is TenaxGC; the purge gas is pure nitrogen and purge flow is 40ml/min; the purge time is 30min. A series of standard PCP water samples 5, 10, 50, 100, 200,400, 800, 1000ppb are analyzed in order to obtain standard curve, and the linear regressive equation obtained is Y=109.65X-687.72, which correlation coefficient r is 0.9949. The precision of the method is determined with 0.5ppb PCP water sample, and the standard deviation measured is 3%. The detection limit for PCP is 0.2ppb.

  3. Determination of long-chain fatty acids in serum by gas chromatography coupled to mass spectrometry

    International Nuclear Information System (INIS)

    The quantification of long-chain fatty acids is fundamental for the diagnosis of several peroxisome disorders, particularly those in which the β-oxidation peroxisome of fatty acids is affected. In this work the implementation of an analytical method for the determination of these markers in serum by gas chromatography coupled to mass spectrometry is described. Besides, samples from patients with a diagnostic impression of adrenoleukodystrophy linked to the X chromosome were analyzed. The necessary experimental conditions were achieved for the separation and quantification of C22:0, C24:0 and C26:0 fatty acids in serum, which are biochemical markers of various peroxisome diseases. The application of this method allowed confirming the diagnosis of three patients with a diagnostic impression of adrenoleukodystrophy linked to the X chromosome. The application of the method in daily practice will allow the Cuban medical system to count on a new laboratory parameter for the diagnosis of peroxisome disorders

  4. Diagnosis of propionic acidemia by gas chromatography coupled to mass spectrometry in a case analysis

    International Nuclear Information System (INIS)

    Propionic acidemia is an inherited metabolic disease caused by a deficiency in the propionyl-CoA carboxilase, a biotin-dependent mitochondrial enzyme. The disorder is a clinically heterogeneous disease and one of the most frequently occurring organic acidurias. We report the first Cuban case with a severe form of propionic acidemia followed by acidosis and death. The diagnosis was carried out by gas chromatography coupled to mass spectrometry. Our aim is to highlight the importance of organic acids urine analysis as part of the first laboratory tests in undiagnosed seriously ill children. The definitive diagnosis is important as it serves as a clear guideline to establish a suitable treatment and allows geneticists to provide patients with a proper genetic counseling

  5. Preparation of inulin-type fructooligosaccharides using fast protein liquid chromatography coupled with refractive index detection.

    Science.gov (United States)

    Li, J; Cheong, K L; Zhao, J; Hu, D J; Chen, X Q; Qiao, C F; Zhang, Q W; Chen, Y W; Li, S P

    2013-09-20

    A fast protein liquid chromatography coupled with refractive index detection (FPLC-RID) method was firstly developed for preparation and purification of fructooligosaccharides with different degree of polymerization from burdock, Arctium lappa. After extraction with 60% ethanol and decolorization with MCI gel CHP20P, total fructooligosaccharides were purified on Bio-Gel P-2 column eluted with water at the flow rate of 0.3 ml/min, which was the optimized conditions. The obtained fructooligosaccharides with degree of polymerization of 3-9 were identified based on their methylation analysis, MS and NMR data. This method has the advantages of high automation, good recovery and easy performance, which could be used for preparation of FOS from other sources, as well as other targeted compounds without UV absorbance. PMID:23962565

  6. Determinação de alfa-Tocoferol em alho irradiado utilizando cromatografia líquida de alta eficiência (CLAE Determination of alpha-Tocopherol (vitamin E in irradiated garlic by high performance liquid chromatography (HPLC

    Directory of Open Access Journals (Sweden)

    Magda Dias Gonçalves Rios

    2003-01-01

    Full Text Available The effects of 60Co ionizing radiations in doses of 0, 75, 100, 150, 200 and 250Gy on garlic, upon the alpha-tocopherol concentration were studied. The alpha-tocopherol contents were established by high performance liquid chromatography (HPLC, after direct hexane extraction from the garlic samples. The alpha-tocopherol was determined through normal-phase column, and mobile phase was composed by hexane: iso-propyl alcohol (99:01 v/v, with 2mL/min flow rate and fluorescence detector. It is statistically shown that an irradiation dose of up to 150 Gy does not affect the garlic alpha-tocopherol content.

  7. Determination of alpha-Tocopherol (vitamin E) in irradiated garlic by high performance liquid chromatography (HPLC); Determinacao de alpha-tocoferol em alho irradiado utilizando cromatografia liquida de alta frequencia (CLAE)

    Energy Technology Data Exchange (ETDEWEB)

    Rios, Magda Dias Goncalves; Penteado, Marilene de Vuono Camargo [Sao Paulo Univ., SP (Brazil). Faculdade de Ciencias Farmaceuticas. Dept. de Alimentos e Nutricao Experimental]. E-mail: riosmagda@hotmail.com

    2003-02-01

    The effects of {sup 60}Co ionizing radiations in doses of 0, 75, 100, 150, 200 and 250Gy on garlic, upon the {alpha}-tocopherol concentration were studied. The {alpha}-tocopherol contents were established by high performance liquid chromatography (HPLC), after direct hexane extraction from the garlic samples. The {alpha}-tocopherol was determined through normal phase column, and mobile phase was composed by hexane: iso-propyl alcohol (99:01 v/v), with 2mL/min flow rate and fluorescence detector. It is statistically shown that an irradiation dose of up to 150 Gy does not affect the garlic {alpha}-tocopherol content. (author)

  8. Cuantificación de Sapogeninas del Jugo Fresco y Fermentado de Fique (Furcraea gigantea mediante Cromatografía Liquida de Alta Resolución (HPLC-PDA Sapogenins Quantification of Fresh and Fermented Juice of Fique (Furcraea gigantean by High-Performance Liquid Chromatography (HPLC-PDA

    Directory of Open Access Journals (Sweden)

    Olga L Benavides

    2012-01-01

    Full Text Available Se presenta un estudio sobre la cuantificación de sapogeninas del jugo fresco y fermentado de fique (Furcraea gigantea mediante cromatografía liquida de alta resolución con detector de fotodiodo (HPLC-PDA. El jugo de fique, una planta cultivada ampliamente en Colombia, se fermentó durante 2, 4 y 6 días a 33°C. Mediante hidrólisis ácida se obtovo el extracto de sapogeninas, cuyos componentes identificados por cromatografía gaseosa y espectroscopia másica (GC-MS fueron hecogenina y tigogenina. Usando el método HPLC-PDA se cuantificó la hecogenina y tigogenina presentes. El jugo de fique con cuatro días de fermentación presentó el mayor contenido de sapogeninas. Por lo tanto, se recomienda este proceso para fines de extracción de estos compuestos.A stody on the quantification of sapogenins in fresh and fermented juice of fique (Forcraea gigantean by high-performance liquid chromatography with photodiode array detector (HPLC-PDA. The juice of the fique, a plant that is widely grown in Colombia, was fermented for 2, 4 and 6 days at 33 °C. Using acid hydrolysis, sapogenin extracts were obtained. The sobstances in the extracts, identified by gas chromatography-mass spectrometry (GC-MS were hecogenin and tigogenin. Hecogenin and tigogenin in the juice were determined osing HPLC-PDA. Fique juice with fuor days of fermentation showed the highest content of sapogenins. Therefore, this is the recommend process for the extraction of these compuonds.

  9. Characterisation of Phenolic Compounds in South African Plum Fruits (Prunus salicina Lindl. using HPLC Coupled with Diode-Array, Fluorescence, Mass Spectrometry and On-Line Antioxidant Detection

    Directory of Open Access Journals (Sweden)

    Dalene de Beer

    2013-05-01

    Full Text Available Phenolic compounds are abundant secondary metabolites in plums, with potential health benefits believed to be due to their antioxidant activity, amongst others. Phenolic characterisation of South African Prunus salicina Lindl. plums is necessary to fully evaluate their potential health benefits. An HPLC method using diode-array detection (DAD for quantification of phenolic compounds was improved and fluorescence detection (FLD was added for quantification of flavan-3-ols. Validation of the HPLC-DAD-FLD method showed its suitability for quantification of 18 phenolic compounds, including flavan-3-ols using FLD, and phenolic acids, anthocyanins and flavonols using DAD. The method was suitable for characterisation of the phenolic composition of 11 South African plum cultivars and selections, including various types with yellow and red skin and flesh. The method was used in conjunction with mass spectrometry (MS to identify 24 phenolic compounds. Neochlorogenic acid and cyanidin-3-O-glucoside were the major compounds in most of the plums, while cyanidin-3-O-glucoside was absent in Sun Breeze plums with yellow skin and flesh. Post-column on-line coupling of the ABTS•+ scavenging assay with HPLC-DAD enabled qualitative evaluation of the relative contribution of individual phenolic compounds to the antioxidant activity. The flavan-3-ols, neochlorogenic acid and cyanidin-3-O-glucoside displayed the largest antioxidant response peaks.

  10. Determination of 20 trace elements and arsenic species for a realgar-containing traditional Chinese medicine Niuhuang Jiedu tablets by direct inductively coupled plasma-mass spectrometry and high performance liquid chromatography-inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Jin, Pengfei; Liang, Xiaoli; Xia, Lufeng; Jahouh, Farid; Wang, Rong; Kuang, Yongmei; Hu, Xin

    2016-01-01

    Niuhuang Jiedu tablet (NHJDT) is a realgar-containing traditional Chinese medicine. A direct inductively coupled plasma-mass spectrometry (ICP-MS) method for the simultaneous determination of 20 trace elements (Mg, K, Ca, Na, Fe, As, Zn, Sr, Ba, Cu, Mn, Ni, Pb, V, Cr, Se, Co, Mo, Cd, Hg) in NHJDT, as well as in water, gastric fluid and intestinal fluid was established. Meanwhile, a high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) method was developed for the determination of arsenite (As(III)), arsenate (As(V)), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA) and for the identification of arsenobetaine (AsB) and arsenocholine (AsC) in these extracts. Both methods were fully validated in the respect of linearity, sensitivity, precision, stability and accuracy. The reliability of the ICP-MS method was further evaluated using a certified standard reference material prepared from dried tomato leaves (NIST, SRM 1572a). The analysis showed that some manufacturers formulated lower amount of realgar than required in the Chinese Pharmacopoeia (ChP) in their preparations. In addition, almost same extraction profiles for total As and inorganic As were found in water and in gastrointestinal fluids, while higher extraction rates for other 19 elements were observed in gastrointestinal fluids. Our findings show that the toxicities of Hg, Cu, Cd and Pb in NHJDP are low, while the real As toxicity in NHJDT should be deeply investigated. PMID:26653746

  11. Multicapillary gas chromatography coupled to inductively coupled plasma-time-of-flight mass spectrometry for rapid mercury speciation analysis

    International Nuclear Information System (INIS)

    A simple, rapid and accurate method on the basis of multicapillary gas chromatography (MCGC) combined with inductively coupled plasma-time-of-flight mass spectrometry (ICP-TOFMS) was developed for speciation analysis of methylmercury (MeHg+) and inorganic mercury (Hg2+). The potential of the ICP-TOFMS for transient multi-isotope detection of very short signals (peak width of 0.4 s at half peak height) was evaluated. Two injection systems (purge-and-trap (PTI) and split (SI) injections) were compared in terms of species separation resolution and transient signal profile. Using purge-and-trap injection, after in situ derivatization of the ionic mercury species with sodium tetraethylborate, a baseline separation of MeHg+ and Hg2+ was achieved within a chromatographic run of +) was used as internal standard. Detection limits of 16 and 257 fg g-1 for MeHg+ (as Hg) and Hg2+, respectively, were achieved. The analytical precision (R.S.D. (%)) for 10 successive injections of a standard mixture containing 10 pg MeHg+ (as Hg) and Hg2+ was 1.2% for MeHg+ and 4.1% for Hg2+. The method was validated by analysis of two biological certified reference materials (CRM): a dogfish muscle (DORM-2) and a freeze-dried tuna fish (CRM 464)

  12. Elemental labelling combined with liquid chromatography inductively coupled plasma mass spectrometry for quantification of biomolecules: A review

    OpenAIRE

    Kretschy, Daniela; Koellensperger, Gunda; Hann, Stephan

    2012-01-01

    This article reviews novel quantification concepts where elemental labelling is combined with flow injection inductively coupled plasma mass spectrometry (FI-ICP-MS) or liquid chromatography inductively coupled plasma mass spectrometry (LC–ICP-MS), and employed for quantification of biomolecules such as proteins, peptides and related molecules in challenging sample matrices. In the first sections an overview on general aspects of biomolecule quantification, as well as of labelling will be pre...

  13. Review of online coupling of sample preparation techniques with liquid chromatography.

    Science.gov (United States)

    Pan, Jialiang; Zhang, Chengjiang; Zhang, Zhuomin; Li, Gongke

    2014-03-01

    Sample preparation is still considered as the bottleneck of the whole analytical procedure, and efforts has been conducted towards the automation, improvement of sensitivity and accuracy, and low comsuption of organic solvents. Development of online sample preparation techniques (SP) coupled with liquid chromatography (LC) is a promising way to achieve these goals, which has attracted great attention. This article reviews the recent advances on the online SP-LC techniques. Various online SP techniques have been described and summarized, including solid-phase-based extraction, liquid-phase-based extraction assisted with membrane, microwave assisted extraction, ultrasonic assisted extraction, accelerated solvent extraction and supercritical fluids extraction. Specially, the coupling approaches of online SP-LC systems and the corresponding interfaces have been discussed and reviewed in detail, such as online injector, autosampler combined with transport unit, desorption chamber and column switching. Typical applications of the online SP-LC techniques have been summarized. Then the problems and expected trends in this field are attempted to be discussed and proposed in order to encourage the further development of online SP-LC techniques. PMID:24560367

  14. On-line concentration sample stacking coupled with water-in-oil microemulsion electrokinetic chromatography.

    Science.gov (United States)

    Huang, Hsi-Ya; Liu, Wan-Ling; Singco, Brenda; Hsieh, Shih-Huan; Shih, Yung-Han

    2011-10-21

    This study describes for the first time, the ability of a normal stacking mode (NSM) on-line concentration step coupled with water-in-oil (W/O) microemulsion electrokinetic chromatography (MEEKC), using six common penicillin antibiotics (oxacillin, penicillin V, penicillin G, nafcillin, ampicillin, and amoxicillin) as test analytes. Optimization of penicillin separation in the conventional W/O MEEKC system demonstrated that change in the type and concentration of the oil phase (1-butanol) and column temperature had a pronounced effect on the separation. With the subsequent development of the NSM coupled with W/O MEEKC, improved separation and detection sensitivities were observed when an organic solvent plug (1-propanol; 1.04 cm) was placed between the W/O microemulsion and the sample solutions. This could be attributed to the solution viscosity difference between the aqueous sample zone and the organic solvent plug causing the penicillin to be stacked in this 1-propanol plug. The optimal NSM W/O MEEKC provided about 12-fold increase in detection sensitivity compared with conventional sample injection (50 mbar, 3 s). Finally, this proposed method was successfully applied in the analyses of several food samples (porcine organs) spiked with penicillin. PMID:21689819

  15. SPECIATION OF SELENIUM(IV) AND SELENIUM(VI) USING COUPLED ION CHROMATOGRAPHY: HYDRIDE GENERATION ATOMIC ABSORPTION SPECTROMETRY

    Science.gov (United States)

    A simple method was developed to speciate inorganic selenium in the microgram per liter range using coupled ion chromatography-hydride generation atomic absorption spectrometry. Because of the differences in toxicity and adsorption behavior, determination of the redox states selenite, Se(IV), and s...

  16. Multivariate analysis of progressive thermal desorption coupled gas chromatography-mass spectrometry.

    Energy Technology Data Exchange (ETDEWEB)

    Van Benthem, Mark Hilary; Mowry, Curtis Dale; Kotula, Paul Gabriel; Borek, Theodore Thaddeus, III

    2010-09-01

    Thermal decomposition of poly dimethyl siloxane compounds, Sylgard{reg_sign} 184 and 186, were examined using thermal desorption coupled gas chromatography-mass spectrometry (TD/GC-MS) and multivariate analysis. This work describes a method of producing multiway data using a stepped thermal desorption. The technique involves sequentially heating a sample of the material of interest with subsequent analysis in a commercial GC/MS system. The decomposition chromatograms were analyzed using multivariate analysis tools including principal component analysis (PCA), factor rotation employing the varimax criterion, and multivariate curve resolution. The results of the analysis show seven components related to offgassing of various fractions of siloxanes that vary as a function of temperature. Thermal desorption coupled with gas chromatography-mass spectrometry (TD/GC-MS) is a powerful analytical technique for analyzing chemical mixtures. It has great potential in numerous analytic areas including materials analysis, sports medicine, in the detection of designer drugs; and biological research for metabolomics. Data analysis is complicated, far from automated and can result in high false positive or false negative rates. We have demonstrated a step-wise TD/GC-MS technique that removes more volatile compounds from a sample before extracting the less volatile compounds. This creates an additional dimension of separation before the GC column, while simultaneously generating three-way data. Sandia's proven multivariate analysis methods, when applied to these data, have several advantages over current commercial options. It also has demonstrated potential for success in finding and enabling identification of trace compounds. Several challenges remain, however, including understanding the sources of noise in the data, outlier detection, improving the data pretreatment and analysis methods, developing a software tool for ease of use by the chemist, and demonstrating our belief

  17. Determination of Nitric Oxide-Derived Nitrite and Nitrate in Biological Samples by HPLC Coupled to Nitrite Oxidation

    OpenAIRE

    Wu, Anguo; Duan, Tingting; Tang, Dan; Xu, Youhua; Feng, Liang; Zheng, Zhaoguang; Zhu, Jiaxiao; Wang, Rushang; Zhu, Quan

    2013-01-01

    Nitrite and nitrate are main stable products of nitric oxide, a pivotal cellular signaling molecule, in biological fluids. Therefore, accurate measurement of the two ions is profoundly important. Nitrite is difficult to be determined for a larger number of interferences and unstable in the presence of oxygen. In this paper, a simple, cost-effective and accurate HPLC method for the determination of nitrite and nitrate was developed. On the basis of the reaction that nitrite is oxidized rapidly...

  18. Measurement of arsenic compounds in water by HPLC-ICP-MS

    OpenAIRE

    Watts, M. J.; O'Reilly, J.; Smiles, C.A.

    2007-01-01

    This report provides a brief introduction to the application of high-pressure liquid chromatography coupled to inductively coupled plasma mass spectrometry (HPLC-ICP-MS) to determine the concentration of various arsenic species in water samples. It describes the validation of this arsenic speciation method developed under the Laboratory Maintenance and Development Capability Programme to provide data on arsenic speciation in a range of challenging sample matrices to support BGS...

  19. Identification of Polish cochineal (Porphyrophora polonica L.) in historical textiles by high-performance liquid chromatography coupled with spectrophotometric and tandem mass spectrometric detection.

    Science.gov (United States)

    Lech, Katarzyna; Jarosz, Maciej

    2016-05-01

    The present work reports a method for identification of Polish cochineal (Porphyrophora polonica L.) in historical fabrics by the use of high-performance liquid chromatography coupled with diode array and tandem mass spectrometric detection with electrospray ionization (HPLC-DAD-ESI MS/MS). This hyphened technique allows detection and identification of 16 new minor colorants present in the discussed scale insect (including two previously observed by Wouters and Verhecken (Ann Soc Entomol Fr. 1989;25:393-410), but specified only as compounds of unknown structures) that do not occur (e.g., in American cochineal). The MS/MS experiments, complemented with UV-VIS data, enable identification of mono- and di-, C- and O-hexosides of kermesic and flavokermesic acids or their derivatives. The present paper introduces a fingerprint of color compounds present in Polish cochineal and defines them, particularly pp6 (ppI, O-hexoside of flavokermesic acid), as its markers allow distinguishing of Polish-cochineal reds from the American ones. Usefulness of the selected set of markers for identification of Polish cochineal has been demonstrated in the examination of textiles from the collection of the National Museum in Warsaw using the multiple reaction monitoring (MRM) method, originally elaborated on the basis of this study. PMID:26935929

  20. [Simultaneous determination of four phthalate esters in water samples using ultrasound-assisted dispersive liquid-liquid microextraction coupled with high performance liquid chromatography].

    Science.gov (United States)

    Ma, Yanling; Chen, Lingxin; Ding, Yangjun; Ming, Yongfei; Li, Jinhua

    2013-02-01

    Ultrasound-assisted dispersive liquid-liquid microextraction coupled with high performance liquid chromatography (UA-DLLME-HPLC) was developed for the determination of four typical phthalate esters (PAEs). The analyzed PAEs included dimethyl phthalate (DMP), diethyl phthalate (DEP), dibutyl phthalate (DBP) and di-n-octyl phthalate (DnOP). The UA-DLLME parameters such as types/volumes of extraction/dispersion solvents, ultrasonic time, ionic strength and extraction time, were investigated. Enrichment factor (EF)was employed to evaluate the extraction efficiency. The conditions were finally chosen: CCl4 (40 microL)/ acetonitrile (1.0 mL) as extraction/dispersion solvents; 30 g/L NaCl; ultrasound/centrifugation of 5 min. Under the optimized extraction conditions, UA-DLLME exhibited strong enrichment ability for the four PAEs. The EFs for DMP, DEP, DBP and DnOP obtained were 71, 144, 169 and 159, respectively. The limits of detection were 3.78, 1.77, 3.07 and 3.30 microg/L for DMP, DEP, DBP and DnOP, respectively. The satisfactory recoveries for three water samples at three spiked levels ranged from 82.99%-114.47%, with the relative standard deviations of 1.93%-8.31%. It is a convenient, speedy, environmentally benign method for the routine analysis of PAEs in water samples. PMID:23697182

  1. Solution for blank and matrix difficulties encountered during phthalate analysis of edible oils by high performance liquid chromatography coupled with tandem mass spectrometry.

    Science.gov (United States)

    Vavrouš, Adam; Pavloušková, Jana; Ševčík, Václav; Vrbík, Karel; Čabala, Radomír

    2016-07-22

    Worldwide production of phthalates has led to their undesirable presence in the food chain. Particularly edible oils have become an area of growing concern owing to numerous reported occurrences of phthalates. The analytical methods used in this field face difficulties associated mainly with matrix complexity or phthalate contamination which this study has aimed to describe and resolve. The proposed procedure consisting of liquid-liquid extraction, solid phase extraction and high performance liquid chromatography coupled with tandem mass spectrometry allowed us to analyze simultaneously 6 individual phthalates and 2 phthalate isomeric mixtures. DSC-18 SPE phase was selected for cleanup owing to the most efficient co-extract removal (assessed using high resolution mass spectrometry). Several sources of phthalate contamination were identified, however, the mobile phase was the most serious. The key improvement was achieved by equipping a contamination trap, a 50-mm reverse phase HPLC column, generating a delay between target and mobile phase peaks of the same compounds. RSDs ranging between 2.4 and 16 % confirm good precision and LOQs between 5.5 and 110μgkg(-1) reflect satisfactory blank management. With up to 19 occurrences in 25 analyzed edible oil samples and levels up to 33mgkg(-1), bis(2-ethylhexyl), diisononyl and diisodecyl phthalates were the most important contaminants. PMID:27318508

  2. Fast determination of arsenosugars in algal extracts by narrow bore high-performance liquid chromatography-inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Todolí, José Luis; Grotti, Marco

    2010-11-19

    The potential of narrow bore high-performance liquid chromatography (HPLC) with detection by inductively coupled plasma mass spectrometry (ICP-MS) for fast determination of arsenosugars in algal extracts was explored. The retention behavior of four naturally occurring dimethylarsinoylribosides on an anion-exchange microbore column was investigated, with the mobile phase flow rate ranging from 60 to 200μLmin(-1). A low sample consumption system consisting of a micronebulizer and a low inner volume cyclonic spray chamber was used as the interface between the micro-column and the ICP mass spectrometer. Both the high efficiency nebulizer, HEN, and the PFA micronebulizer were tested, with the former providing 20-50% greater sensitivity than PFA (depending on the liquid flow rate), but comparable limits of detection and slightly lower chromatographic resolution. With the setup employed and under the optimal conditions, a satisfactory separation of the arsenosugars was achieved in less than 5min. The instrumental limit of detection was 0.20μgAsL(-1) and the precision was better than 3% (RSD%, n=5). The accuracy of the determination was verified by the analysis of a reference algal extract, obtaining values in good agreement with the reference ones. PMID:20965508

  3. Metsulfuron-methyl Molecularly Imprinted Stir Bar Sorptive Extraction Coupled with High Performance Liquid Chromatography for Trace Sulfonylurea Herbicides Analysis in Complex Samples

    Institute of Scientific and Technical Information of China (English)

    XU Zhi-gang; DU Zhuo; LIAN Hai-xian; HU Yu-ling; LI Gong-ke

    2012-01-01

    Metsulfuron-methyl molecularly imprinted polymer(MIP)-coated stir bar was prepared for sorptive extraction of sulfonylurea herbicides in complex samples.The MIP-coating was about 21.3 μm thickness with the relative standard deviation(RSD) of 4.4%(n=10).It was homogeneous and porous with good thermal stability and chemical stability.The extraction capability of the MIP-coating was 2.8 timcs over that of the non-imprinted polymer (NIP)-coating in hexane.The MIP-coating exhibited selective adsorption ability to the template and its analogues.The extraction conditions,including extraction solvent,desorption solvent,extraction time,desorption time and stirring speed,were optimized.A method for the determination of six sulfonylurea herbicides by MIP-coated stir bar sorptive extraction coupled with high performance liquid chromatography(HPLC) was developed.The linear range was 10-200 μg/L and the detection limits were within a range of 2.0-3.3 μg/L.It was also applied to the analysis of sulfonylurea herbicides in spiked river water,soil and rice samples.

  4. Simultaneous Determination of Flavonoids, Isochlorogenic Acids and Triterpenoids in Ilex hainanensis Using High Performance Liquid Chromatography Coupled with Diode Array and Evaporative Light Scattering Detection

    Directory of Open Access Journals (Sweden)

    Hua-Gang Liu

    2013-03-01

    Full Text Available A high performance liquid chromatography coupled with diode array and evaporative light scattering detection (HPLC-DAD-ELSD method for simultaneous determination of eight major bioactive compounds including two flavonoids (rutin and eriodictyol-7-O-β-D-glucopyranoside, two isochlorogenic acids (isochlorogenic acid A and isochlorogenic acid C and four triterpenoids (ilexhainanoside D, ilexsaponin A1, ilexgenin A and ursolic acid in Ilex hainanensis has been developed for the first time. The 283 nm wavelength was chosen for determination of two flavonoids and two isochlorogenic acids. ELSD was applied to determine four triterpenoids. The analysis was performed on an Agilent Zorbax SB-C18 column (250 × 4.6 mm i.d., 5 µm with gradient elution of 0.2% formic acid in water and acetonitrile. The method was validated for linearity, limit of detection, limit of quantification, precision, repeatability and accuracy. The proposed method has been successfully applied for simultaneous quantification of the analytes in four samples of Ilex hainanensis, which is helpful for quality control of this plant.

  5. Online screening of nitric oxide scavengers in natural products using high performance liquid chromatography coupled with tandem diode array and fluorescence detection.

    Science.gov (United States)

    Li, Dapeng; Wang, Ting; Guo, Yujie; Hu, Yuanjia; Yu, Boyang; Qi, Jin

    2015-12-18

    Nitric oxide (NO) is an important cellular signaling molecule with extensive physiological and pathophysiological effects. NO scavengers have the potential to treat inflammation, septic shock and other related diseases, and numerous examples have been chemically synthesized or isolated from natural products. The chemical diversity of natural products, however, means that a huge effort is necessary to efficiently screen and identify bioactive compounds, especially NO scavengers. In this article, we propose an effective analytical method to screen for NO scavengers in three natural products using an online system that couples high performance liquid chromatography with tandem diode array and fluorescence detection (HPLC-DAD-FLD). Eighteen compounds from radix of Scutellaria baicalensis Georgi and green tea displayed significant NO scavenging activity whereas components of Pueraria lobata (Willd.) Ohwi had no discernable activity. The structures of the active compounds were elucidated using Agilent Accurate-Mass Q-TOF LC/MS system. Preliminary analysis of structure-activity relationships indicated that, in flavonoids, a 2,3-double bond and a 3-H atom or a 3-OH group are essential for activity. In tannins, poly-hydroxyl groups are important for NO scavenging activity. Method validation indicated that the newly developed method is both reliable and repeatable. The online method that we present provides a simple, rapid and effective way to identify and characterize NO scavengers present in natural products. PMID:26607316

  6. Evaluation of different extraction procedures for determination of organic Mercury species in petroleum by high performance liquid chromatography coupled with cold vapor atomic fluorescence spectrometry.

    Science.gov (United States)

    Yun, Zhaojun; He, Bin; Wang, Zhenhua; Wang, Thanh; Jiang, Guibin

    2013-03-15

    An extraction procedure for extracting organic mercury species including methylmercury (MeHg) and ethylmercury (EtHg) from petroleum samples was developed. Three extraction methods (shaking, ultrasonic and microwave assisted extraction) using different extraction solvents (TMAH, KOH/CH3OH, HCl and acidic CuSO4/KBr) were investigated by comparing the extraction efficiency of the organic mercury species. Microwave assisted extraction at 60 W for 5 min using TMAH (tetramethylammonium hydroxide, 25%, m/v) provided the most satisfactory extraction efficiency for MeHg and EtHg in petroleum at 86.7% ± 3.4% and 70.6% ± 5.9%, respectively. Speciation analysis of mercury was done by on-line coupling of high performance liquid chromatography with cold vapor generation atomic fluorescence spectrometry (HPLC-CV-AFS). The proposed method was successfully applied to analyze several crude oil and light oil samples. The concentrations of MeHg ranged from under detection limit to 0.515 ng g(-1), whereas EtHg was not detected in the samples. This method can be a very useful tool in evaluating the risk of mercury emissions from petroleum. PMID:23598095

  7. Analysis of sulfate metabolites of the doping agents oxandrolone and danazol using high performance liquid chromatography coupled to tandem mass spectrometry.

    Science.gov (United States)

    Rzeppa, S; Viet, L

    2016-09-01

    The direct detection of sulfate conjugates of anabolic androgenic steroids (AAS) can be a powerful tool in doping control analysis. By skipping the solvolysis step analysis time can be reduced, and due to long term sulfate metabolites the detection time can be significantly extended as demonstrated for some AAS. This study presents the successful identification of sulfate metabolites of the doping agents oxandrolone and danazol in excretion urines by high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS). The sulfate conjugate of 17β-hydroxymethyl-17α-methyl-18-nor-2-oxa-5α-androsta-13-en-3-one could be identified as a new metabolite of oxandrolone. Sulfate conjugates of the danazol metabolites ethisterone and 2α-hydroxymethylethisterone were identified in an excretion urine for the first time. In addition, these sulfate conjugates were synthesized successfully. For a confirmation analysis, the number of analytes can be increased by additional sulfate conjugates of danazol metabolites (2-hydroxymethyl-1,2-dehydroethisterone and 6β-hydroxy-2-hydroxymethylethisterone), which were also identified for the first time. The presented validation data underline the suitability of the identified sulfate conjugates for doping analysis with regard to the criteria given by the technical documents of the World Anti-Doping Agency (WADA). PMID:27394004

  8. Arsenic speciation in edible alga samples by microwave-assisted extraction and high performance liquid chromatography coupled to atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Garcia-Salgado, S. [Departamento de Ingenieria Civil: Tecnologia Hidraulica y Energetica, Escuela Universitaria de Ingenieria Tecnica de Obras Publicas, Universidad Politecnica de Madrid, Alfonso XII 3 y 5, 28014 Madrid (Spain); Quijano, M.A., E-mail: marian.quijano@upm.es [Departamento de Ingenieria Civil: Tecnologia Hidraulica y Energetica, Escuela Universitaria de Ingenieria Tecnica de Obras Publicas, Universidad Politecnica de Madrid, Alfonso XII 3 y 5, 28014 Madrid (Spain); Bonilla, M.M. [Departamento de Ingenieria Civil: Tecnologia Hidraulica y Energetica, Escuela Universitaria de Ingenieria Tecnica de Obras Publicas, Universidad Politecnica de Madrid, Alfonso XII 3 y 5, 28014 Madrid (Spain)

    2012-02-10

    Highlights: Black-Right-Pointing-Pointer Total As and As species were analyzed in edible marine algae. Black-Right-Pointing-Pointer A microwave-assisted extraction method with deionized water was applied. Black-Right-Pointing-Pointer As compounds identified comprised DMA, As(V) and four arsenosugars Black-Right-Pointing-Pointer Considerably high As(V) concentrations were found in the most of the algae studied. - Abstract: Twelve commercially available edible marine algae from France, Japan and Spain and the certified reference material (CRM) NIES No. 9 Sargassum fulvellum were analyzed for total arsenic and arsenic species. Total arsenic concentrations were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) after microwave digestion and ranged from 23 to 126 {mu}g g{sup -1}. Arsenic species in alga samples were extracted with deionized water by microwave-assisted extraction and showed extraction efficiencies from 49 to 98%, in terms of total arsenic. The presence of eleven arsenic species was studied by high performance liquid chromatography-ultraviolet photo-oxidation-hydride generation atomic-fluorescence spectrometry (HPLC-(UV)-HG-AFS) developed methods, using both anion and cation exchange chromatography. Glycerol and phosphate sugars were found in all alga samples analyzed, at concentrations between 0.11 and 22 {mu}g g{sup -1}, whereas sulfonate and sulfate sugars were only detected in three of them (0.6-7.2 {mu}g g{sup -1}). Regarding arsenic toxic species, low concentration levels of dimethylarsinic acid (DMA) (<0.9 {mu}g g{sup -1}) and generally high arsenate (As(V)) concentrations (up to 77 {mu}g g{sup -1}) were found in most of the algae studied. The results obtained are of interest to highlight the need to perform speciation analysis and to introduce appropriate legislation to limit toxic arsenic species content in these food products.

  9. Selenium speciation analysis in a sediment using strong anion exchange and reversed phase chromatography coupled with inductively coupled plasma-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ochsenkuehn-Petropoulou, M.; Michalke, B.; Kavouras, D.; Schramel, P

    2003-02-22

    An analytical procedure for selenium speciation of analysis of selenourea (SeU), selenoethionine (SeE), selenomethionine (SeM), Se(VI), Se(IV), dimethylselenide (dMeSe) and dimethyldiselenide (dMedSe) was developed, based on two complementary liquid chromatography (LC) techniques coupled with inductively coupled plasma-mass spectrometry (ICP-MS). Specifically, strong anion exchange (SAX) chromatography coupled with ICP-MS was used for the separation and quantification of all the earlier mentioned Se compounds, except for the two methyl selenides, which could be separated and determined by reversed phase chromatography coupled with ICP-MS. This procedure was applied to a soil sample from the warm springs area of Thermopyles (Greece). For leaching the Se species from the soil sample, four extraction methods, using water at ambient temperature, hot water, methanol and 0.5 M HCl, were tested for their efficiency of extracting the different Se species. The speciation results obtained by the LC-ICP-MS methods were compared with those obtained by voltammetric techniques. The determination of total selenium in the sample was achieved by graphite furnace atomic absorption spectrometry, as well as by ICP-atomic emission spectrometry, after suitable digestion of the sediment sample.

  10. Determination of Vitamin C (Ascorbic Acid Using High Performance Liquid Chromatography Coupled with Electrochemical Detection

    Directory of Open Access Journals (Sweden)

    Ondrej Zitka

    2008-11-01

    Full Text Available Vitamin C (ascorbic acid, ascorbate, AA is a water soluble organic compound that participates in many biological processes. The main aim of this paper was to utilize two electrochemical detectors (amperometric – Coulouchem III and coulometric – CoulArray coupled with flow injection analysis for the detection of ascorbic acid. Primarily, we optimized the experimental conditions. The optimized conditions were as follows: detector potential 100 mV, temperature 25 °C, mobile phase 0.09% TFA:ACN, 3:97 (v/v and flow rate 0.13 mL·min-1. The tangents of the calibration curves were 0.3788 for the coulometric method and 0.0136 for the amperometric one. The tangent of the calibration curve measured by the coulometric detector was almost 30 times higher than the tangent measured by the amperometric detector. Consequently, we coupled a CoulArray electrochemical detector with high performance liquid chromatography and estimated the detection limit for AA as 90 nM (450 fmol per 5 μL injection. The method was used for the determination of vitamin C in a pharmaceutical preparations (98 ± 2 mg per tablet, in oranges (Citrus aurantium (varied from 30 to 56 mg/100 g fresh weight, in apples (Malus sp. (varied from 11 to 19 mg/100 g fresh weight, and in human blood serum (varied from 38 to 78 μM. The recoveries were also determined.

  11. Chemical fingerprinting and quantitative constituent analysis of Siwu decoction categorized formulae by UPLC-QTOF/MS/MS and HPLC-DAD

    OpenAIRE

    Su, Shulan; Cui, Wenxia; Zhou, Wei; Duan, Jin-Ao; Shang, Erxin; Yuping TANG

    2013-01-01

    Background Siwu decoction categorized formulae (SWDCF) are widely used for treating gynecological diseases. This study aims to elucidate the differences of bioactive constituents in SWDCF by ultra-high performance liquid chromatography coupled with time-of-flight mass spectrometry (UPLC - QTOF - MS /MS) and HPLC-DAD. Methods An efficient method based on UPLC - QTOF - MS /MS was developed for identifying the chemical profiles of SWDCF. HPLC-DAD method was used for quantifying seven chemical ma...

  12. Headspace in-tube microextraction coupled with micellar electrokinetic chromatography of neutral aromatic compounds.

    Science.gov (United States)

    Cho, Sung Min; Park, Bum Su; Jung, Woo Sung; Lee, Sang Won; Jung, Yunhwan; Chung, Doo Soo

    2016-02-01

    Headspace (HS) extraction can be carried out easily and aptly via single drop microextraction coupled with capillary electrophoresis (CE). However, one drawback is the difficulty of keeping the single drop stably at the capillary tip. To solve this problem, we have recently demonstrated HS in-tube microextraction (ITME) of acidic compounds such as chlrophenols in an acidic sample using a basic run buffer plug in the separation capillary for CE as an acceptor phase. In this report, an organic acceptor plug in a capillary was used to extract neutral organic volatile pollutants such as BTEX (benzene, toluene, ethylbenzene, and m-xylene). After extraction, the analytes enriched in the organic acceptor plug were analyzed with micellar electrokinetic chromatography (MEKC). The enrichment factors for BTEX in a standard solution were up to 350 under an optimal condition of 25°C for 20 min. As an application, BTEX spiked into bottled water were analyzed with HS-ITME-MEKC, and the enrichment factors for BTEX were up to 320. The limits of detections were 1-4 ppb, which are at least 200 times lower than the US Environmental Protection Agency guidelines for drinking water, except benzene. The entire procedure of HS-ITME-MEKC was carried out automatically using a commercial CE instrument. PMID:26653509

  13. Direct coupling of packed column supercritical fluid chromatography to continuous corona discharge ion mobility spectrometry.

    Science.gov (United States)

    Rahmanian, A; Ghaziaskar, H S; Khayamian, T

    2013-01-11

    In this study, packed column supercritical fluid chromatography (SFC) was directly coupled to a continuous corona discharge (CD) ion mobility spectrometer (IMS) with several modifications. The main advantage of the developed detector is its capability to introduce full column effluent up to 2000 mL min(-1) CO(2) gas directly into the IMS cell relative to 40 mL min(-1) CO(2) gas as a maximum tolerance, reported for the previous IMS detectors. This achievement was made possible because of using corona discharge instead of (63)Ni as an ionization source and locating the inlet and outlet of the CO(2) gas in the counter electrode of the CD in opposite direction. In addition, a heated interface was placed between back pressure regulator (BPR) and the IMS cell to heat the output of the BPR for introducing sample as the gas phase into the IMS cell. Furthermore, a make-up methanol flow was introduced between the column outlet and BPR to provide a more uniform flow through the BPR and also to prevent freezing and deposition of the analytes in the BPR. The performance of the SFC-CD-IMS was evaluated by analysis of testosterone, medroxyprogesterone, caffeine, and theophylline as test compounds and figures of merit for these compounds have been calculated. PMID:23261285

  14. Liquid chromatography-mass spectrometry coupling by the intermediary of a liquid micro chromatography-electro spray interface; Couplage chromatographie liquide-spectrometrie de masse par l`intermediaire d`une interface electrospray-microchromatographie liquide

    Energy Technology Data Exchange (ETDEWEB)

    Gillard Factor, C.

    1996-12-06

    The objective of this work is to realize a liquid chromatography- mass spectrometry coupling by the intermediary of an electro spray interface and the evaluation of performances of tis analytical tool to study pollutants in water, and more particularly pesticides whom maximum admissible concentration in a table water is 0.1{mu}g/l. This study has allowed to bring to the fore the interest of the ionization mode by electro spray in a LC/MS coupling to identify and quantify pesticides in the state of traces without treating the sample. Then, it was demonstrated the usefulness of this analytical tool to detect high molecular masses molecules. (N.C.)

  15. Temperature-programmed high-performance liquid chromatography coupled to isotope ratio mass spectrometry.

    Science.gov (United States)

    Godin, Jean-Philippe; Hopfgartner, Gérard; Fay, Laurent

    2008-09-15

    The utility of liquid chromatography coupled to the isotope ratio mass spectrometry technique (LC-IRMS) has already been established through a variety of successful applications. However, the analytical constraint related to the use of aqueous mobile phases limits the LC separation mechanism. We report here a new strategy for high-precision (13)C isotopic analyses based on temperature-programmed LC-IRMS using aqueous mobile phases. Under these conditions, the isotopic precision and accuracy were studied. On one hand, experiments were carried out with phenolic acids using isothermal LC conditions at high temperature (170 degrees C); on the other hand, several experiments were performed by ramping the temperature, as conventionally used in a gas chromatography-based method with hydrosoluble fatty acids and pulses of CO 2 reference gas. In isothermal conditions at 170 degrees C, despite the increase of the CO 2 background, p-coumaric acid and its glucuronide conjugate gave reliable isotopic ratios compared to flow injection analysis-isotopic ratio mass spectrometry (FIA-IRMS) analyses (isotopic precision and accuracy are lower than 0.3 per thousand). On the opposite, for its sulfate conjugate, the isotopic accuracy is affected by its coelution with p-coumaric acid. Not surprisingly, this study also demonstrates that at high temperature (170 degrees C), a compound eluting with long residence time (i.e., ferulic acid) is degraded, affecting thus the delta (13)C (drift of 3 per thousand) and the peak area (compared to FIA-IRMS analysis at room temperature). Quantitation is also reported in isothermal conditions for p-coumaric acid in the range of 10-400 ng/mL and with benzoic acid as an internal standard. For temperature gradient LC-IRMS, in the area of the LC gradient (set up at 20 degrees C/min), the drift of the background observed produces a nonlinearity of SD (delta (13)C) approximately 0.01 per thousand/mV. To circumvent this drift, which impacts severely the

  16. Quality assessment of traditional Chinese medicine herb couple by high-performance liquid chromatography and mass spectrometry combined with chemometrics.

    Science.gov (United States)

    Cheng, Tao-Fang; Jia, Yu-Ran; Zuo, Zheng; Dong, Xin; Zhou, Ping; Li, Ping; Li, Fei

    2016-04-01

    This study was designed to develop a simple, specific and reliable method to overall analyze the chemical constituents in clematidis radix et rhizome/notopterygii rhizome et radix herb couple using high-performance liquid chromatography coupled with tandem mass spectrometry and multiple chemometric analysis. First, the separation and qualitative analysis of herb couple was achieved on an Agilent Zorbax Eclipse Plus C18 column (250 mm × 4.6 mm, 5 μm), and 69 compounds were unambiguously or tentatively identified. Moreover, in quantitative analysis, eight ingredients including six coumarins and two triterpenoid sapogenins were quantified by high-performance liquid chromatography coupled with tandem mass spectrometry. In terms of good linearity (r(2) ≥ 0.9995) with a relatively wide concentration range, recovery (85.40-102.50%) and repeatability (0.99-4.45%), the validation results suggested the proposed method was reliable, and successfully used to analyze ten batches of herb couple samples. Then, hierarchical cluster analysis and principal component analysis were used to classify samples and search significant ingredients. The results showed that ten batches of herb couple samples were classified into three groups, and six compounds were found for its better quality control. PMID:26834048

  17. Analysis of plasma protein adsorption onto DC-Chol-DOPE cationic liposomes by HPLC-CHIP coupled to a Q-TOF mass spectrometer

    KAUST Repository

    Capriotti, Anna Laura

    2010-09-22

    Plasma protein adsorption is regarded as a key factor in the in vivo organ distribution of intravenously administered drug carriers, and strongly depends on vector surface characteristics. The present study aimed to characterize the "protein corona" absorbed onto DC-Chol-DOPE cationic liposomes. This system was chosen because it is one of the most efficient and widely used non-viral formulations in vitro and a potential candidate for in vivo transfection of genetic material. After incubation of human plasma with cationic liposomes, nanoparticle-protein complex was separated from plasma by centrifugation. An integrated approach based on protein separation by one-dimensional 12% polyacrylamide gel electrophoresis followed by the automated HPLC-Chip technology coupled to a high-resolution mass spectrometer was employed for protein corona characterization. Thirty gel lanes, approximately 2 mm, were cut, digested and analyzed by HPLC-MS/MS. Fifty-eight human plasma proteins adsorbed onto DC-Chol-DOPE cationic liposomes were identified. The knowledge of the interactions of proteins with liposomes can be exploited for future controlled design of colloidal drug carriers and possibly in the controlled creation of biocompatible surfaces of other devices that come into contact with proteins in body fluids. © 2010 Springer-Verlag.

  18. Improved Quality Control Method for Prescriptions of Polygonum capitatum through Simultaneous Determination of Nine Major Constituents by HPLC Coupled with Triple Quadruple Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Jun Zhang

    2013-09-01

    Full Text Available As a traditional Miao-nationality medicinal plant, Polygonum capitatum has been used in clinical practice for several thousand years. Its prescriptions, including three dosage forms: granules, capsule and tablet are known by the brand name Relinqing® and have played an indispensable role in the treatment of urinary system infection, pyelonephritis and kidney stones. However, no study about the comprehensive quality evaluation of Relinqing® has been reported. In the present paper, a method for the simultaneous determination of nine major compounds in three dosage forms of Relinqing® using HPLC coupled with triple quadrupole mass spectrometry (HPLC-QQQ MS was established to comprehensively evaluate their quality. The nine compounds, including four phenolic acids, four flavonoids and a lignin, were analyzed with acceptable linear regression relationship (r2, 0.9923–0.9992, precision (RSD, 1.25%–2.78%, repeatability (RSD, 2.05%%–3.47%, stability (RSD, 1.84%–3.72% and recovery (93.60%–108.54%, RSD ≤ 3.67%. The present study fills the gap in the multivariate quality control of Relinqing® and provides a valuable reference for quality standards and dosage reforming of this traditional Chinese medicine.

  19. Characterization of in vitro and in vivo metabolites of carnosic acid, a natural antioxidant, by high performance liquid chromatography coupled with tandem mass spectrometry.

    Science.gov (United States)

    Song, Yuelin; Yan, Haixia; Chen, Jinfeng; Wang, Yitao; Jiang, Yong; Tu, Pengfei

    2014-02-01

    Carnosic acid (CA) is a widely employed antioxidant and the main active component in rosemary and sage, but its metabolism remains largely unknown. The present study investigated the metabolism of CA in vitro and in vivo for the first time, using high performance liquid chromatography coupled with hybrid triple quadrupole-linear ion trap mass spectrometry (HPLC-Q-trap-MS). A couple of scan modes were adopted in mass spectrometer domain, including Q1 full scan, neutral loss scan-information dependent acquisition-enhanced product ion (NL-IDA-EPI) and precursor ion scan-information dependent acquisition-enhanced product ion (PI-IDA-EPI). In particular, a prediction was carried out on the basis of in vitro metabolism results, and gave birth to a multiple ion monitoring-information dependent acquisition-enhanced product ion (MIM-IDA-EPI) mode aiming to detect the trace metabolites in CA-treated biological samples. A total of ten metabolites (M4-13), along with three degradative products (M1-3), were identified for CA from in vitro metabolism models, including liver microsomes of human and rats (HLMs and RLMs), human intestinal microsomes (HIMs) and two species of Cunninghamella elegans. Twelve (U1-12) and six (F1-6) metabolites were detected from CA-treated urine and feces, respectively. In addition, five metabolites (SM2-6) in vivo were purified and definitely identified using NMR spectroscopy. The results of both in vitro and in vivo metabolism studies indicated poor metabolic stability for CA, and the glucuronidation and oxidation metabolisms extensively occurred for CA in vitro, while oxidation, glucuronidation and methylation were the main metabolic pathways observed in vivo. PMID:24291799

  20. Multidimensional Separation of Natural Products Using Liquid Chromatography Coupled to Hadamard Transform Ion Mobility Mass Spectrometry

    Science.gov (United States)

    Liu, Wenjie; Zhang, Xing; Knochenmuss, Richard; Siems, William F.; Hill, Herbert H.

    2016-05-01

    A high performance liquid chromatograph (HPLC)was interfaced to an atmospheric drift tube ion mobility time of flight mass spectrometry. The power of multidimensional separation was demonstrated using chili pepper extracts. The ambient pressure drift tube ion mobility provided high resolving powers up to 166 for the HPLC eluent. With implementation of Hadamard transform (HT), the duty cycle for the ion mobility drift tube was increased from less than 1% to 50%, and the ion transmission efficiency was improved by over 200 times compared with pulsed mode, improving signal to noise ratio 10 times. HT ion mobility and TOF mass spectrometry provide an additional dimension of separation for complex samples without increasing the analysis time compared with conventional HPLC.

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

    Science.gov (United States)

    Molinelli, Alejandro R; Rose, Charles H

    2016-01-01

    Voriconazole and posaconazole are triazole antifungal compounds used in the treatment of fungal infections. Therapeutic drug monitoring of both compounds is recommended in order to guide drug dosing to achieve optimal blood concentrations. In this chapter we describe an HPLC-ESI-MS/MS method for the quantification of both compounds in human plasma or serum following a simple specimen preparation procedure. Specimen preparation consists of protein precipitation using methanol and acetonitrile followed by a cleanup step that involves filtration through a cellulose acetate membrane. The specimen is then injected into an HPLC-ESI-MS/MS equipped with a C18 column and separated over an acetonitrile gradient. Quantification of the drugs in the specimen is achieved by comparing the response of the unknown specimen to that of the calibrators in the standard curve using multiple reaction monitoring. PMID:26660172

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

    OpenAIRE

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

    2011-01-01

    A method for the analysis of flavonoids in Astragali Radix by high-performance liquid chromatography (HPLC) combined with photodiode-array detection (DAD) and an electrospray ionization (ESI) - mass spectrometry (MS) was developed. After the samples were extracted with ethanol, the optimum separation conditions for these analytes were achieved using a gradient elution system and a 2.0 × 150 mm Shimadzu VP-ODS column. Eight flavonoids were identified to exist in Astragali Radix based on their ...

  3. Supercritical Fluid Extraction Directly Coupled with Reversed Phase Liquid Chromatography for Quantitative Analysis of Analytes in Complex Matrices

    OpenAIRE

    Wang, Zhenyu

    2004-01-01

    The purpose of this research was to design a simple, novel interface for on-line coupling of Supercritical Fluid Extraction (SFE) with High Performance Reversed Phase Liquid Chromatography (HP-RPLC), and to explore its ability for quantitative analysis of analytes in different matrices. First, a simple interface was developed via a single one six-port injection valve to connect the SFE and LC systems. A water displacement method was utilized to eliminate decompressed CO2 gas in the solid phas...

  4. Identification of the Related Substances in Ampicillin Capsule by Rapid Resolution Liquid Chromatography Coupled with Electrospray Ionization Tandem Mass Spectrometry

    OpenAIRE

    Lei Zhang; Xian Long Cheng; Yang Liu; Miao Liang; Honghuan Dong; Beiran Lv; Wenning Yang; Zhiqiang Luo; Mingmin Tang

    2014-01-01

    Rapid Resolution Liquid Chromatography coupled with Electrospray Ionization Tandem Mass Spectrometry (RRLC-ESI-MSn) was used to separate and identify related substances in ampicillin capsule. The fragmentation behaviors of related substances were used to identify their chemical structures. Finally, a total of 13 related substances in ampicillin capsule were identified, including four identified components for the first time and three groups of isomers on the basis of the exact mass, fragmenta...

  5. Potential of on-line coupling of extraction and chromatography in the analysis of complex samples

    Czech Academy of Sciences Publication Activity Database

    Hyötyläinen, T.; Lüthje, K.; Rautiainen-Rämä, M.; Pól, Jaroslav; Ranta-Aho, O.; Riekkola, M. L.

    Kortrijk: I.O.P.M.S. vzw, 2004 - (Sandra, T.; Sandra, P.), J12 [International Symposium on Capillary Chromatography /27./. Riva del Garda (IT), 31.05.2004-04.06.2004] R&D Projects: GA AV ČR KJB4031405 Institutional research plan: CEZ:AV0Z4031919 Keywords : on-line - extraction * chromatography Subject RIV: CB - Analytical Chemistry, Separation

  6. Detection and quantification of new psychoactive substances (NPSs) within the evolved "legal high" product, NRG-2, using high performance liquid chromatography-amperometric detection (HPLC-AD).

    Science.gov (United States)

    Zuway, Khaled Y; Smith, Jamie P; Foster, Christopher W; Kapur, Nikil; Banks, Craig E; Sutcliffe, Oliver B

    2015-09-21

    The global increase in the production and abuse of cathinone-derived New Psychoactive Substances (NPSs) has developed the requirement for rapid, selective and sensitive protocols for their separation and detection. Electrochemical sensing of these compounds has been demonstrated to be an effective method for the in-field detection of these substances, either in their pure form or in the presence of common adulterants, however, the technique is limited in its ability to discriminate between structurally related cathinone-derivatives (for example: (±)-4′-methylmethcathinone (4-MMC, 2a) and (±)-4′-methyl-N-ethylmethcathinone (4-MEC, 2b) when they are both present in a mixture. In this paper we demonstrate, for the first time, the combination of HPLC-UV with amperometric detection (HPLC-AD) for the qualitative and quantitative analysis of 4-MMC and 4-MEC using either a commercially available impinging jet (LC-FC-A) or custom-made iCell channel (LC-FC-B) flow-cell system incorporating embedded graphite screen-printed macroelectrodes. The protocol offers a cost-effective, reproducible and reliable sensor platform for the simultaneous HPLC-UV and amperometric detection of the target analytes. The two systems have similar limits of detection, in terms of amperometric detection [LC-FC-A: 14.66 μg mL(-1) (2a) and 9.35 μg mL(-1) (2b); LC-FC-B: 57.92 μg mL(-1) (2a) and 26.91 μg mL(-1) (2b)], to the previously reported oxidative electrochemical protocol [39.8 μg mL(-1) (2a) and 84.2 μg mL(-1) (2b)], for two synthetic cathinones, prevalent on the recreational drugs market. Though not as sensitive as standard HPLC-UV detection, both flow cells show a good agreement, between the quantitative electroanalytical data, thereby making them suitable for the detection and quantification of 4-MMC and 4-MEC, either in their pure form or within complex mixtures. Additionally, the simultaneous HPLC-UV and amperometric detection protocol detailed herein shows a marked improvement

  7. [Characterization method for metallothioneins by reversed-phase liquid chromatography coupled with electrospray ionization mass spectrometry].

    Science.gov (United States)

    Huang, Zhiyong; Shen, Jincan; Zhuang, Zhixia; Wang, Xiaoru; Lee, Frank Sen-Chun

    2004-11-01

    Mammalian metallothioneins (MTs) usually have two major isoforms, MT-1 and MT-2, existing in tissues because of the genetic polymorphism. Metallothionein isoforms and sub-isoforms were characterized with a hyphenated technique of reversed-phase liquid chromatography (RPLC) coupled with electrospray ionization mass spectrometry (ESI-MS). The MT-isoform separation was carried out using a C8 narrow-bore column Vydac C8 (250 mm x 2.1 mm i.d., 5 microm, 30 nm). Buffer A was 5 mmol/L ammonium acetate in water (pH 6.0) and buffer B was 5 mmol/L ammonium acetate in methanol-water (1:1, v/v) (pH 6.0). A linear gradient elution was used by increasing buffer B from 10% to 37.5% within 40 min. The flow rate was set at 0.20 mL/min. The tentative formulas of MT isoforms and subisoforms were interpreted with the measured masses at the vicinity of apexes in total ion current chromatogram of ESI-MS and the reference data reported previously. The method was validated with the standard reference materials of MT-1 and MT-2. The results indicated that many MT species interpreted were in good agreement with the reference data reported. The MT sample from rabbit liver was measured with the established method. The results, of which the apo-MT was used by acidification of the sample for simplifying the mass spectra, showed that there were species of MT isoforms and subisoforms in rabbit livers. PMID:15807108

  8. Quantitative analysis of antibiotics in aquifer sediments by liquid chromatography coupled to high resolution mass spectrometry.

    Science.gov (United States)

    Tong, Lei; Liu, Hui; Xie, Cong; Li, Minjing

    2016-06-24

    A highly effective analytical method for multi-residue determination of antibiotics in aquifer sediments was first established in this study. Microwave-assisted solvent extraction (MASE) and solid-phase extraction were used for sample pre-concentration and purification, ultra-high performance liquid chromatography coupled to hybrid quadrupole-high resolution Orbitrap mass spectrometry (UHPLC-Q-Orbitrap) was applied for detection. For high resolution mass spectrometry (HRMS), the target compounds were tentatively identified by retention time and accurate mass which was measured with precursor ions in Target-SIM scan, and then confirmed by the monitoring of daughter ion fragments which were generated in dd-MS(2) scan. The results provided good mass accuracy with mass deviations below 2ppm (except norfloxacin with -2.3ppm) for quantitative analysis of the compounds by HRMS. Reasonable recoveries of all analytes were obtained more than 60% (except doxytetracycline) in fortification samples at concentrations higher than 10μgkg(-1). Relative standard deviations of repeatability and inter-day precision were below 21% and 11%. Limits of detection (LOD) ranged from 0.1 to 3.8μgkg(-1), whereas limits of quantification (LOQ) were established between 0.3-9.0μgkg(-1). The method was applied to analyze real aquifer sediment samples in different aquifer depth of 4.0, 7.5, 13.0 and 18.0m. Chlorotetracycline and ofloxacin were observed at relative high concentrations of 53 and 19μgkg(-1) respectively in 18.0m deepness. The exposure to low doses of these compounds in subsurface environment increases concerns on long-term ecological security of underground system. PMID:27215464

  9. Ionizing radiation effects in Acai oil analysed by gas chromatography coupled to mass spectrometry technique

    International Nuclear Information System (INIS)

    The Acai fruit is a well know Brazilian seed plant used in large scale as a source of feed stock, specially in the Brazilian North-east region. The Acai oil is use in many purposes from fuel sources to medicine. The scope of this paper is to analyzed the chemical structures modification of the acai oil after the ionizing radiation. The radiation were set in the range of 10 to 25 kGy in the extracted Acai oil. The analyses were made by gas chromatography coupled to mass spectrometry techniques. A GC/MS Shimatzu QP-5000 equipped with 30 meters DB-5 capillary column with internal diameter of 0.25 mm and 0.25 μm film thickness was used. Helium was used as carried gas and gave a column head pressure of 12 p.s.i. (1 p.s.i. = 6894.76 Pa) and an average flux of 1 ml/min. The temperature program for the GC column consisted of a 4-minutes hold at 75 deg C, a 15 deg C /min ramp to 200 deg C, 8 minutes isothermal. 20 deg C/min ramp to 250 deg C, 2 minutes isothermal. The extraction of the fatty acids was based on liquid-liquid method using chloroform as solvent. The chromatograms resulted shows the presences of the oleic acid and others fatty acids identify by the mass spectra library (NIST-92). The ionization radiation deplete the fatty acids presents in the Acai oil. Details on the chemical qualitative analytical is present as well in this work. (author)

  10. Ionizing radiation effects in Acai oil analysed by gas chromatography coupled to mass spectrometry technique

    Energy Technology Data Exchange (ETDEWEB)

    Valli, Felipe; Fernandes, Carlos Eduardo; Moura, Sergio; Machado, Ana Carolina; Furasawa, Helio Akira; Pires, Maria Aparecida Faustino; Bustillos, Oscar Vega [Instituto de Pesquisas Energeticas e Nucleares (IPEN-CNEN/SP), Sao Paulo, SP (Brazil)], E-mail: ovega@ipen.br

    2007-07-01

    The Acai fruit is a well know Brazilian seed plant used in large scale as a source of feed stock, specially in the Brazilian North-east region. The Acai oil is use in many purposes from fuel sources to medicine. The scope of this paper is to analyzed the chemical structures modification of the acai oil after the ionizing radiation. The radiation were set in the range of 10 to 25 kGy in the extracted Acai oil. The analyses were made by gas chromatography coupled to mass spectrometry techniques. A GC/MS Shimatzu QP-5000 equipped with 30 meters DB-5 capillary column with internal diameter of 0.25 mm and 0.25 {mu}m film thickness was used. Helium was used as carried gas and gave a column head pressure of 12 p.s.i. (1 p.s.i. = 6894.76 Pa) and an average flux of 1 ml/min. The temperature program for the GC column consisted of a 4-minutes hold at 75 deg C, a 15 deg C /min ramp to 200 deg C, 8 minutes isothermal. 20 deg C/min ramp to 250 deg C, 2 minutes isothermal. The extraction of the fatty acids was based on liquid-liquid method using chloroform as solvent. The chromatograms resulted shows the presences of the oleic acid and others fatty acids identify by the mass spectra library (NIST-92). The ionization radiation deplete the fatty acids presents in the Acai oil. Details on the chemical qualitative analytical is present as well in this work. (author)

  11. Quantitative and chemical fingerprint analysis for the quality evaluation of Receptaculum Nelumbinis by RP-HPLC coupled with hierarchical clustering analysis.

    Science.gov (United States)

    Wu, Yan-Bin; Zheng, Li-Jun; Yi, Jun; Wu, Jian-Guo; Chen, Ti-Qiang; Wu, Jin-Zhong

    2013-01-01

    A simple and reliable method of high-performance liquid chromatography with photodiode array detection (HPLC-DAD) was developed to evaluate the quality of Receptaculum Nelumbinis (dried receptacle of Nelumbo nucifera) through establishing chromatographic fingerprint and simultaneous determination of five flavonol glycosides, including hyperoside, isoquercitrin, quercetin-3-O-β-d-glucuronide, isorhamnetin-3-O-β-d-galactoside and syringetin-3-O-β-d-glucoside. In quantitative analysis, the five components showed good regression (R > 0.9998) within linear ranges, and their recoveries were in the range of 98.31%-100.32%. In the chromatographic fingerprint, twelve peaks were selected as the characteristic peaks to assess the similarities of different samples collected from different origins in China according to the State Food and Drug Administration (SFDA) requirements. Furthermore, hierarchical cluster analysis (HCA) was also applied to evaluate the variation of chemical components among different sources of Receptaculum Nelumbinis in China. This study indicated that the combination of quantitative and chromatographic fingerprint analysis can be readily utilized as a quality control method for Receptaculum Nelumbinis and its related traditional Chinese medicinal preparations. PMID:23337200

  12. Quantitative and Chemical Fingerprint Analysis for the Quality Evaluation of Receptaculum Nelumbinis by RP-HPLC Coupled with Hierarchical Clustering Analysis

    Directory of Open Access Journals (Sweden)

    Jin-Zhong Wu

    2013-01-01

    Full Text Available A simple and reliable method of high-performance liquid chromatography with photodiode array detection (HPLC-DAD was developed to evaluate the quality of Receptaculum Nelumbinis (dried receptacle of Nelumbo nucifera through establishing chromatographic fingerprint and simultaneous determination of five flavonol glycosides, including hyperoside, isoquercitrin, quercetin-3-O-β-d-glucuronide, isorhamnetin-3-O-β-d-galactoside and syringetin-3-O-β-d-glucoside. In quantitative analysis, the five components showed good regression (R > 0.9998 within linear ranges, and their recoveries were in the range of 98.31%–100.32%. In the chromatographic fingerprint, twelve peaks were selected as the characteristic peaks to assess the similarities of different samples collected from different origins in China according to the State Food and Drug Administration (SFDA requirements. Furthermore, hierarchical cluster analysis (HCA was also applied to evaluate the variation of chemical components among different sources of Receptaculum Nelumbinis in China. This study indicated that the combination of quantitative and chromatographic fingerprint analysis can be readily utilized as a quality control method for Receptaculum Nelumbinis and its related traditional Chinese medicinal preparations.

  13. A comparative study on analytical method of total alkaloids from cortex Phellodendri amurens by reversed phase high performance liquid chromatography (RP-HPLC and pressurized capillary electrochromatography (pCEC

    Directory of Open Access Journals (Sweden)

    Bo Yang

    2011-02-01

    Full Text Available A pressurized capillary electrochromatography (pCEC method with post-column detection cell has been developed for the analysis of total alkaloids of cortex Phellodendron amurense Rupr., Rutaceae. The separation of total alkaloids (berberine, palmatine, oatrorrhizine, magnoflorine, phellodendrine, candicine, menisperine was optimized by compositions of the mobile phase, ionic strength of buffers, pH value, and applied voltage. Separation of total alkaloids was achieved within 11 min by using a mobile phase of Na2HPO4-citric acid solution-acetonitrile (pH 4.00; 3 mM (60:40, v/v and applying a voltage of -10 kV. This method showed satisfactory retention times and peak shapes. Meanwhile, a reversed phase high performance liquid chromatography (RP-HPLC has also been established for the separation of total alkaloids extracted from cortex Phellodendri amurens. Baseline separation of total alkaloids was achieved within 25 min by using a mobile phase of acetonitrile-0.1% phosphoric acid with 0.1 g sodium dodecanesulphonate per 100 mL (35:65, v/v. Compared to conventional RP-HPLC, pCEC led to higher column efficiency, less consumption of reagent, and shorter analysis time.

  14. HPLC-ICP-MS联用技术在有机砷形态分析中的应用%Application of HPLC-ICP-MS Coupling Technique in Organoarsenic Species Analysis

    Institute of Scientific and Technical Information of China (English)

    肖亚兵; 阎华; 陈其勇

    2011-01-01

    综述HPLC-ICP-MS联用技术在有机砷形态分析中的应用,并对HPLC与1CP-MS联用接口技术、有机砷形态的HPLC分离(包括离子交换HPLC、离子对HPLC)进行介绍.随着HPLC-ICP-MS联用技术的发展,在有机砷形态分析中应用将更为广泛.

  15. Determination of levodopa in human plasma by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS): application to a bioequivalence study

    OpenAIRE

    Heliana F. Martins; Douglas P. Pinto; Viviane de A. Nascimento; Marlice A. S. Marques; Fábio C. Amendoeira

    2013-01-01

    A sensitive, accurate and simple method using HPLC-MS/MS was developed and validated for levodopa quantitation in human plasma. Analysis was achieved on a pursuit® C18 analytical column (5 µm; 150 x 4.6 mm i.d.) using a mobile phase (methanol and water , 90:10, v/v) containing formic acid 0.5% v/v, after extracting the samples using a simple protein plasma precipitation with perchloric acid. The developed method was validated in accordance with ANVISA guidelines and was successfully applied t...

  16. Determination of levodopa in human plasma by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS: application to a bioequivalence study

    Directory of Open Access Journals (Sweden)

    Heliana F. Martins

    2013-01-01

    Full Text Available A sensitive, accurate and simple method using HPLC-MS/MS was developed and validated for levodopa quantitation in human plasma. Analysis was achieved on a pursuit® C18 analytical column (5 µm; 150 x 4.6 mm i.d. using a mobile phase (methanol and water , 90:10, v/v containing formic acid 0.5% v/v, after extracting the samples using a simple protein plasma precipitation with perchloric acid. The developed method was validated in accordance with ANVISA guidelines and was successfully applied to a bioequivalence study in 60 healthy volunteers demonstrating the feasibility and reliability of the proposed method.

  17. An aromatic hydroxylation assay for hydroxyl radicals utilizing high-performance liquid chromatography (HPLC). Use to investigate the effect of EDTA on the Fenton reaction.

    Science.gov (United States)

    Grootveld, M; Halliwell, B

    1986-01-01

    A highly sensitive HPLC method for the separation of hydroxylation products derived from the attack of hydroxyl radical upon phenol is described. Catechol and hydroquinone are the major hydroxylation products formed, with little resorcinol. The effect of EDTA upon hydroxyl radical generation from an iron (II)-H2O2 system is shown to depend upon the order of addition of chelator and metal ion to the reaction mixture, the ratio [iron salt]/[chelator] and the presence or absence of a phosphate buffer. Reasons for these different effects are discussed. PMID:2849582

  18. Vitamin D analysis in plasma by high performance liquid chromatography (HPLC) with C30 reversed phase column and UV detection - easy and acetonitrile-free

    DEFF Research Database (Denmark)

    Hymøller, Lone; Jensen, Søren Krogh

    2011-01-01

    of animals and humans. Therefore cheap and reliable analytical methods are very much in demand in nutritional and physiological research. After saponification and extraction of plasma or serum samples the current method uses reverse phase high performance liquid chromatography on a C30 column and...

  19. On-line coupling of size exclusion chromatography with mixed-mode liquid chromatography for comprehensive profiling of biopharmaceutical drug product.

    Science.gov (United States)

    He, Yan; Friese, Olga V; Schlittler, Michele R; Wang, Qian; Yang, Xun; Bass, Laura A; Jones, Michael T

    2012-11-01

    A methodology based on on-line coupling of size exclusion chromatography (SEC) with mixed-mode liquid chromatography (LC) has been developed. The method allows for simultaneous measurement of a wide range of components in biopharmaceutical drug products. These components include the active pharmaceutical ingredient (protein) and various kinds of excipients such as cations, anions, nonionic hydrophobic surfactant and hydrophilic sugars. Dual short SEC columns are used to separate small molecule excipients from large protein molecules. The separated protein is quantified using a UV detector at 280 nm. The isolated excipients are switched, online, to the Trinity P1 mixed-mode column for separation, and detected by an evaporative light scattering detector (ELSD). Using a stationary phase with 1.7 μm particles in SEC allows for the use of volatile buffers for both SEC and mix-mode separation. This facilitates the detection of different excipients by ELSD and provides potential for online characterization of the protein with mass spectrometry (MS). The method has been applied to quantitate protein and excipients in different biopharmaceutical drug products including monoclonal antibodies (mAb), antibody drug conjugates (ADC) and vaccines. PMID:22999205

  20. Detection of radiation-induced hydrocarbons in irradiated fish and prawns by means of on-line coupled liquid chromatography-gas chromatography

    International Nuclear Information System (INIS)

    Radiation-induced hydrocarbons were analyzed in a fatty (halibut) and a lean fish (cod) as well as in a prawn species by on-line coupled liquid chromatography (LC) -gas chromatography (GC) combined with mass spectrometry. In irradiated halibut which is known to contain mainly saturated and monounsaturated fatty acids, all expected radiolytic alkanes, alkenes, and alkadienes could be detected. The yields of the C(n-1) and C(n-2:1) hydrocarbons were comparable to those found in irradiated lipids of terrestrial animals and plants. However, in cod and prawns which contain high levels of polyunsaturated fatty acids (PUFA), the C(n-1) hydrocarbons were found in concentrations which were up to 10 times higher whereas the C(n-2:1) products were again comparable to those of terrestrial animals and plants. The identification of radiation-induced hydrocarbons in fish lipids was achieved by transfer of the hydrocarbons from the LC column to the gas chromatographic column in fractions differing in their degree of unsaturation. For the first time, radiation-induced hydrocarbons with more than four double bonds generated from polyunsaturated fatty acids (20:4 omega 6 and 20:5 omega 3) could be identified

  1. [Rapid determination of pesticide multiresidues in vegetables and fruits by accelerated solvent extraction coupled with online gel permeation chromatography-gas chromatography-mass spectrometry].

    Science.gov (United States)

    Ouyang, Yunfu; Tang, Hongbing; Wu, Ying; Li, Guiying

    2012-07-01

    A novel method was developed for the rapid determination of 22 representative pesticide residues in vegetables and fruits based on accelerated solvent extraction (ASE) coupled with online gel permeation chromatography-gas chromatography-mass spectrometry (GPC-GC-MS). The sample was extracted by accelerated solvent extraction with dichloromethane-acetone (1:1, v/v) and purified with a carbon/NH2 column, evaporated to dryness by nitrogen, then dissolved in cyclohexane-acetone (7:3, v/v), and finally identified and quantified by GPC-GC-MS system in selected ion monitoring (SIM) mode. The results showed that the linearities of the 22 pesticides were good in their linear ranges. The limits of detection (S/N = 3) were 0.3-1.8 microg/kg. The limits of quantification (S/N = 10) ranged from 1-6 microg/kg. The recoveries for all at three spiked levels in Chinese cabbages and apples ranged from 70.5% to 107.5% with the relative standard deviations (RSDs) of 2.1%-8.7%. The proposed method is accurate, sensitive and highly efficient in the extraction, and can be used for the quick determination of the pesticide multiresidues in vegetables and fruits. PMID:23189658

  2. Headspace-solid phase microextraction coupled to gas chromatography-combustion-isotope ratio mass spectrometer and to enantioselective gas chromatography for strawberry flavoured food quality control.

    Science.gov (United States)

    Schipilliti, Luisa; Dugo, Paola; Bonaccorsi, Ivana; Mondello, Luigi

    2011-10-21

    Authenticity assessment of flavoured strawberry foods was performed using headspace-solid phase microextraction (HS-SPME) coupled to gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS). An authenticity range was achieved, investigating on the carbon isotope ratio of numerous selected aroma active volatile components (methyl butanoate, ethyl butanoate, hex-(2E)-enal, methyl hexanoate, buthyl butanoate, ethyl hexanoate, hexyl acetate, linalool, hexyl butanoate, octyl isovalerate, γ-decalactone and octyl hexanoate) of organic Italian fresh strawberries. To the author's knowledge, this is the first time that all these components were investigated simultaneously by GC-C-IRMS on the same sample. The results were compared, when applicable, with those obtained by analyzing the HS-SPME extracts of commercial flavoured food matrices. In addition, one Kenyan pineapple and one fresh Italian peach were analyzed to determine the δ(13)C(VPDB) of the volatile components common to strawberry. The δ(13)C(VPDB) values are allowed to differentiate between different biogenetic pathways (C(3) and CAM plants) and more interestingly between plants of the same CO(2) fixation group (C(3) plants). Additional analyses were performed on all the samples by means of Enantioselective Gas Chromatography (Es-GC), measuring the enantiomeric distribution of linalool and γ-decalactone. It was found that GC-C-IRMS and Es-GC measurements were in agreement to detect the presence of non-natural strawberry aromas in the food matrices studied. PMID:21872872

  3. Characterization of Flavonoids and Naphthopyranones in Methanol Extracts of Paepalanthus chiquitensis Herzog by HPLC-ESI-IT-MSn and Their Mutagenic Activity

    Directory of Open Access Journals (Sweden)

    Wagner Vilegas

    2012-12-01

    Full Text Available A HPLC-ESI-IT-MSn method, based on high-performance liquid chromatography coupled to electrospray negative ionization multistage ion trap mass spectrometry, was developed for rapid identification of 24 flavonoid and naphthopyranone compounds. The methanol extracts of the capitulae and scapes of P. chiquitensis exhibited mutagenic activity in the Salmonella/microsome assay, against strain TA97a.

  4. Characterization of Flavonoids and Naphthopyranones in Methanol Extracts of Paepalanthus chiquitensis Herzog by HPLC-ESI-IT-MSn and Their Mutagenic Activity

    OpenAIRE

    Wagner Vilegas; Lourdes Campaner dos Santos; Paulo Takeo Sano; Samara Fernandes de Souza; Eliana Aparecida Varanda; Paula Karina Boldrin; Fabiana Volpe Zanutto

    2012-01-01

    A HPLC-ESI-IT-MSn method, based on high-performance liquid chromatography coupled to electrospray negative ionization multistage ion trap mass spectrometry, was developed for rapid identification of 24 flavonoid and naphthopyranone compounds. The methanol extracts of the capitulae and scapes of P. chiquitensis exhibited mutagenic activity in the Salmonella/microsome assay, against strain TA97a.

  5. Rapid method for simultaneous determination of flavonoid, saponins and polyacetylenes in folium ginseng and radix ginseng by pressurized liquid extraction and high-performance liquid chromatography coupled with diode array detection and mass spectrometry.

    Science.gov (United States)

    Qian, Z M; Lu, J; Gao, Q P; Li, S P

    2009-05-01

    A rapid pressurized liquid extraction (PLE) and high-performance liquid chromatography coupled with diode array detection and mass spectrometry (HPLC-DAD-MS) method for the simultaneous determination of one flavonoid (panasenoside), nine saponins (ginsenoside Rg1, Re, Rf, Rg2, Rb1, Rc, Rb2, Rb3 and Rd) and two polyacetylenes (panaxydol and panaxynol) in folium ginseng and radix ginseng was developed. A Prevail C(18) rocket column (33 mm x 7 mm, 3.0 microm) and gradient elution were used during the analysis. Flavonoid was quantified at 355 nm, and saponins and polyacetylenes were determined at 203 nm. The chromatographic peaks of 12 investigated compounds in samples were unambiguously identified by compared their UV spectra and/or MS data with the related reference compounds. All calibration curves showed good linearity (r>0.999) within the test ranges. The intra- and inter-day variations for 12 analytes were less than 1.17% and 2.17%, respectively. The developed method was successfully applied to determine the investigated compounds in 10 samples of radix ginseng and folium ginseng, respectively. The result showed that PLE combined with rocket column HPLC analysis could provide a rapid method for analysis of compounds in traditional Chinese medicines (TCMs), which is helpful to comprehensive evaluation of quality of radix ginseng and folium ginseng. PMID:19272605

  6. Dispersive liquid-liquid microextraction coupled to liquid chromatography for thiamine determination in foods.

    Science.gov (United States)

    Viñas, Pilar; López-García, Ignacio; Bravo-Bravo, María; Briceño, Marisol; Hernández-Córdoba, Manuel

    2012-05-01

    A miniaturized dispersive liquid-liquid microextraction (DLLME) procedure coupled to liquid chromatography (LC) with fluorimetric detection was evaluated for the preconcentration and determination of thiamine (vitamin B(1)). Derivatization was carried out by chemical oxidation of thiamine with 5 × 10(-5) M ferricyanide at pH 13 to form fluorescent thiochrome. For DLLME, 0.5 mL of acetonitrile (dispersing solvent) containing 90 μL of tetrachloroethane (extraction solvent) was rapidly injected into 10 mL of sample solution containing the derivatized thiochrome and 24% (w/v) sodium chloride, thereby forming a cloudy solution. Phase separation was carried out by centrifugation, and a volume of 20 μL of the sedimented phase was submitted to LC. The mobile phase was a mixture of a 90% (v/v) 10 mM KH(2)PO(4) (pH 7) solution and 10% (v/v) acetonitrile at 1 mL min(-1). An amide-based stationary phase involving a ligand with amide groups and the endcapping of trimethylsilyl was used. Specificity, linearity, precision, recovery, and sensitivity were satisfactory. Calibration graph was carried out by the standard additions method and was linear between 1 and 10 ng mL(-1). The detection limit was 0.09 ng mL(-1). The selectivity of the method was judged from the absence of interfering peaks at the thiamine elution time for blank chromatograms of unspiked samples. A relative standard deviation of 3.2% was obtained for a standard solution containing thiamine at 5 ng mL(-1). The esters thiamine monophosphate and thiamine pyrophosphate can also be determined by submitting the sample to successive acid and enzymatic treatments. The method was applied to the determination of thiamine in different foods such as beer, brewer's yeast, honey, and baby foods including infant formulas, fermented milk, cereals, and purees. For the analysis of solid samples, a previous extraction step was applied based on an acid hydrolysis with trichloroacetic acid. The reliability of the procedure was

  7. Strategies for differentiation of isobaric flavonoids using liquid chromatography coupled to electrospray ionization mass spectrometry

    OpenAIRE

    Fridén, Mikael E; Sjöberg, Per J. R.

    2014-01-01

    Flavonoids are a class of secondary plant metabolites existing in great variety in nature. Due to this variety, identification can be difficult, especially as overlapping compounds in both chromatographic separations and mass spectrometric detection are common. Methods for distinguishing isobaric flavonoids using MS2 and MS3 have been developed. Chromatographic separation of various plant extracts was done with RP-HPLC and detected with positive ESI-MS operated in information-dependent acquis...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-04-15

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

  9. Analytical developments for the determination of monomethylmercury complexes with low molecular mass thiols by reverse phase liquid chromatography hyphenated to inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Bouchet, Sylvain; Björn, Erik

    2014-04-25

    The behavior of monomethylmercury (MMHg) is markedly influenced by its distribution among complexes with low molecular mass (LMM) thiols but analytical methodologies dedicated to measure such complexes are very scarce up to date. In this work, we selected 15 LMM thiols often encountered in living organisms and/or in the environment and evaluated the separation of the 15 corresponding MMHg-thiol complexes by various high performance liquid chromatography (HPLC) columns. Two C18 (Phenomenex Synergi Hydro-RP and LunaC18(2)), two phenyl (Inertsil Ph 3 and 5μm) and one mixed-mode (Restek Ultra IBD) stationary phases were tested for their retention and resolution capacities of the various complexes. The objective was to find simple separation conditions with low organic contents in the mobile phase to provide optimal conditions for detection by inductively coupled plasma mass spectrometry (ICPMS). The 15 complexes were synthesized in solution and characterized by electrospray ionization-mass spectrometry (ESI-MS). The C18 columns tested were either not resolutive enough or too retentive. The 3μm phenyl stationary phase was able to resolve 10 out of the 15 complexes in less than 25min, under isocratic conditions. The mixed-mode column was especially effective at separating the most hydrophilic complexes (6 complexes out of the 15), corresponding to the main LMM thiols found in living organisms. The detection limits (DLs) for these two columns were in the low nanomolar range and overall slightly better for the phenyl column. The possibilities offered by such methodology were exemplified by monitoring the time-course concentrations of four MMHg-thiol complexes within a phytoplankton incubation containing MMHg in the presence of an excess of four added thiols. PMID:24657146

  10. Determination of monoamine neurotransmitters and their metabolites in a mouse brain microdialysate by coupling high-performance liquid chromatography with gold nanoparticle-initiated chemiluminescence

    Energy Technology Data Exchange (ETDEWEB)

    Li Na; Guo Jizhao; Liu Bo; Yu Yuqi [Department of Chemistry, University of Science and Technology of China (USTC), JinZhai Road No: 96, 230026 Hefei, Anhui (China); Cui Hua, E-mail: hcui@ustc.edu.cn [Department of Chemistry, University of Science and Technology of China (USTC), JinZhai Road No: 96, 230026 Hefei, Anhui (China); Mao Lanqun; Lin Yuqing [Beijing National Laboratory for Molecular Sciences, Institute of Chemistry, Chinese Academy of Sciences (CAS), 100080 Beijing (China)

    2009-07-10

    Our previous work showed that gold nanoparticles could trigger chemiluminescence (CL) between luminol and AgNO{sub 3}. In the present work, the effect of some biologically important reductive compounds, including monoamine neurotransmitters and their metabolites, reductive amino acids, ascorbic acid, uric acid, and glutathione, on the novel CL reaction were investigated for analytical purpose. It was found that all of them could inhibit the CL from the luminol-AgNO{sub 3}-Au colloid system. Among them, monoamine neurotransmitters and their metabolites exhibited strong inhibition effect. Taking dopamine as a model compound, the CL mechanism was studied by measuring absorption spectra during the CL reaction and the reaction kinetics via stopped-flow technique. The CL inhibition mechanism is proposed to be due to that these tested compounds competed with luminol for AgNO{sub 3} to inhibit the formation of luminol radicals and to accelerate deposition of Ag atoms on surface of gold nanoparticles, leading to a decrease in CL intensity. Based on the inhibited CL, a novel method for simultaneous determination of monoamine neurotransmitters and their metabolites was developed by coupling high-performance liquid chromatography with this CL reaction. The new method was successfully applied to determine the compounds in a mouse brain microdialysate. Compared with the reported HPLC-CL methods, the proposed method is simple, fast, and could determine more analytes. Moreover, the limits of linear ranges for NE, E, and DA using the proposed method were one order of magnitude lower than the luminol system without gold nanoparticles.

  11. Development and validation of a hydrophilic interaction chromatography method coupled with a charged aerosol detector for quantitative analysis of nonchromophoric α-hydroxyamines, organic impurities of metoprolol.

    Science.gov (United States)

    Xu, Qun; Tan, Shane; Petrova, Katya

    2016-01-25

    The European Pharmacopeia (EP) metoprolol impurities M and N are polar, nonchromophoric α-hydroxyamines, which are poorly retained in a conventional reversed-phase chromatographic system and are invisible for UV detection. Impurities M and N are currently analyzed by TLC methods in the EP as specified impurities and in the United States Pharmacopeia-National Formulary (USP-NF) as unspecified impurities. In order to modernize the USP monographs of metoprolol drug substances and related drug products, a hydrophilic interaction chromatography (HILIC) method coupled with a charged aerosol detector (CAD) was explored for the analysis of the two impurities. A comprehensive column screening that covers a variety of HILIC stationary phases (underivatized silica, amide, diol, amino, zwitterionic, polysuccinimide, cyclodextrin, and mixed-mode) and optimization of HPLC conditions led to the identification of a Halo Penta HILIC column (4.6 × 150 mm, 5 μm) and a mobile phase comprising 85% acetonitrile and 15% ammonium formate buffer (100 mM, pH 3.2). Efficient separations of metoprolol, succinic acid, and EP metoprolol impurities M and N were achieved within a short time frame (<8 min). The HILIC-CAD method was subsequently validated per USP validation guidelines with respect to specificity, robustness, linearity, accuracy, and precision, and could be incorporated into the current USP-NF monographs to replace the outdated TLC methods. Furthermore, the developed method was successfully applied to determine organic impurities in metoprolol drug substance (metoprolol succinate) and drug products (metoprolol tartrate injection and metoprolol succinate extended release tablets). PMID:26580821

  12. Investigation of metallodrug-protein interactions by size-exclusion chromatography coupled with inductively coupled plasma mass spectrometry (ICP-MS)

    Energy Technology Data Exchange (ETDEWEB)

    Szpunar, J.; Makarov, A. [CNRS, EP132, Helioparc 2, av. Pr. Angot, 64000 Pau (France); Pieper, T.; Keppler, B.K. [Institute of Inorganic Chemistry, University of Vienna, Waehringerstr. 42, A-1090 Vienna (Austria); Lobinski, R. [CNRS, EP132, Helioparc 2, av. Pr. Angot, 64000 Pau (France)

    1999-04-22

    The coupling of size-exclusion HPLC with ICP-MS was developed for the studies of the kinetics of metallodrug binding to human serum proteins. Two platinum- and three ruthenium-based drugs were investigated. Various SEC columns (of different lengths and with different packings) were compared for the separation of the protein-bound and unbound fractions of a metallodrug prior to on-line detection of the metal (Ru or Pt). The approach developed offers considerable advantages over the methods based on ultrafiltration followed by the off-line metal determination in terms of speed, simplicity, precision and selectivity regarding the molecular weight of the complexes involved. (Copyright (c) 1999 Elsevier Science B.V., Amsterdam. All rights reserved.)

  13. Investigation of metallodrug-protein interactions by size-exclusion chromatography coupled with inductively coupled plasma mass spectrometry (ICP-MS)

    International Nuclear Information System (INIS)

    The coupling of size-exclusion HPLC with ICP-MS was developed for the studies of the kinetics of metallodrug binding to human serum proteins. Two platinum- and three ruthenium-based drugs were investigated. Various SEC columns (of different lengths and with different packings) were compared for the separation of the protein-bound and unbound fractions of a metallodrug prior to on-line detection of the metal (Ru or Pt). The approach developed offers considerable advantages over the methods based on ultrafiltration followed by the off-line metal determination in terms of speed, simplicity, precision and selectivity regarding the molecular weight of the complexes involved. (Copyright (c) 1999 Elsevier Science B.V., Amsterdam. All rights reserved.)

  14. Plasma amino-acid determinations by reversed-phase HPLC: Improvement of the orthophthalaldehyde method and comparison with ion exchange chromatography

    OpenAIRE

    Ziegler, Frédéric; Le Boucher, Jacques; Coudray-Lucas, Colette; Cynober, Luc

    1992-01-01

    Reversed-phase high performance liquid chromatographic (RPHPLC) determination of amino-acids with on-line pre-column ortho-phthalaldehyde (OPA) derivatization and fluorescence detection is rapid and sensitive. However, high-performance ionexchange chromatography (HP-IEC) with post-column ninhydrine reaction is the most widely used amino-acid (AA) assay for biological samples. These two methods have been compared for the determination of individual plasma AA concentrations. An excellent correl...

  15. Optimization of the SPME parameters and its online coupling with HPLC for the analysis of tricyclic antidepressants in plasma samples.

    Science.gov (United States)

    Alves, Claudete; Fernandes, Christian; Dos Santos Neto, Alvaro José; Rodrigues, José Carlos; Costa Queiroz, Maria Eugênia; Lanças, Fernando Mauro

    2006-07-01

    Solid-phase microextraction (SPME)-liquid chromatography (LC) is used to analyze tricyclic antidepressant drugs desipramine, imipramine, nortriptyline, amitriptyline, and clomipramine (internal standard) in plasma samples. Extraction conditions are optimized using a 2(3) factorial design plus a central point to evaluate the influence of the time, temperature, and matrix pH. A Polydimethylsiloxane-divinylbenzene (60-mum film thickness) fiber is selected after the assessment of different types of coating. The chromatographic separation is realized using a C(18) column (150 x 4.6 mm, 5-microm particles), ammonium acetate buffer (0.05 mol/L, pH 5.50)-acetonitrile (55:45 v/v) with 0.1% of triethylamine as mobile phase and UV-vis detection at 214 nm. Among the factorial design conditions evaluated, the best results are obtained at a pH 11.0, temperature of 30 degrees C, and extraction time of 45 min. The proposed method, using a lab-made SPME-LC interface, allowed the determination of tricyclic antidepressants in in plasma at therapeutic concentration levels. PMID:16884589

  16. Stability considerations of aspartame in the direct analysis of artificial sweeteners in water samples using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).

    Science.gov (United States)

    Berset, Jean-Daniel; Ochsenbein, Nicole

    2012-07-01

    A HPLC-MS/MS method is presented for the simultaneous determination of frequently used artificial sweeteners (ASs) and the main metabolite of aspartame (ASP), diketopiperazine (DKP), in environmental water samples using the direct-injection (DI) technique, thereby achieving limits of quantification (LOQ) of 10 ng L(-1). For a reliable quantification of ASP pH should be adjusted to 4.3 to prevent formation of the metabolite. Acesulfame (ACE), saccharin (SAC), cyclamate (CYC) and sucralose (SUC) were ubiquitously found in water samples. Highest concentrations up to 61 μg L(-1) of ACE were found in wastewater effluents, followed by surface water with concentrations up to 7 μg L(-1), lakes up to 600 ng L(-1) and groundwater and tap water up to 70 ng L(-1). The metabolite DKP was only detected in wastewater up to 200 ng L(-1) and at low detection frequencies. PMID:22503463

  17. Methyl mercury in nail clippings in relation to fish consumption analysis with gas chromatography coupled to inductively coupled plasma mass spectrometry: a first orientation.

    Science.gov (United States)

    Krystek, Petra; Favaro, Paulo; Bode, Peter; Ritsema, Rob

    2012-08-15

    For the identification of human exposure to one of the most toxic compounds, which is methyl mercury (MeHg(+)), fingernail clippings were selected as the matrix of interest. Within this pilot study, six samples from different origins and from people with different food consumption patterns were chosen. Species-analysis of MeHg(+) was performed according to the following procedure: dissolution of the sample material in tetramethylammonium hydroxide (TMAH), derivatisation of MeHg(+) with sodium tetraethylborate (NaBEt(4)), extraction into iso-octane and measurement with gas chromatography hyphenated to inductively coupled plasma mass spectrometry (GC-ICPMS) for the quantification MeHg(+). PMID:22841050

  18. Zirconium (IV)-based metal organic framework (UIO-67) as efficient sorbent in dispersive solid phase extraction of plant growth regulator from fruits coupled with HPLC fluorescence detection.

    Science.gov (United States)

    Liu, Lijie; Xia, Lian; Wu, Chuanxiang; Qu, Fengli; Li, Guoliang; Sun, Zhiwei; You, Jinmao

    2016-07-01

    A stable zirconium (Ⅳ)-based metal organic frameworks (UIO-67) material possessing good chemical, thermal and water stability was synthesized and applied as a sorbent for the dispersive solid phase extraction (DSPE) of 8 plant growth regulators (PGRs) in fruit samples. Fluorescence labeling combined with high performance liquid chromatography fluorescence detection (HPLC-FLD), was used to quantify the target analytes. Characterization of the UIO-67 material was performed by X-ray diffraction(XRD) and scanning electron microscopy (SEM). The experimental parameters, such as amount of UIO-67, type and volume of eluting solvent, adsorption and desorption time, were optimized. Under the optimized conditions, good linearity was observed in the range of 10-1000 pmol/mL with R(2)>0.9989. The limits of detection and limits of quantification were in the range of 0.21-0.57ng/mL and 0.81-1.91ng/mL, respectively. The intra-day and inter-day precisions (based on the relative standard deviation, n=3) of the PGR derivatives were under 3.1% and 5.3% respectively and the accuracies of the method for the PGRs were in the range from 89.3% to 102.3%. The developed method was successfully applied to analyze PGRs residues in fruit samples. The proposed method is proved to be simple, environment-friendly and inexpensive and it is feasible to directly use UIO-67 as sorbent to extract targets by varying conditions. PMID:27154644

  19. Optimizing TiO2-based phosphopeptide enrichment for automated multidimensional liquid chromatography coupled to tandem mass spectrometry

    OpenAIRE

    Cantin, Greg T.; Shock, Teresa R.; Park, Sung Kyu; Madhani, Hiten D.; Yates, John R.

    2007-01-01

    An automated online multidimensional liquid chromatography system coupled to ESI-based tandem mass spectrometry was used to assess the effectiveness of TiO2 in the enrichment of phosphopeptides from tryptic digests of protein mixtures. By monitoring the enrichment of phosphopeptides, an optimized set of loading, wash, and elution conditions were realized for TiO2. A comparison of TiO2 with other resins used for phosphopeptide enrichment, Fe(III)-IMAC and ZrO2, was also carried out using trypt...

  20. Determination of selenite and selenate in human urine by ion chromatography and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Gammelgaard, Bente; Jons, O.

    2000-01-01

    The selenium species selenite, selenate and selenomethionine were separated in aqueous solution by ion chromatography. The separation was performed on an IonPac AG11 in series with an AS11 anion exchange column by elution with 25 mM sodium hydroxide in 2% methanol. The Se-78 and Se-82 isotopes were...... monitored in the inductively coupled plasma mass spectrometry (ICP-MS) detector. When the chromatographic system was applied to analysis of urine samples diluted 1 + 1, the selenomethionine signal appeared in the front together with other unresolved selenium species, while the selenite and selenate signals...

  1. Rapid determination of polysaccharides in BianTi Soft extract by spectrophotometry coupled with gas chromatography-mass spectrometry

    OpenAIRE

    Minxia Zheng; Jie Shen; Kai Yang; Songxiang Qian; Sujuan Feng

    2010-01-01

    A simple approach for the rapid determination of polysaccharides in BianTi Soft Extract using spectrophotometry coupled with gas chromatography-mass spectrometry (GC-MS) was developed. The mixed standard solution composed of D-glucose, D-mannose, galactose and D-xylose in different proportions (1.00: 1.01: 0.12: 0.05) was prepared according to the monosaccharide composition analysis of the polysaccharides by GC-MS. The determination of polysaccharides by UV-Vis spectrophotometer was performed...

  2. Qualitative and quantitative analysis of chemical constituents of Centipeda minima by HPLC-QTOF-MS & HPLC-DAD.

    Science.gov (United States)

    Chan, Chi-On; Jin, Deng-Ping; Dong, Nai-Ping; Chen, Si-Bao; Mok, Daniel Kam Wah

    2016-06-01

    A high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC-QTOF-MS) method in both positive and negative ion modes was established to investigate the major constituents in the ethanolic extract of Centipeda minima (EBSC). Twelve common components including flavones and their glycosides, phenolic and polyphenolic acids, and sesquiterpene lactone were identified in ten batches of samples based on comparison with the retention time and accurate mass of external standards (mass accuracy within 3ppm) or the fragmentation patterns of tandem MS. Meanwhile, a simple, accurate and reliable HPLC-DAD method was also developed to determine the content of 10 chemical markers simultaneously. Results obtained from method validations including linearity, accuracy and precision showed that this new method is reliable and robust. Isochlorogenic acid A and brevilin A were found to be the most abundant in the ethanol extract of EBSC and could be served as markers for quality control of EBSC. PMID:27131150

  3. Inventory of metal complexes circulating in plant fluids: a reliable method based on HPLC coupled with dual elemental and high-resolution molecular mass spectrometric detection.

    Science.gov (United States)

    Flis, Paulina; Ouerdane, Laurent; Grillet, Louis; Curie, Catherine; Mari, Stéphane; Lobinski, Ryszard

    2016-08-01

    Description of metal species in plant fluids such as xylem, phloem or related saps remains a complex challenge usually addressed either by liquid chromatography-mass spectrometry, X-ray analysis or computational prediction. To date, none of these techniques has achieved a complete and true picture of metal-containing species in plant fluids, especially for the least concentrated complexes. Here, we present a generic analytical methodology for a large-scale (> 10 metals, > 50 metal complexes) detection, identification and semiquantitative determination of metal complexes in the xylem and embryo sac liquid of the green pea, Pisum sativum. The procedure is based on direct injection using hydrophilic interaction chromatography with dual detection by elemental (inductively coupled plasma mass spectrometry) and molecular (high-resolution electrospray mass spectrometry) mass spectrometric detection. Numerous and novel complexes of iron(II), iron(III), copper(II), zinc, manganese, cobalt(II), cobalt(III), magnesium, calcium, nickel and molybdenum(IV) with several ligands including nicotianamine, citrate, malate, histidine, glutamine, aspartic acid, asparagine, phenylalanine and others are observed in pea fluids and discussed. This methodology provides a large inventory of various types of metal complexes, which is a significant asset for future biochemical and genetic studies into metal transport/homeostasis. PMID:27111838

  4. 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. PMID:26986639

  5. Application of hollow fiber-supported liquid-phase microextraction coupled with HPLC for the determination of guaifenesin enantiomer-protein binding.

    Science.gov (United States)

    Hatami, Mehdi; Farhadi, Khalil

    2012-07-01

    A hollow fiber liquid-phase microextraction technique coupled with high-performance liquid chromatography with fluorescence detection was employed for determination and evaluation of the binding characteristics of drugs to bovine serum albumin (BSA). Enantiomers of guaifenesin (an expectorant drug) were investigated as a model system. After optimization of some influencing parameters on microextraction, the proposed method was used for calculation of the target drug distribution coefficient between n-octanol and the buffer solution as well as study of drug-BSA binding in physiological conditions. The developed method shows a new, improved and simple procedure for determination of free drug concentration in biological fluids and the extent of drug-protein binding. PMID:22102436

  6. Strategies for differentiation of isobaric flavonoids using liquid chromatography coupled to electrospray ionization mass spectrometry.

    Science.gov (United States)

    Fridén, Mikael E; Sjöberg, Per J R

    2014-07-01

    Flavonoids are a class of secondary plant metabolites existing in great variety in nature. Due to this variety, identification can be difficult, especially as overlapping compounds in both chromatographic separations and mass spectrometric detection are common. Methods for distinguishing isobaric flavonoids using MS(2) and MS(3) have been developed. Chromatographic separation of various plant extracts was done with RP-HPLC and detected with positive ESI-MS operated in information-dependent acquisition (IDA) mode. Two methods for the determination of flavonoid identity and substitution pattern, both featuring IDA criteria, were used together with the HPLC equipment. A third method where the collision energy was ramped utilized direct infusion. With the developed strategies, it is possible to differentiate between many isobaric flavonoids. Various classes of flavonoids were found in all of the plant extracts, in the red onion extract 45 components were detected and for 29 of them the aglycone was characterized, while the substituents were tentatively identified for 31 of them. For the strawberry extract, those numbers were 66, 30 and 60, and for the cherry extract 99, 56 and 71. The great variety of flavonoids, several of them isobaric, found in each of the extracts highlights the need for reliable methods for flavonoid characterization. Methods capable of differentiating between most of the isobars analyzed have been developed. PMID:25044850

  7. Novel applications of high performance ion chromatography-inductively coupled plasma mass spectrometry (HPIC-ICP-MS)

    CERN Document Server

    Hann, S

    2001-01-01

    This work demonstrates the development of highly sensitive and selective analytical methods, which make use of the hyphenation of high performance ion chromatography (HPIC) to inductively coupled plasma sector field mass spectrometry (ICP-SFMS). On-line coupling a chromatographic separation method with an elemental detection method provides two advantages: (1) the components of a possibly interfering matrix can be separated allowing accurate and precise ultra trace analysis of the element of interest and (2) elemental species of an element can be separated and quantified. In this work, matrix separation methods for interference free determination of 232Th, 234U, 235U and 238U in geological matrices were developed and employed. Furthermore HPIC-ICP-SFMS was applied for ultra trace analysis of Pd in environmental and geological matrices. The usefulness of HPIC-ICP-SFMS for speciation studies was demonstrated by investigating the interaction of an anti-cancer drug (cisplatin) with guanosine monophosphates.

  8. Novel applications of high performance ion chromatography-inductively coupled plasma mass spectrometry (HPIC-ICP-MS)

    International Nuclear Information System (INIS)

    This work demonstrates the development of highly sensitive and selective analytical methods, which make use of the hyphenation of high performance ion chromatography (HPIC) to inductively coupled plasma sector field mass spectrometry (ICP-SFMS). On-line coupling a chromatographic separation method with an elemental detection method provides two advantages: (1) the components of a possibly interfering matrix can be separated allowing accurate and precise ultra trace analysis of the element of interest and (2) elemental species of an element can be separated and quantified. In this work, matrix separation methods for interference free determination of 232Th, 234U, 235U and 238U in geological matrices were developed and employed. Furthermore HPIC-ICP-SFMS was applied for ultra trace analysis of Pd in environmental and geological matrices. The usefulness of HPIC-ICP-SFMS for speciation studies was demonstrated by investigating the interaction of an anti-cancer drug (cisplatin) with guanosine monophosphates. (author)

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

    Science.gov (United States)

    Zhu, Mingzhi; Dong, Xia; Guo, Mingquan

    2015-01-01

    Duchesnea indica (D. indica) is an important traditional Chinese medicine, and has long been clinically used to treat cancer in Asian countries. It has been described previously as a rich source of phenolic compounds with a broad array of diversified structures, which are the major active ingredients. However, an accurate and complete phenolic profiling has not been determined yet. In the present work, the total phenolic compounds in crude extracts from D. indica were enriched and fractionated over a macroporous resin column, then identified by HPLC-ESI-MS/MS and ESI-IT-MS (ion trap MS). A total of 27 phenolic compounds were identified in D. indica, of which 21 compounds were identified for the first time. These 27 phenolic compounds encompassing four phenolic groups, including ellagitannins, ellagic acid and ellagic acid glycosides, hydroxybenzoic acid and hydroxycinnamic acid derivatives, and flavonols, were then successfully quantified using peak areas against those of the corresponding standards with good linearity (R² > 0.998) in the range of the tested concentrations. As a result, the contents of individual phenolic compounds varied from 6.69 mg per 100 g dry weight (DW) for ellagic acid to 71.36 mg per 100 g DW for brevifolin carboxylate. Not only did this study provide the first phenolic profiling of D. indica, but both the qualitative identification and the subsequent quantitative analysis of 27 phenolic compounds from D. indica should provide a good basis for future exploration of this valuable medicinal plant. PMID:26694333

  10. High performance liquid chromatography (HPLC) evaluation of carotenoids in irradiated guavas; Avaliacao por cromatografia liquida de alta eficiencia (CLAE) de carotenoides em goiabas irradiadas

    Energy Technology Data Exchange (ETDEWEB)

    Lima, Keila S. Cople; Vital, Helio C. [Centro Tecnologico do Exercito (CTEx), Rio de Janeiro, RJ (Brazil). Secao de Defesa Nuclear]. E-mail: keilacople@ig.com.br; Lima, Antonio L. Santos; Pereira, Maria Helena G. [Centro Tecnologico do Exercito (CTEx), Rio de Janeiro, RJ (Brazil). Secao de Quimica]. E-mail: stolima@ipd.eb.br; Godoy, Ronoel L. Oliveira; Fonseca, Marcos J.O. [Embrapa Agroindustria de Alimentos, Rio de Janeiro, RJ (Brazil)]. E-mail: ronoel@ctaa.embrapa.br

    2005-07-01

    The use of ionizing gamma irradiation has shown very effective as an auxiliary technology for the decrease of post-harvest waste, grains disinfestation, pathogenic microorganisms control, increase in shelf life for meats, fruits, vegetables and bulbs and tubercles sprouts inhibition, maintaining nutritional quality. The carotenoids are pigments widely found in fruits and vegetables and are beneficial to human being health. This work was undergone using the irradiator with cesium source at the Army Technological Center, Brazil, with maximum dose rate of 2 kGy per hour. The objective is to evaluate the low gamma radiation doses (0.5, 1.0 and 1.5 kGy) influence in the total carotenoid and content lycopene in guavas CV Pal uma, with excellent weight classification. The total carotenoid content was extracted from the guava with acetone and moved to petroleum ether and determined by spectrophotometer at 450 nm. The determination of lycopene was accomplished by HPLC. The results showed that, in spite of lycopene loss with irradiation, the best dose was 0.5 kGy. (author)

  11. Determination of biogenic amines in traditional Chinese fermented foods by reversed-phase high-performance liquid chromatography (RP-HPLC).

    Science.gov (United States)

    Gong, Xiao; Wang, Xiaoxi; Qi, Ningli; Li, Jihua; Lin, Lijing; Han, Zhiping

    2014-01-01

    A survey of biogenic amine content of traditional Chinese fermented foods (douchi, sufu, fermented sausage, yulu, and shrimp paste) was carried out. Eight major biogenic amines including putrescine, cadaverine, histamine, phenylethylamine, tyramine, spermine, spermidine and tryptamine were separated by reversed-phase HPLC-DAD on Inertsil ODS-SP column after pre-column derivatisation with dansyl chloride. The results showed that spermine (1.65-3.96 mg 100 g(-1)), putrescine (0.20-10.89 mg 100 g(-1)), cadaverine (3.60-12.14 mg 100 g(-1)), and histamine (0.57-20.24 mg 100 g(-1)) were the most represented amines. All amines were detected in yulu, while sufu showed a much higher content of most amines. Shrimp paste showed the lowest level of total biogenic amines. Moreover, the composition and content of eight biogenic amines in the selected samples varied among different food types, origins and batches. Although the average content for each amine is within the range that may elicit direct adverse reactions, consumers should be aware of the potential synergistic effect among different amines and limit their consumption at each meal. PMID:24844287

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

    Directory of Open Access Journals (Sweden)

    Mingzhi Zhu

    2015-12-01

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

  13. Determination of cyclopiazonic acid in white mould cheese by liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) using a novel internal standard.

    Science.gov (United States)

    Ansari, Parisa; Häubl, Georg

    2016-11-15

    For the determination of cyclopiazonic acid (CPA) in food and feed samples a simple and accurate LC-MS/MS method, which does not require extensive sample clean-up steps, was developed and validated. A fully carbon-13-labelled internal standard was used to compensate for matrix effects. Briefly, the samples were extracted with 1% formic acid in acetonitrile and directly analysed with HPLC-MS/MS. The following MS/MS transitions were used: m/z 337/196 and 337/182 for cyclopiazonic acid; m/z 357/210 and 357/191 for (13)C20-cyclopiazonic acid. Applying this optimised method, LODs down to 0.2μgkg(-1) and LOQs down to 0.5μgkg(-1) were determined in the validated matrices. The focus of this study was testing different types of white mould cheese but other complex samples could also be analyzed successfully with this method. It was interesting to find out, that in some commercially available white mould cheese, high concentrations of CPA (up to 3700μgkg(-1)) could be found. PMID:27283720

  14. Extraction, Separation, and Identification of Phenolic Compounds in Virgin Olive Oil by HPLC-DAD and HPLC-MS

    Directory of Open Access Journals (Sweden)

    Maria Tasioula-Margari

    2015-08-01

    Full Text Available The aim of this study was to evaluate the recovery of individual phenolic compounds extracted from virgin olive oil (VOO, from different Greek olive varieties. Sufficient recoveries (90% of all individual phenolic compounds were obtained using methanol as an extraction solvent, acetonitrile for residue solubilization, and two washing steps with hexane. Moreover, in order to elucidate structural characteristics of phenolic compounds in VOO, high performance liquid chromatography with a diode array detector (HPLC-DAD at 280 and 340 nm and HPLC coupled to electrospray ionization mass spectrometry (HPLC-ESI-MS in the negative-ion mode were performed. The most abundant phenolic compounds were oleuropein derivatives with m/z 319 and 377 and ligstroside derivatives with m/z 303, 361. Lignans, such as 1-acetoxypinoresinol and pinoresinol were also present in substantial quantities in the phenolic fraction. However, pinoresinol was co-eluted with dialdehydic form of ligstroside aglycone (DAFLA and it was not possible to be quantified separately. The phenolic extracts, obtained from different VOO samples, yielded similar HPLC profiles. Differences, however, were observed in the last part of the chromatogram, corresponding to isomers of the aldehydic form of ligstroside aglycone. Oxidized phenolic products, originating from secoiridoids, were also detected.

  15. Extraction, Separation, and Identification of Phenolic Compounds in Virgin Olive Oil by HPLC-DAD and HPLC-MS.

    Science.gov (United States)

    Tasioula-Margari, Maria; Tsabolatidou, Eleftheria

    2015-01-01

    The aim of this study was to evaluate the recovery of individual phenolic compounds extracted from virgin olive oil (VOO), from different Greek olive varieties. Sufficient recoveries (90%) of all individual phenolic compounds were obtained using methanol as an extraction solvent, acetonitrile for residue solubilization, and two washing steps with hexane. Moreover, in order to elucidate structural characteristics of phenolic compounds in VOO, high performance liquid chromatography with a diode array detector (HPLC-DAD) at 280 and 340 nm and HPLC coupled to electrospray ionization mass spectrometry (HPLC-ESI-MS) in the negative-ion mode were performed. The most abundant phenolic compounds were oleuropein derivatives with m/z 319 and 377 and ligstroside derivatives with m/z 303, 361. Lignans, such as 1-acetoxypinoresinol and pinoresinol were also present in substantial quantities in the phenolic fraction. However, pinoresinol was co-eluted with dialdehydic form of ligstroside aglycone (DAFLA) and it was not possible to be quantified separately. The phenolic extracts, obtained from different VOO samples, yielded similar HPLC profiles. Differences, however, were observed in the last part of the chromatogram, corresponding to isomers of the aldehydic form of ligstroside aglycone. Oxidized phenolic products, originating from secoiridoids, were also detected. PMID:26783843

  16. Cobalamin speciation using reversed-phase micro-high-performance liquid chromatography interfaced to inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Micro-high-performance liquid chromatography interfaced to inductively coupled plasma mass spectrometry was optimized for the determination and separation of a mixture of cobalt containing species. Four cobalamin species (cyanocobalamin, hydroxocobalamin, methylcobalamin, and 5'-deoxyadenosylcobalamin) representing the various forms of vitamin B12 as well as the harmful corrinoid analogue cobinamide dicyanide were separated using reversed-phase microcapillary chromatography with columns containing C18 packing material with a 2-μm particle size. Selection of organic solvents for the separation took into consideration compatibility with the inductively coupled plasma mass spectrometer being used for element specific detection. Optimized method conditions included use of a methanol gradient and make-up solution for the nebulizer. Some issues associated with dead volume were overcome by the extension of the gradient program. The total analysis time was 52 min. The column-to-column variability was evaluated and was found to be very reasonable (9% RSD on average), confirming that this method is rugged and that the technology should be easily transferred to other laboratories

  17. Cobalamin speciation using reversed-phase micro-high-performance liquid chromatography interfaced to inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Yanes, Enrique G. E-mail: yanes@bhnrc.usda.gov; Miller-Ihli, Nancy J. E-mail: miller-ihli@bhnrc.usda.gov

    2004-06-18

    Micro-high-performance liquid chromatography interfaced to inductively coupled plasma mass spectrometry was optimized for the determination and separation of a mixture of cobalt containing species. Four cobalamin species (cyanocobalamin, hydroxocobalamin, methylcobalamin, and 5'-deoxyadenosylcobalamin) representing the various forms of vitamin B12 as well as the harmful corrinoid analogue cobinamide dicyanide were separated using reversed-phase microcapillary chromatography with columns containing C18 packing material with a 2-{mu}m particle size. Selection of organic solvents for the separation took into consideration compatibility with the inductively coupled plasma mass spectrometer being used for element specific detection. Optimized method conditions included use of a methanol gradient and make-up solution for the nebulizer. Some issues associated with dead volume were overcome by the extension of the gradient program. The total analysis time was 52 min. The column-to-column variability was evaluated and was found to be very reasonable (9% RSD on average), confirming that this method is rugged and that the technology should be easily transferred to other laboratories.

  18. Cobalamin speciation using reversed-phase micro-high-performance liquid chromatography interfaced to inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Yanes, Enrique G.; Miller-Ihli, Nancy J.

    2004-06-01

    Micro-high-performance liquid chromatography interfaced to inductively coupled plasma mass spectrometry was optimized for the determination and separation of a mixture of cobalt containing species. Four cobalamin species (cyanocobalamin, hydroxocobalamin, methylcobalamin, and 5'-deoxyadenosylcobalamin) representing the various forms of vitamin B12 as well as the harmful corrinoid analogue cobinamide dicyanide were separated using reversed-phase microcapillary chromatography with columns containing C18 packing material with a 2-μm particle size. Selection of organic solvents for the separation took into consideration compatibility with the inductively coupled plasma mass spectrometer being used for element specific detection. Optimized method conditions included use of a methanol gradient and make-up solution for the nebulizer. Some issues associated with dead volume were overcome by the extension of the gradient program. The total analysis time was 52 min. The column-to-column variability was evaluated and was found to be very reasonable (9% RSD on average), confirming that this method is rugged and that the technology should be easily transferred to other laboratories.

  19. Simultaneous determination of some food additives in soft drinks and other liquid foods by flow injection on-line dialysis coupled to high performance liquid chromatography.

    Science.gov (United States)

    Kritsunankul, Orawan; Jakmunee, Jaroon

    2011-06-15

    Flow injection on-line dialysis was developed for sample pretreatment prior to the simultaneous determination of some food additives by high performance liquid chromatography (FID-HPLC). A liquid sample or mixed standard solution (900 μL) was injected into a donor stream (5%, w/v, sucrose) of FID system and was pushed further through a dialysis cell, while an acceptor solution (0.025 mol L(-1) phosphate buffer, pH 3.75) was held in the opposite side of the dialysis membrane. The dialysate was then flowed to an injection loop of the HPLC valve, where it was further injected into the HPLC system and analyzed under isocratic reverse-phase HPLC conditions and UV detection (230 nm). The order of elution of five food additives was acesulfame-K, saccharin, caffeine, benzoic acid and sorbic acid, respectively, with the analysis time of 14 min. On-line dialysis and HPLC analysis could be performed in parallel, providing sample throughput of 4.3h(-1). Dialysis efficiencies of five food additives were in ranges of 5-11%. Linear calibration graphs were in ranges of 10-100 mg L(-1) for acesulfame-K and saccharin, 10-250 mg L(-1) for benzoic acid and 10-500 mg L(-1) for caffeine and sorbic acid. Good precisions (RSD<5%) for all the additives were obtained. The proposed system was applied to soft drink and other liquid food samples. Acceptable percentage recoveries could be obtained by appropriate dilution of the sample before injecting into the system. The developed system has advantages of high degrees of automation for sample pretreatment, i.e., on-line sample separation and dilution and low consumption of chemicals and materials. PMID:21641449

  20. Microfluidic chip based nano liquid chromatography coupled to tandem mass spectrometry for the determination of abused drugs and metabolites in human hair.

    Science.gov (United States)

    Zhu, Kevin Y; Leung, K Wing; Ting, Annie K L; Wong, Zack C F; Ng, Winki Y Y; Choi, Roy C Y; Dong, Tina T X; Wang, Tiejie; Lau, David T W; Tsim, Karl W K

    2012-03-01

    A microfluidic chip based nano-HPLC coupled to tandem mass spectrometry (nano-HPLC-Chip-MS/MS) has been developed for simultaneous measurement of abused drugs and metabolites: cocaine, benzoylecgonine, cocaethylene, norcocaine, morphine, codeine, 6-acetylmorphine, phencyclidine, amphetamine, methamphetamine, MDMA, MDA, MDEA, and methadone in the hair of drug abusers. The microfluidic chip was fabricated by laminating polyimide films and it integrated an enrichment column, an analytical column and a nanospray tip. Drugs were extracted from hairs by sonication, and the chromatographic separation was achieved in 15 min. The drug identification and quantification criteria were fulfilled by the triple quardropule tandem mass spectrometry. The linear regression analysis was calibrated by deuterated internal standards with all of the R(2) at least over 0.993. The limit of detection (LOD) and the limit of quantification (LOQ) were from 0.1 to 0.75 and 0.2 to 1.25 pg/mg, respectively. The validation parameters including selectivity, accuracy, precision, stability, and matrix effect were also evaluated here. In conclusion, the developed sample preparation method coupled with the nano-HPLC-Chip-MS/MS method was able to reveal the presence of drugs in hairs from the drug abusers, with the enhanced sensitivity, compared with the conventional HPLC-MS/MS. PMID:22281681

  1. Determination of iodate by HPLC-UV after on-line electrochemical reduction to iodide.

    Science.gov (United States)

    Wang, Tao; Lin, Weimei; Dai, Xueliang; Gao, Lijun; Wang, Bing; Quan, Dongqin

    2015-02-01

    In this study, a novel on-line pre-column electrochemical instrument (PECI) coupled with high-performance liquid chromatography (HPLC) was developed, and a novel method based on PEC-HPLC-UV for amplifying the ultraviolet (UV) response of iodate (IO₃⁻) was studied. Iodate undergoes reduction in the PECI, and the resulting I(-) was injected to an HPLC system and detected by a UV detector. For IO₃⁻ analysis, conditions that can influence the reduction efficiency, including applied potential, pH value and salt concentration, were investigated in detail. In an appropriate condition, the UV response of iodate after passing through PECI was almost 10 times more than that of the initial form with good precision (relative standard deviation 2.0-4.3%). The detection limit and quantity limit were 9 and 20 ng, respectively. It can be concluded that the proposed method is simple and highly sensitive. PMID:25002682

  2. Postcolumn reaction detectors for HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Frei, R.W.; Jansen, H.; Brinkman, U.A.T.

    1985-12-01

    Currently, the best and most reliable HPLC (high-performance liquid chromatography) detectors are UV-VIS absorbance, fluorescence, and electrochemical detectors. It is attractive to try to expand their range of application by using suitable chemical derivatization techniques to convert the analytes of interest with their originally poor detection properties into compounds that can be detected with high sensitivity with these detectors. Besides an improvement of the detection properties, the chemical reaction can also enhance the selectivity of the total analytical method. The derivatization can be carried out either prior to the HPLC separation or by doing the reaction in an on-line postcolumn mode. Comparative advantages and disadvantages of these two approaches have been discussed previously. This paper will discuss on-line postcolumn derivatization. A general scheme of an HPLC system equipped with an on-line postcolumn reaction detector is given. 40 references, 6 figures, 2 tables.

  3. Simultaneous Identification and Quantification of Canrenone and 11-α-Hydroxy-Canrenone by LC-MS and HPLC-UVD

    OpenAIRE

    Ya-Juan Wang; Meng-Yi Yang; Li-Ming Zhao; Wen-Jing Sun; Feng-Jie Cui; Tian-Zhen Zhang; Da-Ming Huang

    2011-01-01

    A procedure for simultaneous identification and quantification of canrenone and its biotransformed product 11- α -hydroxy-canrenone by high-performance liquid chromatography with ultraviolet detector (HPLC-UVD) and mass spectrometry (LC-MS) methods was proposed. The optimal determination variables on the HPLC-UVD or LC-MS coupled with a ZORBAX Eclipse XDB-C18 column (150 mm × 4.6 mm, 5 μm) were set as follows: detection wavelength of 280 nm, mobile phase of water and methanol gradient elution...

  4. Comparison of microbial communities in Lake Tahoe surface sample with Tonga Trench water column samples using High Pressure Liquid Chromatography - Electrospray Ionization - Mass Spectroscopy (HPLC - ESI - MS) and Global Natural Products Social Molecular Network (GNPS)

    Science.gov (United States)

    Belmonte, M. A.

    2015-12-01

    Intact polar lipids (IPLs) are lipids composed of a head group, a glycerol, and a fatty acid chain that make up the lipid bilayer of cell membranes in living cells; and the varying head groups can be indicative of the type of microbes present in the environment (Van Mooy 2010). So by distinguishing and identifying the IPL distribution in an environment one can make inferences about the microbial communities in the said environment. In this study, we used High Pressure Liquid Chromatography-Electrospray Ionization- Mass Spectroscopy (HPLC-ESI-MS) and Global Natural Products Social Molecular Networking (GNPS) to compare the IPL distributions of two oligotrophic environments: surface waters of Lake Tahoe in the Sierra Nevada Mountains, and the water column of the Tonga Trench in the South Pacific. We hypothesized that the similar nutrient dynamics of the two oligotrophic environments would result in similar eukaryotic and prokaryotic communities, which would be reflected in the IPL composition of suspended particulate organic matter (POM). For simplicity we focused on the classes of IPLs most commonly observed in the marine environment: phosphotidylglycerol (PG), phosphotidylethanolamine (PE), diacylglyceryl-trimethyl-homoserine (DGTS), diacylglyceryl-hydroxymethyl-trimethylalanine (DGTA), sulfoquinovosyldiacylglycerol (SQDG), monoglycosyldiacylglycerol (MGDG) and diglycosyldiacylglycerol (DGDG). Our results showed that all of the marine IPLs of interest were present in Lake Tahoe which confirms that there are many of the same microbial communities in the fresh waters of Lake Tahoe and the salt waters Tonga Trench.

  5. Determination of sulfonamides in meat by liquid chromatography coupled with atmospheric pressure chemical ionization mass spectrometry

    International Nuclear Information System (INIS)

    Liquid chromatography/atmospheric pressure chemical ionization-mass spectrometry (LC-APCI-MS) has been used for the determination of sulfonamides in meat. Five typical sulfonamides were selected as target compounds, and beef meat was selected as a matrix sample. As internal standards, sulfapyridine and isotope labeled sulfamethazine (13C6-SMZ) were used. Compared to the results of recent reports, our results have shown improved precision to a RSD of 1.8% for the determination of sulfamethazine spiked with 75 ng/g level in meat

  6. Rapid determination of 19 quinolone residues in spiked fish and pig muscle by high-performance liquid chromatography (HPLC) tandem mass spectrometry.

    Science.gov (United States)

    Li, Y L; Hao, X L; Ji, B Q; Xu, C L; Chen, W; Shen, C Y; Ding, T

    2009-03-01

    A multiresidue method has been developed for the confirmation and quantification of 19 quinolones (enrofloxacin, ciprofloxacin, norfloxacin, ofloxacin, flumequine, oxolinic acid, difloxacin, sarafloxacin, sparfloxacin, danofloxacin, fleroxacin, marbofloxacin, enoxacin, orbifloxacin, pefloxacin, nalidixic acid, pipemidic acid, lomefloxacin and cinoacin) in pig and fish by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with acetonitrile, analytes separated by LC on a C18 column using 0.1% formic acid-methanol with a linear gradient elution programme, and detected by MS/MS. The linear range was 0.3-50 microg kg(-1) with correlation coefficients (r) more than 0.9956. The limits of detection were 0.1 microg kg(-1). Mean recoveries for each analyte in pig muscle and fish ranged from 75.3% to 96.3% and from 79.7% to 94.2% with relative standard deviations below 10%. The method is fast, safe, sensitive and precise, and can be used simultaneously to analyse residual quinolones. PMID:19680903

  7. A single marker choice strategy in simultaneous characterization and quantification of multiple components by rapid resolution liquid chromatography coupled with triple quadrupole tandem mass spectrometry (RRLC-QqQ-MS).

    Science.gov (United States)

    Ning, Zhangchi; Liu, Zhenli; Song, Zhiqian; Zhao, Siyu; Dong, Yunzhuo; Zeng, Honglian; Shu, Yisong; Lu, Cheng; Liu, Yuanyan; Lu, Aiping

    2016-05-30

    Single standard to determine multi-components (SSDMC) method has been accepted as an efficient technique for the quality control of Traditional Chinese medicines (TCMs), especially for overcoming the shortage of reference standards. HPLC-UV methods have been applied to establish SSDMC method for quantitative analysis in several plant medicines and Chinese patent medicines, however, no LC-MS methods have been used. The purpose of this study is to put forward an improved strategy for the choice of single marker in SSDMC using rapid resolution liquid chromatography coupled with triple quadrupole tandem mass spectrometry (RRLC-QqQ-MS). Five different Panax genus plants, recorded in the Chinese Pharmacopeia 2015 edition, were used as research subjects. An improved SSDMC strategy for simultaneous characterization and determination of 18 bioactive saponins in five Panax plants was put forward, and which was validated to be more superior. Then, it was fully investigated with respect to linearity, LODs, LOQs, precision and accuracy. Coupling with multivariate statistical analysis, the established and validated SSDMC strategy could be successively used in discrimination of the five Panax genus plants. PMID:26955755

  8. Protein Stable Isotope Fingerprinting (P-SIF): Multidimensional Protein Chromatography Coupled to Stable Isotope-Ratio Mass Spectrometry

    Science.gov (United States)

    Pearson, A.; Bovee, R. J.; Mohr, W.; Tang, T.

    2012-12-01

    As metagenomics increases our insight into microbial community diversity and metabolic potential, new approaches are required to determine the biogeochemical expression of this potential within ecosystems. Because stable isotopic analysis of the major bioactive elements (C, N) has been used historically to map flows of substrates and energy among macroscopic food webs, similar principles may apply to microbes. To address this challenge, we have developed a new analytical approach called Protein Stable Isotope Fingerprinting (P-SIF). P-SIF generates natural stable isotopic fingerprints of microbial individual or community proteomes. The main advantage of P-SIF is the potential to bridge the gap between diversity and function, thereby providing a window into the "black box" of environmental microbiology and helping to decipher the roles of uncultivated species. Our method implements a three-way, orthogonal scheme to separate mixtures of whole proteins into subfractions dominated by single or closely-related proteins. Protein extracts first are isoelectrically focused in a gel-free technique that yields 12 fractions separated over a gradient of pH 3-10. Each fraction then is separated by size-exclusion chromatography into 20 pools, ranging from >100kD to ~10kD. Finally, each of these pools is subjected to HPLC and collected in 40 time-slices based on protein hydrophobicity. Theoretical calculation reveals that the true chromatographic resolution of the total scheme is 5000, somewhat less than the 9600 resulting fractions. High-yielding fractions are subjected to δ13C analysis by spooling-wire microcombustion irMS (SWiM-irMS) optimized for samples containing 1-5 nmol carbon. Here we will present the method, results for a variety of pure cultures, and preliminary data for a sample of mixed environmental proteins. The data show the promise of this method for unraveling the metabolic complexity hidden within microbial communities.

  9. Rapid screening and identification of compounds with DNA-binding activity from Folium Citri Reticulatae using on-line HPLC-DAD-MS(n) coupled with a post column fluorescence detection system.

    Science.gov (United States)

    Fu, Qingrong; Zhang, Cangman; Lin, Zongtao; Sun, Hongyang; Liang, Yi; Jiang, Haixiu; Song, Zhiling; Wang, Hong; Chen, Shizhong

    2016-02-01

    To study the interactions between natural compounds and deoxyribonucleic acid (DNA), a method has been established combining a high-performance liquid chromatography-diode array detector-multi-stage mass spectrometer with a fluorescence detector (HPLC-DAD-MS(n)-FLD). The FLD was used to monitor fluorescence intensity of the ethidium bromide-DNA (EB-DNA) complex when a compound separated by HPLC was introduced. This novel method was used to simultaneously obtain the HPLC fingerprint, UV spectra, MS(n) fragments and DNA-binding activity profile of various components in Folium Citri Reticulatae. As a result, 35 compounds were identified, of which 25 were found in the extract of Folium Citri Reticulatae for the first time, and 33 compounds showed DNA-binding activities, with the most active being feruloylhexaric and p-coumaroylhexaric acids. In addition, the precision, stability and reproducibility of this method were validated by two positive controls, quercetin and hesperidin. This new on-line method is accurate, precise and reliable for further high-throughput screening of DNA-binding compounds from food samples and other complex matrices. PMID:26304344

  10. Effect of Ionic Liquid on the Determination of Aromatic Amines as Contaminants in Hair Dyes by Liquid Chromatography Coupled to Electrochemical Detection

    OpenAIRE

    Maria Valnice Boldrin Zanoni; Thiago Mescoloto Lizier

    2012-01-01

    The room temperature ionic liquid (IL) 1-butyl-3-methylimidazolium bis-(trifluorometanesulfonyl)imide BMIm[NTf2] was used as a novel medium for improvement of separation and quantization of 16 aromatic amines typically present as contaminants in consumer products and detected by HPLC coupled to an electrochemical detector. The aromatic amines, namely 4,4'-diaminodiphenylmethane, 4-chloroaniline, 2-methoxy-5-methyl-aniline, 3,3'-dimethylbenzidine, 2,4-diaminoto...

  11. Speciation of arsenic in human nail and hair from arsenic-affected area by HPLC-inductively coupled argon plasma mass spectrometry

    International Nuclear Information System (INIS)

    Nail and hair are rich in fibrous proteins, i.e., α-keratins that contain abundant cysteine residues (up to 22% in nail and 10-14% in hair). Although they are metabolically dead materials in the epidermis, the roots are highly influenced by the health status of the living beings and their analyses are used as a tool to monitor occupational and environmental exposure to toxic elements. The aims of the present study are to speciate arsenicals in human nail and hair and also to judge whether they should be used as a biomarker to arsenic (As) exposure and/or toxicity. All human fingernail and hair samples (n = 47) were collected from the As-affected area of West Bengal, India. Speciation of arsenicals in water extracts of fingernails and hair at 90 degree sign C was carried out by HPLC-inductively coupled argon plasma mass spectrometer (ICP MS). Fingernails contained iAsIII (58.6%), iAsV (21.5), MMAV (7.7), DMAIII (9.2), and DMAV (3.0), and hair contained iAsIII (60.9%), iAsV (33.2), MMAV (2.2), and DMAV (3.6). Fingernails contained DMAIII, but hair did not. The higher percentage of iAsIII both in fingernails and hair than that of iAsV suggests more affinity of iAsIII to keratin. Although all arsenicals in fingernails and hair correlate to As exposure positively, As speciation in fingernails seems to be more correlated with arsenism than that in hair. Exogenous contamination is a confounding factor for hair to consider it as a biomarker, whereas this is mostly absent in fingernails, which recommends it to be a better biomarker to arsenic exposure. DMAIII content in fingernails and DMAV contents in both fingernails and hair could be the biomarker to As exposure

  12. Speciation analysis of selenium metabolites in urine and breath by HPLC- and GC-inductively coupled plasma-MS after administration of selenomethionine and methylselenocysteine to rats.

    Science.gov (United States)

    Ohta, Yuki; Kobayashi, Yayoi; Konishi, Sakae; Hirano, Seishiro

    2009-11-01

    Selenium is an essential trace element found in vegetables as selenomethionine (SeMet) and methylselenocysteine (MeSeCys). In the present study, we used stable isotopes of Se to investigate differences between how SeMet and MeSeCys are metabolized, using methylseleninic acid (MSA) as a reference methylselenol source. A mixture containing (76)Se-SeMet, (77)Se-MeSeCys, and (82)Se-MSA (each 25 microg Se/kg b.w.) was orally administered to rats, and then, speciation analyses of Se in urine and exhaled gas were conducted using HPLC-inductively coupled plasma (ICP)-MS and GC-ICP-MS, respectively. The proportions of (76)Se-, (77)Se-, and (82)Se-selenosugar (Se-sugar) to total urinary Se metabolites originating from each tracer were very similar, while the proportion of (77)Se-tirmethylselenonium (TMSe) was much less than that of(76)Se- and (82)Se-TMSe in urine, suggesting that(77)Se-SeMet is less efficiently metabolized to TMSe. Similarly, there was significantly less (77)Se-dimethylselenide (DMSe) originating from (77)Se-SeMet than(76)Se- and (82)Se-DMSe originating from (76)Se-MeSeCys and (82)Se-MSA in exhaled gas. It is generally accepted that DMSe and TMSe are metabolites of methylselenol, a putative metabolic intermediate in Se metabolism. Methylselenol is believed to be responsible for the cancer chemoprevention effects of Se. These results suggest that MeSeCys is converted to methylselenol more efficiently than is SeMet and that urinary TMSe and exhaled DMSe might be useful biomarkers for the generation of cancer chemopreventive forms of Se. PMID:19715347

  13. On-line coupling of an ion chromatograph to the ICP-MS: Separations with a cation exchange chromatography column

    Energy Technology Data Exchange (ETDEWEB)

    Roellin, Stefan [Studsvik Nuclear AB, Nykoeping (Sweden)

    1999-12-01

    An ion chromatography system was coupled on-line to the ICP-MS. All separations were made with a cation exchange chromatography column. Fundamental laws about elution parameters affecting individual retention times and elution forms are explained by applying a proper ion exchange mechanism for the isocratic elution (separations with constant eluent concentration) of mono-, di-, tri-, and tetravalent cations and the actinide species MO{sub 2}{sup +} and MO{sub 2}{sup 2+}. A separation method with two eluents has been investigated to separate mono- from divalent ions in order to separate isobaric overlaps of Rb/Sr and Cs/Ba. The ions normally formed by actinides in aqueous solutions in the oxidation states III to VI are M{sup 3+}, M{sup 4+}, MO{sub 2}{sup +} and MO{sub 2}{sup 2+} respectively. Elution parameters were investigated to separate all four actinide species from each other in order to separate isobaric overlaps of the actinides Np, Pu, U and Am. A major question of concern over the possible release of actinides to the environment is the speciation of actinides within their four possible oxidation states. To check the possibility of speciation analysis with ion chromatography, a separation method was investigated to separate U{sup 4+} and UO{sub 2}{sup 2+} without changing the redox species composition during the separation. First results of Pu speciation analysis showed that Pu could be eluted as three different species. Pu(VI) was always eluting at the same time as Np(V). This was surprising as Pu(VI) is expected to have the same chemical characteristics as U(VI) and thus was expected to elute at the same time as U(VI)

  14. Validated assay for the simultaneous quantification of total vincristine and actinomycin-D concentrations in human EDTA plasma and of vincristine concentrations in human plasma ultrafiltrate by high-performance liquid chromatography coupled with tandem mass spectrometry

    NARCIS (Netherlands)

    C.W.N. Damen; T. Israëls; H.N. Caron; J.H.M. Schellens; H. Rosing; J.H. Beijnen

    2009-01-01

    A sensitive, specific and efficient high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS) assay for the simultaneous determination of total vincristine and actinomycin-D concentrations in human plasma and an assay for the determination of unbound vincristine are presented. Ele

  15. Pesticide analysis at ppt concentration levels: coupling nano-liquid chromatography with dielectric barrier discharge ionization-mass spectrometry.

    Science.gov (United States)

    Mirabelli, Mario F; Wolf, Jan-Christoph; Zenobi, Renato

    2016-05-01

    We report the coupling of nano-liquid chromatography (nano-LC) with an ambient dielectric barrier discharge ionization (DBDI)-based source. Detection and quantification were carried out by high-resolution mass spectrometry (MS), using an LTQ-Orbitrap in full scan mode. Despite the fact that nano-LC systems are rarely used in food analysis, this coupling was demonstrated to deliver extremely high sensitivity in pesticide analysis, with limits of detection (LODs) as low as 10 pg/mL. In all cases, the limits of quantification (LOQs) were compliant with the current EU regulation. An excellent signal linearity over up to four orders of magnitude was also observed. Therefore, this method can easily compete with conventional GC-(EI)-MS or LC-ESI-MS/MS methods and in some cases outperform them. The method was successfully tested for food sample analysis, with apples and baby food, extracted using the QuEChERS approach. Our results demonstrate an outstanding sensitivity (at femtogram level) and reproducibility of the nano-LC-DBDI coupling, capable of improving routine pesticide analysis. To the best of our knowledge, this is the most sensitive and reproducible plasma-MS-based method for pesticide analysis reported to date. PMID:26898206

  16. Direct determination of melamine in dairy products by gas chromatography/mass spectrometry with coupled column separation

    International Nuclear Information System (INIS)

    A coupled capillary column system was developed for the qualitative and quantitative determination of melamine with isotope internal standard in dairy products by gas chromatography/mass spectrometry (GC/MS) without derivatization. A 30 m of DB-5ms ((5%-phenyl)-methylpolysiloxane, 0.25 mm i.d., 0.25 μm df) coupled with a 1.5 m of Innowax (polyethylene glycol, 0.32 mm i.d., 0.25 μm df) by a quartz capillary column connector was introduced as separation column. Three advantages were discussed for the coupled system. The sample was fortified with a ring-labeled 13C315N3-melamine as an isotope internal standard and extracted by 1% of trichloroacetic acid aqueous solution. 2.2% of lead acetate solution was then added to deposit protein in the sample matrix. After purification by cation exchange cartridge, the sample solution was directly injected and detected by GC/MS. A six-point calibration curve ranging from 0.05 to 2 mg kg-1 of melamine in sample was used to establish instrument response. The recovery was 93.9-102% with relative standard deviation from 3.1 to 8.7% when isotope internal standard used. The calculated method detection limit was 0.01 mg kg-1.

  17. Simultaneous determination of capsaicin and dihydrocapsaicin for vegetable oil adulteration by immunoaffinity chromatography cleanup coupled with LC-MS/MS.

    Science.gov (United States)

    Ma, Fei; Yang, Qingqing; Matthäus, Bertrand; Li, Peiwu; Zhang, Qi; Zhang, Liangxiao

    2016-05-15

    Capsaicin and dihydrocapsaicin were selected as adulteration markers to authenticate vegetable oils. In this study, a method of immunoaffinity chromatography (IAC) combined with liquid chromatography-tandem mass spectrometry was established for the determination of capsaicin and dihydrocapsaicin in vegetable oils. In this method, immunosorbents were obtained by covalently coupling highly specific capsaicinoid polyclonal antibodieswith CNBr-activated Sepharose 4B, and then packed into a polyethylene column. In this paper, the major parameters affecting IAC extraction efficiency, including loading, washing and eluting conditions, were also investigated. The IAC column displayed high selectivity for capsaicin and dihydrocapsaicin with the maximum capacity of 240ng. The limit of detection (LOD) and limit of quantification (LOQ) for capsaicin were calculated as 0.02 and 0.08μgkg(-1), and for dihydrocapsaicin were 0.03 and 0.10μgkg(-1). The recoveries of capsaicin and dihydrocapsaicin in oil samples were in the range of 87.3-95.2% with the relative standard deviation (RSD) of less than 6.1%. The results indicated that capsaicinoid compounds could not be found in edible vegetable oils. Therefore, the proposed method is simple, reliable and adequate for routine monitoring of capsaicinoid compounds in vegetable oils and has an excellent potential for detection of adulteration with inedible waste oil. PMID:26739369

  18. Analysis of neonicotinoids by gas chromatography coupled to nuclide 63Ni - Electron Capture Detector - GC/ECD

    International Nuclear Information System (INIS)

    Recently, several reports have been published discussing reduction in bee population which polymerizes cultures around the world this phenomenon is known as Colony Collapse Disorder (CCD). The phenomenon describes the lack of worker honeybees in the colony despite having pups and food. The causes of this problem are unknown but there are studies that claim that reduction of population of bees is linked to poisoning through insecticides specifically neonicotinoids. Among this type of pesticide are imidacloprid (C9H10ClN5O2), clothianidin (C6H8ClN5O2S) and thiamethoxam (C8H10ClN5O3S). This paper presents the analysis of neonicotinoids - clothianidin, imidacloprid and thiamethoxam - by the technique of gas chromatography coupled to nuclide 63Ni electron capture detector (GC/ECD). The electron capture detector (ECD) is a gas chromatography detector that has been used for the detection of organic halogens, nitriles, nitrates and organometallic compounds. The ECD detector ionizes the analytes by the beta particles from the nuclide sources 63Ni within carrier gas N2. The electrons produced in this process are collected and create a current that are amplified and generates a chromatographic peak. Methodology and details of the analysis are present in this work. (author)

  19. Determination of azithromycin residue in pork using a molecularly imprinted monolithic microcolumn coupled to liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Zhou, Tong; Yang, Haicui; Jin, Zhen; Liu, Qingying; Song, Xuqin; He, Limin; Fang, Binghu; Meng, Chenying

    2016-04-01

    Using spiramycin as a dummy template, a molecularly imprinted polymer monolithic micro-column with high selection to azithromycin was prepared in a micropipette tip. The imprinting factor of the monolithic micro-column prepared was approximately 2.67 and the morphological structure of the polymers was characterized by scanning electron microscopy. A simple, sensitive, and reproducible method based on the imprinted monolithic micro-column coupled to liquid chromatography with tandem mass spectrometry was developed for determining the residues of azithromycin in pork. Pork samples were extracted with acetonitrile, cleaned up under the optimal monolithic micro-column conditions, and analyzed using liquid chromatography with tandem mass spectrometry in the multiple reaction monitoring mode. The assay exhibited a linear dynamic range of 0.50-50 μg/L with the correlation coefficient (r(2) ) above 0.99. In the three spiking levels of 0.50, 1.0, and 10 μg/kg, the average recoveries of azithromycin from pork samples were between 85.8 and 96.5% with a relative standard deviation below 10%. The limit of detection and limit of quantitation were 0.03 and 0.1 μg/kg, respectively. PMID:26854282

  20. Novel molecularly-imprinted solid-phase microextraction fiber coupled with gas chromatography for analysis of furan.

    Science.gov (United States)

    Hashemi-Moghaddam, Hamid; Ahmadifard, Mojtaba

    2016-04-01

    This study combined a molecularly-imprinted polymer with headspace solid-phase microextraction (HS-SPME). Preparation of molecularly-imprinted polymer is not effective for volatile compounds. To overcome this limitation, pyrrole was chosen as a template for the preparation of the furan-imprinted polymer. The holes in the synthesized polymer were suitable for furan adsorption because the chemical structure of pyrrole is similar to that of furan. The extraction properties of the fiber to furan were examined using an HS-SPME device coupled with gas chromatography-flame ionization detection (GC-FID) and gas chromatography-mass spectrometry (GC-MS). The effects of the extraction parameters of exposure time, sampling temperature, and salt concentration on extraction efficiency were studied. Satisfactory reproducibility was obtained for extractions from spiked water samples at RSDdetection limit for furan was 0.042 ng ml(-1). The fabricated fiber was successfully applied for headspace extraction of furan from tap water and canned tuna as shown by GC-MS analysis. PMID:26838393

  1. High performance liquid chromatography coupled with resonance Rayleigh scattering for the detection of three fluoroquinolones and mechanism study

    Science.gov (United States)

    Zhou, Mingqiong; Peng, Jingdong; He, Rongxing; He, Yuting; Zhang, Jing; Li, Aiping

    2015-02-01

    A reliable and versatile high performance liquid chromatography coupled with resonance Rayleigh scattering method was established for the determination of three fluoroquinolones, including levofloxacin, norfloxacin and enrofloxacin in water sample and human urine sample. In pH 4.4-4.6 Britton-Robinson buffer medium, the fluoroquinolones separated by high performance liquid chromatography could react with erythrosine to form 1:1 ion-association complexes, which could make contributions to the great enhancement of RRS. The resonance Rayleigh scattering signal was recorded at λex = λem = 330 nm. The resonance Rayleigh scattering spectral characteristics of the drugs and the experimental conditions such as pH, detection wavelength, erythrosine concentration, flow rate, the length of reaction tube were studied. Quantum chemistry calculation, Fourier transform infrared spectroscopy and absorption spectroscopy were used to discuss the reaction mechanism. The recoveries of samples added standard ranged from 97.53% to 102.00%, and the relative standard deviation was below 4.64%. The limit of detection (S/N = 3) of 0.05-0.12 μg mL-1 was reached, and the linear regression coefficients were all above 0.999. The proposed method was proved as a simple, low cost and high sensitivity method.

  2. Analysis of neonicotinoids by gas chromatography coupled to nuclide {sup 63}Ni - Electron Capture Detector - GC/ECD

    Energy Technology Data Exchange (ETDEWEB)

    Amaral, Priscila O.; Leao, Claudio; Redigolo, Marcelo M.; Crepaldi, Caike; Bustillos, Oscar V., E-mail: priscilaoamaral@gmail.com, E-mail: claudio.leao@usp.br, E-mail: marceloredigolo@gmail.com, E-mail: caike1995@gmail.com, E-mail: ovega@ipen.bremails [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2015-07-01

    Recently, several reports have been published discussing reduction in bee population which polymerizes cultures around the world this phenomenon is known as Colony Collapse Disorder (CCD). The phenomenon describes the lack of worker honeybees in the colony despite having pups and food. The causes of this problem are unknown but there are studies that claim that reduction of population of bees is linked to poisoning through insecticides specifically neonicotinoids. Among this type of pesticide are imidacloprid (C{sub 9}H{sub 10}ClN{sub 5}O{sub 2}), clothianidin (C{sub 6}H{sub 8}ClN{sub 5}O{sub 2}S) and thiamethoxam (C{sub 8}H{sub 10}ClN{sub 5}O{sub 3}S). This paper presents the analysis of neonicotinoids - clothianidin, imidacloprid and thiamethoxam - by the technique of gas chromatography coupled to nuclide {sup 63}Ni electron capture detector (GC/ECD). The electron capture detector (ECD) is a gas chromatography detector that has been used for the detection of organic halogens, nitriles, nitrates and organometallic compounds. The ECD detector ionizes the analytes by the beta particles from the nuclide sources {sup 63}Ni within carrier gas N{sub 2}. The electrons produced in this process are collected and create a current that are amplified and generates a chromatographic peak. Methodology and details of the analysis are present in this work. (author)

  3. A New Metal Tag for Highly Selective and Sensitive Analyses of Amino Acids and Dipeptides by HPLC/ICP-MS

    OpenAIRE

    Daigo Iwahata; Kazuki Nakamura; Rie Yamada; Hiroshi Miyano; Naoyuki Yamada

    2013-01-01

    We have developed a novel metal tag, bis(ethylenediamine)-4'-methyl-4-carboxybipyridine-ruthenium N-succinimidyl ester (ECRS) for sensitive analysis of amino acids using high performance liquid chromatography/inductively coupled plasma mass spectrometry (HPLC/ICP-MS). ECRS is a functional reagent, containing an ester group at one end that can be activated to bind to amino group and a chelated ruthenium at the other. The activated ester was reacted briefly with amino groups under weakly alkal...

  4. Multiclass determination of phytochemicals in vegetables and fruits by ultra high performance liquid chromatography coupled to tandem mass spectrometry.

    Science.gov (United States)

    Alarcón-Flores, María Isabel; Romero-González, Roberto; Vidal, José Luis Martínez; Frenich, Antonia Garrido

    2013-11-15

    In this study a simultaneous determination of several classes of phytochemicals (isoflavones, glucosinolates, flavones, flavonols and phenolic acids) in tomato, broccoli, carrot, eggplant and grape has been carried out by ultra high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Solid-liquid extraction assisted by rotary agitator was utilised, using a mixture of methanol:water (80:20, v/v) as solvent. The analytical procedure was validated in all the matrices, obtaining recoveries ranging from 60% to 120% with repeatability values (expressed as relative standard deviations, RSDs) lower than 25%. Limits of quantification (LOQs) were always equal or lower than 50μg/kg, except for some glucosinolates (125μg/kg). Finally the method was applied to different matrices such as tomato, broccoli, carrot, grape and eggplant, observing that chlorogenic acid was detected in most of the samples at higher concentrations in relation to the other compounds. PMID:23790894

  5. Determination of volatile N-nitrosamines in irradiated fermented sausage by gas chromatography coupled to a thermal energy analyzer.

    Science.gov (United States)

    Byun, Myung-Woo; Ahn, Hyun-Joo; Kim, Jae-Hyun; Lee, Ju-Woon; Yook, Hong-Sun; Han, Sang-Bae

    2004-10-29

    Volatile N-nitrosodimethylamine (NDMA) and N-nitrosopyrrolidine (NPYR) in irradiated pepperoni and salami sausages were determined using a gas chromatography coupled to a thermal energy analyzer (GC-TEA). These fermented sausages with aerobic or vacuum packaging were irradiated at 0, 5, 10, and 20 kGy, and then stored for 4 weeks at 4 degrees C. Both NDMA and NPYR in the fermented sausage were significantly reduced by irradiation. The vacuum packaging showed significantly lower (P 10 kGy) was needed to reduce the carcinogenic N-nitrosamines in the fermented sausage during storage and the GC-TEA analysis was effective in determining the N-nitrosamines in irradiated meats even at low trace levels. PMID:15553169

  6. Identification of the Related Substances in Ampicillin Capsule by Rapid Resolution Liquid Chromatography Coupled with Electrospray Ionization Tandem Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Lei Zhang

    2014-01-01

    Full Text Available Rapid Resolution Liquid Chromatography coupled with Electrospray Ionization Tandem Mass Spectrometry (RRLC-ESI-MSn was used to separate and identify related substances in ampicillin capsule. The fragmentation behaviors of related substances were used to identify their chemical structures. Finally, a total of 13 related substances in ampicillin capsule were identified, including four identified components for the first time and three groups of isomers on the basis of the exact mass, fragmentation behaviors, retention time, and chemical structures in the literature. This study avoided time-consuming and complex chemosynthesis of related substances of ampicillin and the results could be useful for the quality control of ampicillin capsule to guarantee its safety in clinic. In the meantime, it provided a good example for the rapid identification of chemical structures of related substances of drugs.

  7. Identification of the related substances in ampicillin capsule by rapid resolution liquid chromatography coupled with electrospray ionization tandem mass spectrometry.

    Science.gov (United States)

    Zhang, Lei; Cheng, Xian Long; Liu, Yang; Liang, Miao; Dong, Honghuan; Lv, Beiran; Yang, Wenning; Luo, Zhiqiang; Tang, Mingmin

    2014-01-01

    Rapid Resolution Liquid Chromatography coupled with Electrospray Ionization Tandem Mass Spectrometry (RRLC-ESI-MS(n)) was used to separate and identify related substances in ampicillin capsule. The fragmentation behaviors of related substances were used to identify their chemical structures. Finally, a total of 13 related substances in ampicillin capsule were identified, including four identified components for the first time and three groups of isomers on the basis of the exact mass, fragmentation behaviors, retention time, and chemical structures in the literature. This study avoided time-consuming and complex chemosynthesis of related substances of ampicillin and the results could be useful for the quality control of ampicillin capsule to guarantee its safety in clinic. In the meantime, it provided a good example for the rapid identification of chemical structures of related substances of drugs. PMID:25530907

  8. Analysis of N-nitrosodiethylamine by ion chromatography coupled with UV photolysis pretreatment

    Directory of Open Access Journals (Sweden)

    Xueli Li

    2016-04-01

    Full Text Available Nitrosamines such as N-nitrosodiethylamine (NDEA are commonly detected by spectrophotometry after photolysis and Griess reaction (PG in food industries for lower cost. Results of this research indicate that NDEA decays rapidly under UV irradiation, and concentrations of the generated NO2− and NO3− ions vary with photolysis conditions. Thus, the measurement of the PG method may be inconsistent because it is based on the amount of photoproduced NO2−. In addition, more errors may be present in the PG method since NO3− cannot be measured colorimetrically using Griess reagent. In this work, the sum of the concentrations of photoproduced NO2− and NO3− was found to be equivalent to the initial NDEA before photolysis, and a photolysis–ion chromatography method was validated, which may serve as a feasible and accurate method to determine nitrosamines.

  9. Nano Liquid Chromatography Directly Coupled to Electron Ionization Mass Spectrometry for Free Fatty Acid Elucidation in Mussel.

    Science.gov (United States)

    Rigano, Francesca; Albergamo, Ambrogina; Sciarrone, Danilo; Beccaria, Marco; Purcaro, Giorgia; Mondello, Luigi

    2016-04-01

    Recently the miniaturization of liquid chromatography (LC) systems and progresses in mass spectrometry instrumentation have enabled direct introduction of the effluent coming from a nanoLC column into the high-vacuum region of an electron ionization source. In the present research, a nanoLC system was directly coupled to an electron ionization mass spectrometer (EI-MS) without any interface or modification of the ion source. The advantage with respect to atmospheric pressure ionization techniques, normally coupled with LC, is major identification power because of a more extensive and reproducible fragmentation pattern, without any matrix effect or mobile-phase interference. In particular, a nanoLC/EI-MS method was developed for elucidation of the free fatty acid profile in mussel samples, avoiding a previous derivatization step, required when gas chromatographic analysis is involved. A total of 20 fatty acids were reliably identified through the comparison with commercial libraries. A quantitative determination was also carried out by using the response factors approach along with the internal standard method, allowing for quantification of 14 fatty acids. Among them, palmitic acid resulted the most abundant, followed by ω6 arachidonic acid. The quantitative data were compared with those obtained by a well-established technique, such as gas chromatography with flame ionization detection (GC-FID). Both nanoLC/EI-MS and GC-FID methods were validated and similar results were obtained in terms of limit of detection and quantification, resulting in the picomole range, and sensitivity as well was not significantly different, as demonstrated by comparing the slope values of the calibration curves (p < 0.05, from a t-test). PMID:26937891

  10. Simplified sample preparation procedure for measuring isotope-enriched methylmercury by gas chromatography and inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Avramescu, Mary-Luyza; Zhu, Joy; Yumvihoze, Emmanuel; Hintelmann, Holger; Fortin, Danielle; Lean, David R S

    2010-06-01

    Many procedures have been developed to measure the concentration of monomethylmercury (MeHg) from different sample matrices, and the use of stable isotopes of mercury now provides opportunities to determine its formation and degradation rates. Here, a modified procedure for measuring mercury isotopes in sediment samples that uses acid leaching-ion exchange-thiosulfate extraction (TSE) to isolate and purify the methylated mercury from the matrix is proposed. The latter is followed by aqueous-phase ethylation, purge and trap on Tenax, gas chromatography separation of ethylated mercury compounds, and inductively coupled plasma mass spectrometry detection. The new TSE procedure bridges together two well-known methods, the acid-leaching and distillation-derivatization procedures, offering the advantages of artifact-free formation of the first, and low detection limits and the possibility of quantification of individual isotopes of mercury of the second. The modified procedure retains the derivatization, purge and trap, and gas chromatography and inductively coupled plasma mass spectrometry (GC-ICP-MS) detection steps from the distillation-derivatization procedure, and eliminates the distillation step, which is not only laborious but also expensive, due to the high cost of installation and time-consuming cleaning process. Major advantages of the TSE procedure proposed include the extraction and analysis of a large number of samples in a short time, excellent analyte recoveries, and the lack of artifact formation. Sediment certified reference materials (CRMs), BCR 580 and IAEA 405, were used to test the TSE procedure accuracy. Recoveries between 94 to 106% and 95 to 96% were obtained for CRMs and spiked samples (Milli-Q(R) water), respectively. Comparisons among thiosulfate extraction, distillation, and acid-leaching procedures have shown good agreement of methylmercury values. PMID:20821567

  11. HPLC for quality control of polyimides

    Science.gov (United States)

    Young, P. R.; Sykes, G. F.

    1979-01-01

    High Pressure Liquid Chromatography (HPLC) as a quality control tool for polyimide resins and prepregs are presented. A data base to help establish accept/reject criteria for these materials was developed. This work is intended to supplement, not replace, standard quality control tests normally conducted on incoming resins and prepregs. To help achieve these objectives, the HPLC separation of LARC-160 polyimide precursor resin was characterized. Room temperature resin aging effects were studied. Graphite reinforced composites made from fresh and aged resin were fabricated and tested to determine if changes observed by HPLC were significant.

  12. Recent development of multi-dimensional chromatography strategies in proteome research.

    Science.gov (United States)

    Tang, Jia; Gao, Mingxia; Deng, Chunhui; Zhang, Xiangming

    2008-04-15

    As a complementary approach to two-dimensional polyacrylamide gel electrophoresis (2D-PAGE), multi-dimensional chromatography separation methods have been widely applied in all kinds of biological sample investigations. Multi-dimensional liquid chromatography (MDLC) coupled with bio-mass spectrometry (MS) is playing important roles in proteome research due to its high speed, high resolution and high sensitivity. Proteome analysis strategies mainly include bottom-up and top-down approaches which carry out biological sample separation based on peptide and protein levels, respectively. Electrophoretic methods combined with liquid chromatography like IEF-HPLC and HPLC-SDS-PAGE have been successful applied for protein separations. As for MDLC strategy, ion-exchange chromatography (IEX) together with reversed phase liquid chromatography (RPLC) is still a most widely used chromatography in proteome analysis, other chromatographic methods are also frequently used in protein pre-fractionations, while affinity chromatography is usually adopted for specific functional protein analysis. Recent MDLC technologies and applications to variety of proteome analysis have been achieved great development. A digest peptide-based approach as so-called "bottom-up" and intact protein-based approach "top-down" analysis of proteome samples were briefly reviewed in this paper. The diversity of combinations of different chromatography modes to set up MDLC systems was demonstrated and discussed. Novel developments of MDLC techniques such as high-abundance protein depletion and chromatography array were also included in this review. PMID:18289947

  13. Simultaneous determination of three curcuminoids in Curcuma longa L. by high performance liquid chromatography coupled with electrochemical detection

    Directory of Open Access Journals (Sweden)

    Yuling Long

    2014-10-01

    Full Text Available A novel method for analysis of three active components curcumin, demethoxycurcumin and bisdemethoxycurcumin in Curcuma longa L. was developed by HPLC coupled with electrochemical detection. Three curcuminoids were well separated on a C18 column and detected with high sensitivity. A mobile phase containing acetonitrile and 10 mM Na2HPO4–H3PO4 (pH 5.0 (50:50, v/v was used. Good linearity was obtained in the range of 0.208–41.6, 0.197–39.4, and 0.227–114 μM for curcumin, demethoxycurcumin and bisdemethoxycurcumin respectively. The limit of detection reached up to 10−8 M, which was lower than that by UV detection. The relative standard deviations (RSDs ranged from 1.06% to 1.88% for intra-day precision and from 4.30% to 5.79% for inter-day precision, respectively. The proposed method has been applied in real herb sample and recoveries ranging from 86.3% to 111% were obtained.

  14. Simultaneous determination of three curcuminoids in Curcuma longa L. by high performance liquid chromatography coupled with electrochemical detection

    Institute of Scientific and Technical Information of China (English)

    Yuling Long; Wenpeng Zhang; Fang Wang; Zilin Chen

    2014-01-01

    A novel method for analysis of three active components curcumin, demethoxycurcumin and bisdemethoxycurcumin in Curcuma longa L. was developed by HPLC coupled with electrochemical detection. Three curcuminoids were well separated on a C18 column and detected with high sensitivity. A mobile phase containing acetonitrile and 10 mM Na2HPO4-H3PO4 (pH 5.0) (50:50, v/v) was used. Good linearity was obtained in the range of 0.208-41.6, 0.197-39.4, and 0.227-114μM for curcumin, demethoxycurcumin and bisdemethoxycurcumin respectively. The limit of detection reached up to 10 ? 8 M, which was lower than that by UV detection. The relative standard deviations (RSDs) ranged from 1.06%to 1.88%for intra-day precision and from 4.30%to 5.79%for inter-day precision, respectively. The proposed method has been applied in real herb sample and recoveries ranging from 86.3%to 111%were obtained.

  15. Quantification of six bioactive compounds in Zhenqi Fuzheng preparation by high-performance liquid chromatography couple

    Institute of Scientific and Technical Information of China (English)

    Yi-Kai Shi; Fang Cui; Fang-Di Hu; Ying-Yan Bi; Yu-Feng Ma; Shi-Lan Feng

    2011-01-01

    A simple and accurate high-performance liquid chromatography(HPLC)coupled with diode array detector(DAD)and evaporative light scattering detector(ELSD)was established for the determination of six bioactive compounds in Zhenqi Fuzheng preparation(ZFP).The

  16. Determination of trimethylselenonium ion in urine by ion chromatography and inductively coupled plasma mass spectrometry detection

    DEFF Research Database (Denmark)

    Gammelgaard, Bente; Jessen, K.D.; Kristensen, F.H.;

    2000-01-01

    H 3. The Se-78 and Se-82 isotopes were used for the inductively coupled plasma mass spectrometry (ICP-MS) detection. Using the chromatographic system on urine diluted 1 + 1, a large shift in retention times was observed. TMSe+ could be separated from the other species, but the signal from SeMet co...

  17. Dispersive solvent-free ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction coupled with HPLC for determination of ulipristal acetate.

    Science.gov (United States)

    Gong, Aiqin; Zhu, Xiashi

    2015-01-01

    In this paper, a simple and efficient ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction (UA IL-DLLME) coupled with high-performance liquid chromatography for the analysis of ulipristal acetate (UPA) was developed. UPA could be easily migrated into 1-octyl-3-methylimidazolium hexafluorophosphate [C8mimPF6] IL phase without dispersive solvent. The research of extraction mechanism showed that hydrophobic interaction force played a key role in the IL-DLLME. Several important parameters affecting the extraction recovery were optimized. Under the optimized conditions, 25-fold enrichment factor was obtained and the limit of detection (LOD) was 6.8 ng mL(-1) (tablet) or 9.3 ng mL(-1) (serum) at a signal-to-noise ratio of 3. The calibration curve was linear over the range of 0.03-6.0 µg mL(-1). The proposed method was successfully applied to the UPA tablets and the real mice serum samples. PMID:25281147

  18. Determination of polycyclic aromatic hydrocarbons in coffee and tea samples by magnetic solid-phase extraction coupled with HPLC-FLD.

    Science.gov (United States)

    Shi, Yating; Wu, Hao; Wang, Chaoqiong; Guo, Xiaozhen; Du, Juanli; Du, Liming

    2016-05-15

    This study reports the synthesis of a benign nano-adsorbent based on an ionic liquid of immobilized Fe3O4@3-(Trimethoxysilyl)propyl methacrylate@ionic liquid magnetic nanoparticles (Fe3O4@MPS@IL NPs). This material was applied to the magnetic solid phase extraction of seven heavy molecular weight polycyclic aromatic hydrocarbons (PAHs) from coffee and tea samples for high performance liquid chromatography coupled with fluorescence detection. The effects of various parameters of the analytical method were investigated, including pH, sorbent amount, desorption solvent, desorption volume, and extraction and desorption time. Under the optimized conditions, good linearities were obtained, with correlation coefficients (R(2)) between 0.9987 and 0.9998. The detection limits of the proposed method were in the range of 0.1-10ngL(-1). The spiked recoveries of the seven PAHs in coffee and tea samples ranged from 87.5% to 104.5%, with RSDs of less than 3.7%. In addition, a satisfactory reproducibility was achieved, with intra- and inter-day precisions with RSDs of less than 3.1% and 3.8%, respectively. PMID:26775946

  19. Development and validation of polymerized high internal phase emulsion monoliths coupled with HPLC and fluorescence detection for the determination of trace tetracycline antibiotics in environmental water samples.

    Science.gov (United States)

    Du, Fuyou; Zheng, Xian; Sun, Lin; Qin, Qun; Guo, Lin; Ruan, Guihua

    2015-11-01

    A polymerized high internal phase emulsion monolith was used as a novel sorbent for solid-phase extraction coupled with high-performance liquid chromatography and fluorescence detection for the determination of oxytetracycline, tetracycline, doxycycline, and chlorotetracycline in environmental water samples. The polymerized high internal phase emulsion monolithic column was prepared by the in situ polymerization of the continuous phase of a high internal phase emulsion containing glycidyl methacrylate, styrene, and divinylbenzene in pipette tips, and then functionalized with iminodiacetic acid. The resulting monolith exhibited highly interconnected porosity and large surface areas, making it an excellent candidate as an solid-phase extraction sorbent for the enrichment of trace tetracycline antibiotics. Several factors affecting the extraction performance of polymerized high internal phase emulsion monoliths, including the pH of sample solution, the eluting solvents, the sample loading flow rate and volume, were investigated, respectively. Under the optimized conditions, the mean recoveries of oxytetracycline, tetracycline, doxycycline, and chlorotetracycline spiked in pond and farm wastewater samples ranged from 78.1 to 119.3% with relative standard deviation less than 15%. The detection limits (S/N = 3) of the proposed method were in the range of 51-137 pg/mL. This study demonstrated that the monolithic polymerized high internal phase emulsion would be promising solid-phase extraction sorbents in the extraction and proconcentration of trace analytes from complex samples. PMID:26331390

  20. Using of liquid chromatography coupled with diode array detector for determination of naphthoquinones in plants and for investigation of influence of pH of cultivation medium on content of plumbagin in Dionaea muscipula.

    Science.gov (United States)

    Babula, Petr; Mikelova, Radka; Adam, Vojtech; Kizek, Rene; Havel, Ladislav; Sladky, Zdenek

    2006-09-14

    The interest of many investigators in naphthoquinones is due to their broad-range of biological actions from phytotoxic to fungicidal. The main aim of this work was to investigate the influence of different pH values of cultivation medium on naphthoquinone content in Dionaea muscipula. For this purpose, we optimized the simultaneous analysis of the most commonly occurring naphthoquinones (1,4-naphthoquinone, lawsone, juglone and plumbagin) by high performance liquid chromatography coupled with diode array detector (HPLC-DAD). The most suitable chromatographic conditions were as follows: mobile phase: 0.1 mol l-1 acetic acid:methanol in ratio of 33:67 (%, v/v), flow rate: 0.75 ml min-1 and temperature: 42 degrees C. Moreover, we looked for the most suitable technique for preparation of plant samples (D. muscipula, Juglans regia, Paulownia tomentosa, Impatience glandulifera, Impatience parviflora, Drosera rotundifolia, Drosera spathulata and Drosera capensis) due to their consequent analysis by HPLC-DAD. It clearly follows from the results obtained that sonication were the most suitable technique for preparation of J. regia plants. We also checked the recoveries of the determined naphthoquinones, which were from 96 to 104%. Finally, we investigated the changes in content of plumbagin in D. muscipula plants according to different pH of cultivation medium. The content increased with increasing pH up to 5 and, then, changed gradually. The lower content of plumbagin at lower pH values was of interest to us. Therefore, we determined the content of this naphthoquinone in the cultivation medium, what has not been studied before. We discovered that the lower tissue content of plumbagin was due to secretion of this naphthoquinone into the cultivation medium. PMID:16765109

  1. Determination of phosphoric acid triesters in human plasma using solid-phase microextraction and gas chromatography coupled to inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Shah, Monika; Meija, Juris; Cabovska, Baiba; Caruso, Joseph A

    2006-01-27

    A simple and sensitive method for determination of phosphoric acid triesters at trace levels in human plasma sample is described. In this work, solid-phase microextraction (SPME) is employed as a sample preparation procedure for extraction and pre-concentration of alkyl and aryl phosphates followed by gas chromatography coupled to inductively coupled plasma mass spectrometry (GC-ICP-MS) for phosphorus-specific and very sensitive determination of these compounds in human plasma. The detection limits from blood plasma were 50 ngL(-1) (tripropyl phosphate), 17 ngL(-1) (tributyl phosphate), 240 ngL(-1) (tris(2-chloroethyl) phosphate) and 24 ngL(-1) (triphenyl phosphate). Sample preparation involves plasma deproteinization followed by direct immersion SPME with 65 microm poly(dimethylsiloxane/divinylbenzene) fiber. Extraction was performed at 40 degrees C for 30 min and at pH 7.0 in 10 mM sodium carbonate buffer. The reported method, to our knowledge, describes the first application of SPME with element-specific detection for analysis of phosphoric acid esters. Application of the method to the plasma samples, previously stored in poly(vinyl chloride) plasma bags revealed the presence of triphenyl phosphate, which was further confirmed by SPME GC time-of-flight high-resolution mass spectrometry. PMID:16337211

  2. Determination of actinides in environmental and biological samples using high-performance chelation ion chromatography coupled to sector-field inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Truscott, J B; Jones, P; Fairman, B E; Evans, E H

    2001-08-31

    High-performance chelation ion chromatography, using a neutral polystyrene substrate dynamically loaded with 0.1 mM dipicolinic acid, coupled with sector-field inductively coupled plasma mass spectrometry has been successfully used for the separation of the actinides thorium, uranium, americium, neptunium and plutonium. Using this column it was possible to separate the various actinides from each other and from a complex sample matrix. In particular, it was possible to separate plutonium and uranium to facilitate the detection of the former free of spectral interference. The column also exhibited some selectivity for different oxidation states of Np, Pu and U. Two oxidation states each for plutonium and neptunium were found, tentatively identified as Np(V) and Pu(III) eluting at the solvent front, and Np(IV) and Pu(IV) eluting much later. Detection limits were 12, 8, and 4 fg for 237Np, 239Pu, and 241Am, respectively, for a 0.5 ml injection. The system was successfully used for the determination of 239Pu in NIST 4251 Human Lung and 4353 Rocky Flats Soil, with results of 570+/-29 and 2939+/-226 fg g(-1), respectively, compared with a certified range of 227-951 fg g(-1) for the former and a value of 3307+/-248 fg g(-1) for the latter. PMID:11589474

  3. Analysis of perfluoroalkyl substances in cord blood by turbulent flow chromatography coupled to tandem mass spectrometry

    International Nuclear Information System (INIS)

    A fast on-line analytical method based on turbulent flow chromatography (TFC) in combination with tandem mass spectrometry has been applied for the first time for the analysis of eighteen perfluoroalkyl substances (PFASs), in cord blood. A simple and rapid sample pre-treatment was optimised consisting on protein precipitation of 100 μL of sample with acetonitrile (1:1) followed by centrifugation during 10 min. The method was adapted to be sensitive enough and robust with minimum sample injection volume requirements (20 μL). The optimised methodology presented method limits of detection (MLOD) between 0.031 and 0.76 μg/L, detection capabilities (CCα) in the range between 0.005 and 0.99 μg/L and decision limits (CCβ) ranging from 0.006 to 1.16 μg/L. The recoveries in blank blood were calculated by spiking experiments with a mixture of 18 PFASs and established between 70 and 126% for most of compounds. Isotopic dilution was carried out for quantification of selected analytes. In-house validation of this new approach was carried out according to the requirements in the 2002/657/EC Decision. Finally the good applicability of this new approach was proved by the analysis of 60 cord blood samples from two different Mediterranean cities, Barcelona (Spain) and Heraklion (Greece). Ions perfluorohexanesulfonate (PFHxS) and perfluorooctanesulfonate (PFOS) were found at highest concentration and the more frequently compounds were PFHxS, PFOS and perfluorooctanoic acid (PFOA). The newly developed method proved to be suitable for large-scale epidemiologic studies, and to the data on PFASs exposure during pregnancy. -- Highlights: ► An on-line method has been developed for the analysis of 18 perfluoroalkyl substances. ► The method is based on turbulent flow chromatography tandem mass spectrometry. ► The method was applied in 60 cord blood samples from 2 Mediterranean cities. ► Acidic compounds were more frequently found and the method was proved to be suitable for

  4. Analysis of perfluoroalkyl substances in cord blood by turbulent flow chromatography coupled to tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Llorca, Marta; Perez, Francisca [Department of Environmental Chemistry, IDAEA-CSIC, Barcelona (Spain); Farre, Marinella, E-mail: mfuqam@cid.csic.es [Department of Environmental Chemistry, IDAEA-CSIC, Barcelona (Spain); Agramunt, Silvia [Centre for Research in Environmental Epidemiology (CREAL), Barcelona (Spain); IMIM (Hospital del Mar Research Institute), Barcelona (Spain); Kogevinas, Manolis [Centre for Research in Environmental Epidemiology (CREAL), Barcelona (Spain); IMIM (Hospital del Mar Research Institute), Barcelona (Spain); CIBER Epidemiologia y Salud Publica (CIBERESP), Barcelona (Spain); National School of Public Health, Athens (Greece); Barcelo, Damia [Department of Environmental Chemistry, IDAEA-CSIC, Barcelona (Spain); Catalan Institute for Water Research (ICRA), Girona (Spain); King Saud University, Riyadh (Saudi Arabia)

    2012-09-01

    A fast on-line analytical method based on turbulent flow chromatography (TFC) in combination with tandem mass spectrometry has been applied for the first time for the analysis of eighteen perfluoroalkyl substances (PFASs), in cord blood. A simple and rapid sample pre-treatment was optimised consisting on protein precipitation of 100 {mu}L of sample with acetonitrile (1:1) followed by centrifugation during 10 min. The method was adapted to be sensitive enough and robust with minimum sample injection volume requirements (20 {mu}L). The optimised methodology presented method limits of detection (MLOD) between 0.031 and 0.76 {mu}g/L, detection capabilities (CC{alpha}) in the range between 0.005 and 0.99 {mu}g/L and decision limits (CC{beta}) ranging from 0.006 to 1.16 {mu}g/L. The recoveries in blank blood were calculated by spiking experiments with a mixture of 18 PFASs and established between 70 and 126% for most of compounds. Isotopic dilution was carried out for quantification of selected analytes. In-house validation of this new approach was carried out according to the requirements in the 2002/657/EC Decision. Finally the good applicability of this new approach was proved by the analysis of 60 cord blood samples from two different Mediterranean cities, Barcelona (Spain) and Heraklion (Greece). Ions perfluorohexanesulfonate (PFHxS) and perfluorooctanesulfonate (PFOS) were found at highest concentration and the more frequently compounds were PFHxS, PFOS and perfluorooctanoic acid (PFOA). The newly developed method proved to be suitable for large-scale epidemiologic studies, and to the data on PFASs exposure during pregnancy. -- Highlights: Black-Right-Pointing-Pointer An on-line method has been developed for the analysis of 18 perfluoroalkyl substances. Black-Right-Pointing-Pointer The method is based on turbulent flow chromatography tandem mass spectrometry. Black-Right-Pointing-Pointer The method was applied in 60 cord blood samples from 2 Mediterranean cities

  5. 管内固相微萃取-气相色谱法在线联用技术用于水样中的痕量分析%On-Line Coupling of In-Tube Solid Phase Microextraction to Capillary Gas Chromatography for Trace Analysis of Aqueous Samples

    Institute of Scientific and Technical Information of China (English)

    关亚风; 王涵文; 刘文民

    2004-01-01

    Since the development of solid phase microextraction ( SPME ) method, many modifications have been made to improve the availability and application of the technique The in-tube SPME (ITSPME) was emerged and employed in high performance liquid chromatography (HPLC)

  6. Lipidomic profiling of dried seahorses by hydrophilic interaction chromatography coupled to mass spectrometry.

    Science.gov (United States)

    Shen, Qing; Dai, Zhiyuan; Huang, Yao-Wen; Cheung, Hon-Yeung

    2016-08-15

    Dried seahorse is a precious raw food material for cooking soups. In this study, a lipidomics strategy using the techniques of solid-phase extraction (SPE) and hydrophilic interaction chromatography-tandem mass spectrometry (HILIC-QTOF/MS) was developed for extraction, visualization, and quantification of phospholipids in dried seahorses. The parameters of SPE were optimized, and 1 mL of sample and chloroform/methanol (1:2, v/v) were found to be the best loading volume and eluting solvent, respectively. Afterwards, each phospholipid class was successfully separated on a HILIC column and analyzed by mass spectrometry. A total of 50 phospholipid molecular species were identified and determined, including 15 phosphatidylcholines (PCs), 14 phosphatidylethanolamines (PEs), 12 phosphatidylinositols (PIs) and 9 phosphatidylserines (PSs). In comparison to previously methods, this strategy was robust and efficient in extraction, characterization, and determination of phospholipids. The dried seahorse was found to contain large amounts of polyunsaturated fatty acyl phospholipids which are beneficial to human health. PMID:27006218

  7. Determination of catecholamines by ion chromatography coupled to acidic potassium permanganate chemiluminescence detection

    Institute of Scientific and Technical Information of China (English)

    Hong Wei Wu; Mei Lan Chen; Dan Shou; Yan Zhu

    2012-01-01

    A simple,fast,sensitive,highly selective and eco-friendly analytical method for the determination of catecholamines in human urine by ion chromatography (IC) with chemiluminescence (CL) detection was described in this paper.Using 12 mmoi/L H2SO4 without any organic additive as eluent,three catecholamines including epinephrine (EP),norepinephrine (NE) and dopamine (DA)were well separated on a cation-exchange column.The CL detection was based on the reaction of analytes with acidic potassium permanganate in the presence of formaldehyde as an enhancer.The absence of methanol and acetonitrile in eluent made the proposed method more sensitive and eco-friendly.Under the optimal conditions,the linear range of the proposed method was in the range of 0.02-0.5 μg/mL.The limit of detection (LOD) was in the range of 0.6 and 5.1 μg/L.The relative standard deviations (RSD) for 0.1 μg/mL mixed standard solution were in the range of 0.8-1.9% (n =11).The method has been applied to the determination of catecholamines in human urine successfully.Excellent spiked recoveries were achieved for catecholamines ranged from 91.2% to 112.7%.

  8. Analysis of additives in dairy products by liquid chromatography coupled to quadrupole-orbitrap mass spectrometry.

    Science.gov (United States)

    Jia, Wei; Ling, Yun; Lin, Yuanhui; Chang, James; Chu, Xiaogang

    2014-04-01

    A new method combining QuEChERS with ultrahigh-performance liquid chromatography and electrospray ionization quadrupole Orbitrap high-resolution mass spectrometry (UHPLC/ESI Q-Orbitrap) was developed for the highly accurate and sensitive screening of 43 antioxidants, preservatives and synthetic sweeteners in dairy products. Response surface methodology was employed to optimize a quick, easy, cheap, effective, rugged, and safe (QuEChERS) sample preparation method for the determination of 42 different analytes in dairy products for the first time. After optimization, the maximum predicted recovery was 99.33% rate for aspartame under the optimized conditions of 10 mL acetionitrile, 1.52 g sodium acetate, 410 mg PSA and 404 mgC18. For the matrices studied, the recovery rates of the other 42 compounds ranged from 89.4% to 108.2%, with coefficient of variation 0.999. The limits of detection for the analytes are in the range 0.0001-3.6 μg kg(-1). This method has been successfully applied on screening of antioxidants, preservatives and synthetic sweeteners in commercial dairy product samples, and it is very useful for fast screening of different food additives. PMID:24607030

  9. Multi-mycotoxin analysis in dairy products by liquid chromatography coupled to quadrupole orbitrap mass spectrometry.

    Science.gov (United States)

    Jia, Wei; Chu, Xiaogang; Ling, Yun; Huang, Junrong; Chang, James

    2014-06-01

    A new analytical method was developed and validated for simultaneous analysis of 58 mycotoxins in dairy products. Response surface methodology was employed to optimize a quick, easy, cheap, effective, rugged, and safe (QuEChERS) sample preparation method. Ultrahigh-performance liquid chromatography and electrospray ionization quadrupole Orbitrap high-resolution mass spectrometry (UHPLC/ESI Q-Orbitrap) was used for the separation and detection of all the analytes. The method was validated by taking into consideration the guidelines specified in Commission Decision 2002/657/EC and 401/2006/EC. The extraction recoveries were in a range of 86.6-113.7%, with coefficient of variation 0.99. The limits of detection for the analytes are in the range 0.001-0.92 μg kg(-1). The repeatability was lower than 6.4%. This method has been successfully applied on screening of mycotoxins in commercial dairy product samples, and it is very useful for fast screening of different food contaminants. PMID:24794937

  10. Plasma jet desorption atomization-atomic fluorescence spectrometry and its application to mercury speciation by coupling with thin layer chromatography.

    Science.gov (United States)

    Liu, Zhifu; Zhu, Zhenli; Zheng, Hongtao; Hu, Shenghong

    2012-12-01

    A novel plasma jet desorption atomization (PJDA) source was developed for atomic fluorescence spectrometry (AFS) and coupled on line with thin layer chromatography (TLC) for mercury speciation. An argon dielectric barrier discharge plasma jet, which is generated inside a 300 μm quartz capillary, interacts directly with the sample being analyzed and is found to desorb and atomize surface mercury species rapidly. The effectiveness of this PJDA surface sampling technique was demonstrated by measuring AFS signals of inorganic Hg(2+), methylmercury (MeHg), and phenylmercury (PhHg) deposited directly on TLC plate. The detection limits of the proposed PJDA-AFS method for inorganic Hg(2+), MeHg, and PhHg were 0.51, 0.29, and 0.34 pg, respectively, and repeatability was 4.7%, 2.2%, and 4.3% for 10 pg Hg(2+), MeHg, and PhHg. The proposed PJDA-AFS was also successfully coupled to TLC for mercury speciation. Under optimized conditions, the measurements of mercury dithizonate (Hg-D), methylmercury dithizonate (MeHg-D), and phenylmercury dithizonate (PhHg-D) could be achieved within 3 min with detection limits as low as 8.7 pg. The combination of TLC with PJDA-AFS provides a simple, cost-effective, relatively high-throughput way for mercury speciation. PMID:23153091

  11. Determination of total phthalates in edible oils by high-performance liquid chromatography coupled with photodiode array detection.

    Science.gov (United States)

    Xie, Qilong; Sun, Dekui; Han, Yangying; Jia, Litao; Hou, Bo; Liu, Shuhui; Li, Debao

    2016-03-01

    The previously reported procedure for the determination of the total phthalate in fatty food involved the extraction of phthalates using chloroform/methanol followed by the removal of the solvents before alkaline hydrolysis requiring 20 h and derivatization of phthalic acid. In this study, a phase-transfer catalyst (tetrabutylammonium chloride) was used in the liquid-liquid heterogeneous hydrolysis of phthalates in oil matrix shortening the reaction time to within 25 min. The resulting phthalic acid in the hydrolysate was extracted by a novel molecular complex based dispersive liquid-liquid microextraction method coupled with back-extraction before high-performance liquid chromatography coupled with photodiode array detection. Under the optimal experimental conditions, the linearity of the method was in the range of 0.5-12 nmol/g with the correlation coefficients (r) >0.997. The detection limit (S/N = 3) was 0.11 nmol/g. Intraday and interday repeatability values expressed as relative standard deviation were 3.9 and 7.1%, respectively. The recovery rates ranged from 82.4 to 99.0%. The developed method was successfully applied for the analysis of total phthalate in seven edible oils. PMID:26695378

  12. Elemental labelling combined with liquid chromatography inductively coupled plasma mass spectrometry for quantification of biomolecules: A review

    International Nuclear Information System (INIS)

    Highlights: ► Survey of bio-analytical approaches utilizing biomolecule labelling. ► Detailed discussion of methodology and chemistry of elemental labelling. ► Biomedical and bio-analytical applications of elemental labelling. ► FI-ICP-MS and LC–ICP-MS for quantification of elemental labelled biomolecules. ► Review of selected applications. - Abstract: This article reviews novel quantification concepts where elemental labelling is combined with flow injection inductively coupled plasma mass spectrometry (FI-ICP-MS) or liquid chromatography inductively coupled plasma mass spectrometry (LC–ICP-MS), and employed for quantification of biomolecules such as proteins, peptides and related molecules in challenging sample matrices. In the first sections an overview on general aspects of biomolecule quantification, as well as of labelling will be presented emphasizing the potential, which lies in such methodological approaches. In this context, ICP-MS as detector provides high sensitivity, selectivity and robustness in biological samples and offers the capability for multiplexing and isotope dilution mass spectrometry (IDMS). Fundamental methodology of elemental labelling will be highlighted and analytical, as well as biomedical applications will be presented. A special focus will lie on established applications underlining benefits and bottlenecks of such approaches for the implementation in real life analysis. Key research made in this field will be summarized and a perspective for future developments including sophisticated and innovative applications will given.

  13. Separation, detection and characterization of nanomaterials in municipal wastewaters using hydrodynamic chromatography coupled to ICPMS and single particle ICPMS.

    Science.gov (United States)

    Proulx, Kim; Hadioui, Madjid; Wilkinson, Kevin J

    2016-07-01

    Engineered nanoparticles (ENP) are increasingly being incorporated into consumer products and reaching the environment at a growing rate. Unfortunately, few analytical techniques are available that allow the detection of ENP in complex environmental matrices. The major limitations with existing techniques are their relatively high detection limits and their inability to distinguish ENP from other chemical forms (e.g. ions, dissolved) or from natural colloids. Of the matrices that are considered to be a priority for method development, ENP are predicted to be found at relatively high concentrations in wastewaters and wastewater biosolids. In this paper, we demonstrate the capability of hydrodynamic chromatography (HDC) coupled to inductively coupled plasma mass spectrometry (ICPMS), in its classical and single particle modes (SP ICPMS), to identify ENP in wastewater influents and effluents. The paper first focuses on the detection of standard silver nanoparticles (Ag NP) and their mixtures, showing that significant dissolution of the Ag NP was likely to occur. For the Ag NP, detection limits of 0.03 μg L(-1) were found for the HDC ICPMS whereas 0.1 μg L(-1) was determined for the HDC SP ICPMS (based on results for the 80 nm Ag NP). In the second part of the paper, HDC ICPMS and HDC SP ICPMS were performed on some unspiked natural samples (wastewaters, river water). While nanosilver was below detection limits, it was possible to identify some (likely natural) Cu nanoparticles using the developed separation technology. PMID:26970748

  14. Fast quantification of endogenous carbohydrates in plasma using hydrophilic interaction liquid chromatography coupled with tandem mass spectrometry.

    Science.gov (United States)

    Zhu, Bangjie; Liu, Feng; Li, Xituo; Wang, Yan; Gu, Xue; Dai, Jieyu; Wang, Guiming; Cheng, Yu; Yan, Chao

    2015-01-01

    Endogenous carbohydrates in biosamples are frequently highlighted as the most differential metabolites in many metabolomics studies. A simple, fast, simultaneous quantitative method for 16 endogenous carbohydrates in plasma has been developed using hydrophilic interaction liquid chromatography coupled with tandem mass spectrometry. In order to quantify 16 endogenous carbohydrates in plasma, various conditions, including columns, chromatographic conditions, mass spectrometry conditions, and plasma preparation methods, were investigated. Different conditions in this quantified analysis were performed and optimized. The reproducibility, precision, recovery, matrix effect, and stability of the method were verified. The results indicated that a methanol/acetonitrile (50:50, v/v) mixture could effectively and reproducibly precipitate rat plasma proteins. Cold organic solvents coupled with vortex for 1 min and incubated at -20°C for 20 min were the most optimal conditions for protein precipitation and extraction. The results, according to the linearity, recovery, precision, matrix effect, and stability, showed that the method was satisfactory in the quantification of endogenous carbohydrates in rat plasma. The quantified analysis of endogenous carbohydrates in rat plasma performed excellently in terms of sensitivity, high throughput, and simple sample preparation, which met the requirement of quantification in specific expanded metabolomic studies after the global metabolic profiling research. PMID:25359182

  15. Application of the Reversed-phase Liquid Chromatography Coupled to Ion Trap Mass Spectrometry with Principal Components Analysis for Metabonomics Studies of Scutellarin in Rat Urine

    Institute of Scientific and Technical Information of China (English)

    Xiao Rong RAN; Sheng Zhu SI; Qiong Lin LIANG; Guo An LUO

    2006-01-01

    Metabonomics, a novel systemic approach, was applied to studies of Traditional Chinese Medicine scutellarin in rat urine. The liquid chromatography coupled with ion trap mass spectrometry combined with PCA was used in this paper. With this methodology, two potential metabolites of scutellarin were detected and the nine ions responsible for the gender variation and one ion for the dosage variation were found.

  16. Investigation of drugs of abuse and relevant metabolites in Dutch sewage water by liquid chromatography coupled to high resolution mass spectrometry

    NARCIS (Netherlands)

    L. Bijlsma; E. Emke; F. Hernández; P. de Voogt

    2012-01-01

    An extensive study on the presence of illicit drugs and pharmaceuticals with potential for abuse in sewage waters was made for the first time in the Netherlands. A total number of 24 target drugs were investigated in influent and effluent wastewater using liquid chromatography coupled to a high reso

  17. Speciation of arsenic(III)/arsenic(V) and selenium(IV)/ selenium(VI) using coupled ion chromatography - hydride generation atomic absorption spectrometry

    Science.gov (United States)

    Simple analytical methods have been developed to speciate inorganic arsenic and selenium in the ppb range using coupled ion chromatography-hydride generation atomic absorption spectrometry. Because of the differences in toxicity and adsorption behavior, determinations of the redox states arsenite A...

  18. Coupling Temperature Control with Electrochemically Modulated Liquid Chromatography: Fundamental Aspects and Applications

    Energy Technology Data Exchange (ETDEWEB)

    Lisa M. Ponton

    2004-12-19

    The primary focus of the doctoral research presented herein has been the integration of temperature control into electrochemically modulated liquid chromatography (EMLC). The combination of temperature control and the tunable characteristics of carbonaceous EMLC stationary phases have been invaluable in deciphering the subtleties of the retention mechanism. The effects of temperature and E{sub app} on the retention of several naphthalene disulfonates were therefore examined by the van' Hoff relationship. The results indicate that while the retention of both compounds is exothermic at levels comparable to that in many reversed-phase separations, the potential dependence of the separation is actually entropically affected in a manner paralleling that of several classical ion exchange systems. Furthermore, the retention of small inorganic anions at constant temperature also showed evidence of an ion exchange type of mechanism. While a more complete mechanistic description will come from examining the thermodynamics of retention for a wider variety of analytes, this research has laid the groundwork for full exploitation of temperature as a tool to develop retention rules for EMLC. Operating EMLC at elevated temperature and flow conditions has decreased analysis time and has enabled the separation of analytes not normally achievable on a carbon stationary phase. The separation of several aromatic sulfonates was achieved in less than 1 min, a reduction of analysis time by more than a factor of 20 as compared to room temperature separations. The use of higher operating temperatures also facilitated the separation of this mixture with an entirely aqueous mobile phase in less than 2 min. This methodology was extended to the difficult separation of polycyclic aromatic hydrocarbons on PGC. This study also brought to light the mechanistic implications of the unique retention behavior of these analytes through variations of the mobile phase composition.

  19. Determination of zearalenone content in cereals and feedstuffs by immunoaffinity column coupled with liquid chromatography.

    Science.gov (United States)

    Fazekas, B; Tar, A

    2001-01-01

    The zearalenone content of maize, wheat, barley, swine feed, and poultry feed samples was determined by immunoaffinity column cleanup followed by liquid chromatography (IAC-LC). Samples were extracted in methanol-water (8 + 2, v/v) solution. The filtered extract was diluted with distilled water and applied to immunoaffinity columns. Zearalenone was eluted with methanol, dried by evaporation, and dissolved in acetonitrile-water (3 + 7, v/v). Zearalenone was separated by isocratic elution of acetonitrile-water (50 + 50, v/v) on reversed-phase C18 column. The quantitative analysis was performed by fluorescence detector and confirmation was based on the UV spectrum obtained by a diode array detector. The mean recovery rate of zearalenone was 82-97% (RSD, 1.4-4.1%) on the original (single-use) immunoaffinity columns. The limit of detection of zearalenone by fluorescence was 10 ng/g at a signal-to-noise ratio of 10:1 and 30 ng/g by spectral confirmation in UV. A good correlation was found (R2 = 0.89) between the results obtained by IAC-LC and by the official AOAC-LC method. The specificity of the method was increased by using fluorescence detection in parallel with UV detection. This method was applicable to the determination of zearalenone content in cereals and other kinds of feedstuffs. Reusability of immunoaffinity columns was examined by washing with water after sample elution and allowing columns to stand for 24 h at room temperature. The zearalenone recovery rate of the regenerated columns varied between 79 and 95% (RSD, 3.2-6.3%). Columns can be regenerated at least 3 times without altering their performance and without affecting the results of repeated determinations. PMID:11601464

  20. Characterization of polysorbate 85, a nonionic surfactant, by liquid chromatography vs. ion mobility separation coupled with tandem mass spectrometry

    International Nuclear Information System (INIS)

    Graphical abstract: -- Highlights: •Liquid chromatography (LC) separates amphiphilic blends according to hydrophobicity. •Ion mobility (IM) spectrometry separates these blends based on molecular size/shape. •LC–MS provides the separation resolution needed for quantifying fatty acid content. •IM–MS enables rapid, solvent-free separation and the detection of trace components. •With either method, tandem MS allows to count the hydrophobic substituents. -- Abstract: Liquid chromatography (LC) and ion mobility (IM) separation have been coupled with mass spectrometry (MS) and tandem mass spectrometry (MS2) to characterize a commercially important nonionic surfactant, polysorbate 85. The constituents of this amphiphilic blend contained a sorbitan or isosorbide core that was chain extended with poly(ethylene oxide) (PEO) and partially esterified at the PEO termini with oleic acid or, to a lesser extent, other fatty acids. Using interactive LC in reverse-phase mode, the oligomers of the surfactant were separated according to their hydrophobicity/hydrophilicity balance. On the other hand, IM spectrometry dispersed the surfactant oligomers by their charge and collision cross section (i.e. size/shape). With either separation method, an increased number of fatty ester groups and/or lack of the polar sorbitan (or isosorbide) core led to higher retention/drift times, enabling the separation of isobaric species or species with superimposed isotope patterns, so that their ester content could be conclusively identified by MS2. LC–MS and IM–MS permitted the detection of several byproducts besides the major PEO-sorbitan oleate oligomers. LC–MS provides the separation resolution needed for quantitative determination of the degree of esterification. IM–MS, which minimizes analysis time and solvent use, is ideally suitable for a fast, qualitative survey of samples differing in their minor constituents or impurities

  1. Enhanced separation and characterization of deamidated peptides with RP-ERLIC-based multidimensional chromatography coupled with tandem mass spectrometry.

    Science.gov (United States)

    Hao, Piliang; Qian, Jingru; Dutta, Bamaprasad; Cheow, Esther Sok Hwee; Sim, Kae Hwan; Meng, Wei; Adav, Sunil S; Alpert, Andrew; Sze, Siu Kwan

    2012-03-01

    Deamidation of asparaginyl residues in proteins produces a mixture of asparaginyl, n-aspartyl, and isoaspartyl residues, which affects the proteins' structure, function, and stability. Thus, it is important to identify and quantify the products to evaluate the effects in biological systems. It is still a challenging task to distinguish between the n-Asp and isoAsp deamidation products in a proteome-wide analysis because of their similar physicochemical properties. The quantification of the isomeric deamidated peptides is also rather difficult because of their coelution/poor separation in reverse-phase liquid chromatography (RPLC). We here propose a RP-ERLIC-MS/MS approach for separating and quantifying on a proteome-wide scale the three products related to deamidation of the same peptide. The key to the method is the use of RPLC in the first dimensional separation and ERLIC (electrostatic repulsion-hydrophilic interaction chromatography) in the second, with direct online coupling to tandem MS. The coelution of the three deamidation-related peptides in RPLC is then an asset, as they are collected in the same fraction. They are then separated and identified in the second dimension with ERLIC, which separates peptides on the basis of both pI and GRAVY values. The coelution of the three products in RPLC and their efficient separation in ERLIC were validated using synthetic peptides, and the performance of ERLIC-MS/MS was tested using peptide mixtures from two proteins. Applying this sequence to rat liver tissue, we identified 302 unique N-deamidated peptides, of which 20 were identified via all three deamidation-related products and 70 of which were identified via two of them. PMID:22239700

  2. Characterization of polysorbate 85, a nonionic surfactant, by liquid chromatography vs. ion mobility separation coupled with tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Solak Erdem, Nilüfer; Alawani, Nadrah; Wesdemiotis, Chrys, E-mail: wesdemiotis@uakron.edu

    2014-01-15

    Graphical abstract: -- Highlights: •Liquid chromatography (LC) separates amphiphilic blends according to hydrophobicity. •Ion mobility (IM) spectrometry separates these blends based on molecular size/shape. •LC–MS provides the separation resolution needed for quantifying fatty acid content. •IM–MS enables rapid, solvent-free separation and the detection of trace components. •With either method, tandem MS allows to count the hydrophobic substituents. -- Abstract: Liquid chromatography (LC) and ion mobility (IM) separation have been coupled with mass spectrometry (MS) and tandem mass spectrometry (MS{sup 2}) to characterize a commercially important nonionic surfactant, polysorbate 85. The constituents of this amphiphilic blend contained a sorbitan or isosorbide core that was chain extended with poly(ethylene oxide) (PEO) and partially esterified at the PEO termini with oleic acid or, to a lesser extent, other fatty acids. Using interactive LC in reverse-phase mode, the oligomers of the surfactant were separated according to their hydrophobicity/hydrophilicity balance. On the other hand, IM spectrometry dispersed the surfactant oligomers by their charge and collision cross section (i.e. size/shape). With either separation method, an increased number of fatty ester groups and/or lack of the polar sorbitan (or isosorbide) core led to higher retention/drift times, enabling the separation of isobaric species or species with superimposed isotope patterns, so that their ester content could be conclusively identified by MS{sup 2}. LC–MS and IM–MS permitted the detection of several byproducts besides the major PEO-sorbitan oleate oligomers. LC–MS provides the separation resolution needed for quantitative determination of the degree of esterification. IM–MS, which minimizes analysis time and solvent use, is ideally suitable for a fast, qualitative survey of samples differing in their minor constituents or impurities.

  3. Fingerprint analysis of Ophiopogonis Radix by HPLC-UV-ELSD coupled with chemometrics methods%HPLC-UV-ELSD结合化学计量学方法研究麦冬的指纹图谱

    Institute of Scientific and Technical Information of China (English)

    李宁; 车彦云; 张梁; 张加余; 周渊; 姜勇; 屠鹏飞

    2013-01-01

    A new,simple and reliable method using HPLC-UV-ELSD was developed to generate the fingerprint of Ophiopogonis Radix.Homoisoflavonoids and steroidal saponins were determined simultaneously in a single run.A total of 27 Ophiopogonis Radix samples were analyzed,and 18 reference substances were used for the identification of the common peaks.The fingerprint was further analyzed by chemometrics methods including similarity analysis (SA),hierarchical clustering analysis (HCA) and principal component analysis (PCA).The results indicated that the combination of chromatographic fingerprint and chemometrics analysis could be used for the geographical differentiation and quality evaluation of Ophiopogonis Radix.%本文利用HPLC-UV-ELSD技术建立了一种新的麦冬化学指纹图谱分析方法.该方法简单、可靠,可同时对高异黄酮及甾体皂苷两类成分进行检测.在此基础上,对27批麦冬药材的指纹图谱进行了分析.采用18个对照品对部分共有峰进行了指认.采用相似度分析、聚类分析、主成分分析等化学计量学方法对指纹图谱进行了进一步分析.结果显示,色谱指纹图谱结合化学计量学方法可用于不同产地麦冬的鉴定及药材的质量评价.

  4. New method for caffeine quantification by planar chromatography coupled with electropray ionization mass spectrometry using stable isotope dilution analysis.

    Science.gov (United States)

    Aranda, Mario; Morlock, Gertrud

    2007-01-01

    A new high-performance thin-layer chromatography/electrospray ionization mass spectrometry (HPTLC/ESI-MS) method for the quantification of caffeine in pharmaceutical and energy drink samples was developed using stable isotope dilution analysis (SIDA). After sample preparation, samples and caffeine standard were applied on silica gel 60 F254 HPTLC plates and over-spotted with caffeine-d3 used for correction of the plunger positioning. After chromatography, densitometric detection was performed by UV absorption at 274 nm. The bands were then eluted by means of a plunger-based extractor into the ESI interface of a single-quadrupole mass spectrometer. For quantification by MS the [M+H]+ ions of caffeine and caffeine-d3 were recorded in the positive ion single ion monitoring (SIM) mode at m/z 195 and 198, respectively. The calibration showed a linear regression with a determination coefficient (R2) of 0.9998. The repeatability (RSD, n=6) in matrix wasbrand names were determined three times and ranged between RSD+/-0.68% and+/-2.64% (sample 1) and between+/-3.44% and+/-8.60% (sample 2). The method accuracy was evaluated by comparing the results obtained by HPTLC/SIDA-ESI-MS with those from the validated HPTLC/UV method. The results for pharmaceutical and energy drink samples were (ng/band) 99.82+/-3.75 and 338.09+/-4.87 by HPTLC/SIDA-ESI-MS and 104.74+/-1.51 and 334.86+/-5.63 by HPTLC/UV. According to the F-test (homogeneity of variances) and the t-test (comparison of means) the two methods show no significant difference. The detection and quantification limits were 75 and 250 microg L-1 (0.75 and 2.5 ng/band), respectively, which were a factor of 13 lower than those established for HPTLC/UV. The positioning error (RSD+/-6%) was calculated by comparing HPTLC/SIDA-ESI-MS with HPTLC/ESI-MS. However, using SIDA the positioning error was nullified. HPTLC/SIDA-ESI-MS was demonstrated to be a highly reliable method for the quantification of compounds by planar chromatography

  5. Quantification of neurotransmitters in mouse brain tissue by using liquid chromatography coupled electrospray tandem mass spectrometry.

    Science.gov (United States)

    Kim, Tae-Hyun; Choi, Juhee; Kim, Hyung-Gun; Kim, Hak Rim

    2014-01-01

    A simple and rapid liquid chromatography tandem mass spectrometry method has been developed for the determination of BH4, DA, 5-HT, NE, EP, Glu, and GABA in mouse brain using epsilon-acetamidocaproic acid and isotopically labeled neurotransmitters as internal standards. Proteins in the samples were precipitated by adding acetonitrile, and then the supernatants were separated by a Sepax Polar-Imidazole (2.1 mm × 100 mm, i.d., 3 μm) column by adding a mixture of 10 mM ammonium formate in acetonitrile/water (75 : 25, v/v, 300 μl/min) for BH4 and DA. To assay 5-HT, NE, EP, Glu, and GABA; a Luna 3 μ C18 (3.0 mm × 150 mm, i.d., 3 μm) column was used by adding a mixture of 1% formic acid in acetonitrile/water (20 : 80, v/v, 350 μl/min). The total chromatographic run time was 5.5 min. The method was validated for the analysis of samples. The calibration curve was linear between 10 and 2000 ng/g for BH4 (r(2) = 0.995) , 10 and 5000 ng/g for DA (r(2) = 0.997) , 20 and 10000 ng/g for 5-HT (r(2) = 0.994) , NE (r(2) = 0.993) , and EP (r(2) = 0.993) , and 0.2 and 200 μg/g for Glu (r(2) = 0.996) and GABA (r(2) = 0.999) in the mouse brain tissues. As stated above, LC-MS/MS results were obtained and established to be a useful tool for the quantitative analysis of BH4, DA, 5-HT, NE, EP, Glu, and GABA in the experimental rodent brain. PMID:25258696

  6. Vortex-assisted low density solvent liquid-liquid microextraction and salt-induced demulsification coupled to high performance liquid chromatography for the determination of five organophosphorus pesticide residues in fruits.

    Science.gov (United States)

    Seebunrueng, Ketsarin; Santaladchaiyakit, Yanawath; Srijaranai, Supalax

    2015-01-01

    A simple and rapid microextraction method, vortex-assisted low density solvent liquid-liquid microextraction and salt-induced demulsification (VLLME-SID) coupled to high performance liquid chromatography (HPLC) was developed for the determination of organophosphorus pesticide (OPP) residues in fruits. The studied OPPs were azinphos-methyl, parathion-methyl, fenitrothion, diazinon and chlorpyrifos. For VLLME-SID, a mixture of low density solvents (1-dodecanol and hexane) was used as the extraction solvent under vortex agitation for enhancing dispersion. After complete dispersion, the emulsion was formed and the OPPs were extracted into extraction solvent droplets. Then, the emulsion was quickly broken up into two clear phases after the addition of AlCl3 as a demulsifier. Centrifugation was not required in this procedure. Under the optimal conditions, high enrichment factors (180-282), low limit of detections (LODs) (0.05-1 ng mL(-1)) and good precision (RSD≤7% for retention time and peak area) were obtained. The proposed method was successfully applied to the analysis of OPP residues in fruit samples (watermelon, grape, and cantaloupe). The LODs for samples were in the range 0.0006-0.0015 mg kg(-1) which are below the established EU-MRLs (0.01-0.3 mg kg(-1)). Good recoveries were also obtained (80-104%). PMID:25476376

  7. Determination of Am and Cm in spent nuclear fuels by isotope dilution inductively coupled plasma mass spectrometry and isotope dilution thermal ionization mass spectrometry after separation by high-performance liquid chromatography

    International Nuclear Information System (INIS)

    Elemental and isotopic determination of americium and curium in spent nuclear fuels is necessary to validate neutronic calculation codes and for nuclear waste disposal purposes. Prior to mass spectrometric analysis, it is mandatory to perform separations in order to eliminate isobaric interferences between U, Pu, Am and Cm. In the spent fuels samples analyzed, a separation of U and Pu has been first realized with an anion-exchange resin. Then a rapid Am/Cm separation has been developed by high-performance liquid chromatography (HPLC) with an on-line detection using the Am and Cm α-emission. The influence of the different parameters on the chromatographic separation are described and discussed. Inductively coupled plasma mass spectrometry (ICP-MS) and thermal-ionization mass spectrometry (TIMS) have been used to measure the isotopic composition of U, Am and Cm and to determine the 241Am/238U and 244Cm/238U ratios with the double spike isotope dilution method. The measurement procedures and the accuracy and precision of the results obtained with a quadrupole ICP-MS on different spent fuels samples are discussed and compared with those obtained by TIMS, used as a reference technique. (orig.)

  8. Standardization of homocysteine on HPLC using DTT as reductant

    OpenAIRE

    Ashavaid, Tester F.; Eghlim, Farah F.; Shalia, Kavita K.; Nair, Kappiareth G.

    2003-01-01

    Determination of plasma total homocysteine by high-pressure liquid chromatography (HPLC) usually requires reduction of protein bound or free homocysteine-disulphides into thiols by a reducing agent and the liberated thiols are then derivatized by a fluorescent marker. In this study we have standardized the HPLC method for homocysteine measurement using dithiothreitol (DTT) as reductant.

  9. Qualitative and Quantitative Analysis of Lignan Constituents in Caulis Trachelospermi by HPLC-QTOF-MS and HPLC-UV

    Directory of Open Access Journals (Sweden)

    Xiao-Ting Liu

    2015-05-01

    Full Text Available A high-performance liquid chromatography coupled with quadrupole tandem time-of-flight mass (HPLC-QTOF-MS and ultraviolet spectrometry (HPLC-UV was established for simultaneous qualitative and quantitative analysis of the major chemical constituents in Caulis Trachelospermi, respectively. The analysis was performed on an Agilent Zorbax Eclipse Plus C18 column (4.6 mm × 150 mm, 5 μm using a binary gradient system of water and methanol, with ultraviolet absorption at 230 nm. Based on high-resolution ESI-MS/MS fragmentation behaviors of the reference standards, the characteristic cleavage patterns of lignano-9, 9'-lactones and lignano-8'-hydroxy-9, 9'-lactones were obtained. The results demonstrated that the characteristic fragmentation patterns are valuable for identifying and differentiating lignano-9,9'-lactones and lignano-8'-hydroxy-9,9'-lactones. As such, a total of 25 compounds in Caulis Trachelospermi were unambiguously or tentatively identified via comparisons with reference standards or literature. In addition, 14 dibenzylbutyrolatone lignans were simultaneously quantified in Caulis Trachelospermi by HPLC-UV method. The method is suitable for the qualitative and quantitative analyses of dibenzylbutyrolatone lignans in Caulis Trachelospermi.

  10. Towards silicon speciation in light petroleum products using gas chromatography coupled to inductively coupled plasma mass spectrometry equipped with a dynamic reaction cell

    Science.gov (United States)

    Chainet, Fabien; Lienemann, Charles-Philippe; Ponthus, Jeremie; Pécheyran, Christophe; Castro, Joaudimir; Tessier, Emmanuel; Donard, Olivier François Xavier

    2014-07-01

    Silicon speciation has recently gained interest in the oil and gas industry due to the significant poisoning problems caused by silicon on hydrotreatment catalysts. The poisoning effect clearly depends on the structure of the silicon species which must be determined and quantified. The hyphenation of gas chromatography (GC) coupled to inductively coupled plasma mass spectrometry (ICP-MS) allows a specific detection to determine the retention times of all silicon species. The aim of this work is to determine the retention indices of unknown silicon species to allow their characterization by a multi-technical approach in order to access to their chemical structure. The optimization of the dynamic reaction cell (DRC) of the ICP-MS using hydrogen as reactant gas successfully demonstrated the resolution of the interferences (14N14N+ and 12C16O+) initially present on 28Si. The linearity was excellent for silicon compounds and instrumental detection limits ranged from 20 to 140 μg of Si/kg depending on the response of the silicon compounds. A continuous release of silicon in the torch was observed most likely due to the use of a torch and an injector which was made of quartz. A non-universal response for silicon was observed and it was clearly necessary to use response coefficients to quantify silicon compounds. Known silicon compounds such as cyclic siloxanes (D3-D16) coming from PDMS degradation were confirmed. Furthermore, more than 10 new silicon species never characterized before in petroleum products were highlighted in polydimethylsiloxane (PDMS) degradation samples produced under thermal cracking of hydrocarbons. These silicon species mainly consisted of linear and cyclic structures containing reactive functions such as ethoxy, peroxide and hydroxy groups which can be able to react with the alumina surface and hence, poison the catalyst. This characterization will further allow the development of innovative solutions such as trapping silicon compounds or

  11. Survey of inorganic arsenic in marine animals and marine certified reference materials by anion exchange high-performance liquid chromatography-inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Sloth, Jens Jørgen; Larsen, Erik Huusfeldt; Julshamn, Kåre

    2005-01-01

    A method for the determination of inorganic arsenic in seafood samples using high-performance liquid chromatography-inductively coupled plasma mass spectrometry is described. The principle of the method relied on microwave-assisted alkaline dissolution of the sample, which at the same time oxidized...... arsenite [As(Ill)] to arsenate [As(V)], whereby inorganic arsenic could be determined as the single species As(V). Anion exchange chromatography using isocratic elution with aqueous ammonium carbonate as the mobile phase was used for the separation of As(V) from other coextracted organoarsenic compounds...

  12. Speciation of eight arsenic compounds in human urine by high performance liquid chromatography with inductively coupled plasma mass spectrometric detection using antimonate for internal chromatographic standardization

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Pritzl, G.; Hansen, S. H.

    1993-01-01

    Four anionic and four cationic arsenic compounds in urine were separated by anion- and cation-exchange high-performance liquid chromatography and detected by inductively coupled plasma mass spectrometry (ICP-MS) at m/z 75. The species were the anions arsenite, arsenate, monomethylarsonate and...... arsenate in urine but was stable after at least 4-fold dilution of the urine with water. Arsenite was unstable in both urine samples and standard mixtures when diluted with the basic (pH 10.3) mobile phase used for anion chromatography. This could not be prevented by adding ascorbic acid as antioxidant...

  13. Miniaturized GC/MS instrumentation for in situ measurements: micro gas chromatography coupled with miniature quadrupole array and paul ion trap mass spectrometers

    Science.gov (United States)

    Holland, P.; Chutjian, A.; Darrach, M.; Orient, O.

    2002-01-01

    Miniaturized chemical instrumentation is needed for in situ measurements in planetary exploration and other spaceflight applications where factors such as reduction in payload requirements and enhanced robustness are important. In response to this need, we are 'continuing to develop miniaturized GC/MS instrumentation which combines chemical separations by gas chromatography (GC) with mass spectrometry (MS) to provide positive identification of chemical compounds in complex mixtures of gases, such as those found in the International Space Station's cabin atmosphere. Our design approach utilizes micro gas chromatography components coupled with either a miniature quadrupole mass spectrometer array (QMSA) or compact, high-resolution Paul ion trap.

  14. Single-run HPLC/ESI-LITMS profiling of ginsenosides in plant extracts and ginseng based products.

    Science.gov (United States)

    Stavrianidi, Andrey; Rodin, Igor; Braun, Arkady; Stekolshchikova, Elena; Shpigun, Oleg

    2015-06-01

    A rapid single-run analytical approach suitable to achieve a comprehensive characterization of ginsenosides - the main bioactive compounds present in plant materials from Panax species and ginseng-based products - was developed. The method is based on high-performance liquid chromatography coupled with electrospray positive ionization linear ion trap mass spectrometry (HPLC/ESI-LITMS). The main ions in the ESI-LITMS spectra were attributed to molecular adducts with sodium and potassium and fragments corresponding to cleavage of the glycosidic bonds. The simplicity of the approach allows laborious sample preparation and sophisticated spectral information-dependent acquisition to be avoided, and provides an opportunity for rapid screening. The method may replace existing HPLC-DAD profiling approaches. The results of this study indicate that HPLC/ESI-LITMS is applicable for quality control purposes on processed products and allows the rapid and direct identification of ginsenosides in crude plant extracts. PMID:25355704

  15. An Inexpensive Digital Gradient Controller for HPLC.

    Science.gov (United States)

    Brady, James E.; Carr, Peter W.

    1983-01-01

    Use of gradient elution techniques in high performance liquid chromatography (HPLC) is often essential for direct separation of complex mixtures. Since most commercial controllers have features that are of marginal value for instructional purposes, a low-cost controller capable of illustrating essential features of gradient elution was developed.…

  16. Determination of diphenylether herbicides in water samples by solid-phase microextraction coupled to liquid chromatography.

    Science.gov (United States)

    Sheu, Hong-Li; Sung, Yu-Hsiang; Melwanki, Mahaveer B; Huang, Shang-Da

    2006-11-01

    Solid-phase microextraction (SPME) coupled to LC for the analysis of five diphenylether herbicides (aclonifen, bifenox, fluoroglycofen-ethyl, oxyfluorfen, and lactofen) is described. Various parameters of extraction of analytes onto the fiber (such as type of fiber, extraction time and temperature, pH, impact of salt and organic solute) and desorption from the fiber in the desorption chamber prior to separation (such as type and composition of desorption solvent, desorption mode, soaking time, and flush-out time) were studied and optimized. Four commercially available SPME fibers were studied. PDMS/divinylbenzene (PDMS/DVB, 60 microm) and carbowax/ templated resin (CW/TPR, 50 microm) fibers were selected due to better extraction efficiencies. Repeatability (RSD, 0.994), and detection limit (0.33-1.74 and 0.22-1.94 ng/mL, respectively, for PDMS/DVB and CW/TPR) were investigated. Relative recovery (81-104% for PDMS/DVB and 83-100% for CW/TPR fiber) values have also been calculated. The developed method was successfully applied to the analysis of river water and water collected from a vegetable garden. PMID:17313105

  17. Metal oxide affinity chromatography platform-polydopamine coupled functional two-dimensional titania graphene nanohybrid for phosphoproteome research.

    Science.gov (United States)

    Yan, Yinghua; Sun, Xueni; Deng, Chunhui; Li, Yan; Zhang, Xiangmin

    2014-05-01

    In this work, a facile route was initially developed for preparation of a novel metal oxide affinity chromatography (MOAC) material by grafting titania nanoparticles on polydopamine (PD)-coated graphene (denoted as G@PD@TiO2). In the first step, self-assemble polymerization of dopamine on graphene was performed in basic solution at room temperature, which not only offered the coupling linker between titania and graphene but also improved the hydrophilicity and biological compatibility of the nanohybrids. Thereafter, the titania nanoparticles were grafted on the surface of the PD-coated graphene via a simple hydrothermal treatment. The as-prepared G@PD@TiO2 nanohybrids exhibited high sensitivity (detection limit of 5 fmol) and high selectivity for phosphopeptides at a low molar ratio of phosphopeptides/nonphosphopeptides (1:1000). Moreover, the as-prepared nanohybrids were also investigated for enrichment of phosphopeptides from real biological samples (human serum and mouse brain). A total number of 556 phosphorylation sites were identified from the digest of mouse brain proteins, showing great potential in the practical application. PMID:24673251

  18. Profiling the Metabolism of Astragaloside IV by Ultra Performance Liquid Chromatography Coupled with Quadrupole/Time-of-Flight Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Xu-Dong Cheng

    2014-11-01

    Full Text Available Astragaloside IV is a compound isolated from the Traditional Chinese Medicine Astragalus membranaceus, that has been reported to have bioactivities against cardiovascular disease and kidney disease. There is limited information on the metabolism of astragaloside IV, which impedes comprehension of its biological actions and pharmacology. In the present study, an ultra-performance liquid chromatography coupled with quadrupole/time-of-flight mass spectrometry (UPLC-Q-TOF-MS/MS-based approach was developed to profile the metabolites of astragaloside IV in rat plasma, bile, urine and feces samples. Twenty-two major metabolites were detected. The major components found in plasma, bile, urine and feces included the parent chemical and phases I and II metabolites. The major metabolic reactions of astragaloside IV were hydrolysis, glucuronidation, sulfation and dehydrogenation. These results will help to improve understanding the metabolism and reveal the biotransformation profiling of astragaloside IV in vivo. The metabolic information obtained from our study will guide studies into the pharmacological activity and clinical safety of astragaloside IV.

  19. Volatile Fingerprint of Italian Populations of Orchids Using Solid Phase Microextraction and Gas Chromatography Coupled with Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Alessandra Manzo

    2014-06-01

    Full Text Available The volatile fraction of Ophrys sphegodes Mill. subsp. sphegodes, Ophrys bertolonii subsp. benacensis (Reisigl O. Danesch, E. Danasch & Ehrend. and Neotinea tridentata (Scop. R.M. Bateman, Pridgeon & M.W. Case, three orchid species with different pollinator attraction strategies, sampled in vivo and in situ, were evaluated by headspace solid phase microextraction coupled with gas-chromatography and mass spectrometry. The results were compared with the volatile compounds emitted by flowering plant samples picked from the same populations of orchid species. Hydrocarbons, aldehydes, alcohols and terpenes were the major constituents of “in vivo” orchid scents and some distinctive differences in volatile metabolite composition were observed between Ophrys and Neotinea species. Moreover, the odour bouquets of the picked flowering plant samples were different from the in vivo ones and in particular different proportions of the various terpenes and an increase of α-pinene were observed. In conclusion HS/SPME GCMS proved to be a suitable technique for analyzing and distinguishing the volatile fingerprint of different orchid species, sampled in vivo and in situ in a non-disruptive way, with potentially great advantages for ecophysiological studies of rare and endangered species.

  20. Determination of hexavalent chromium in sludge incinerator emissions using ion chromatography and inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Arar, E.J.; Long, S.E. (Technology Applications, Inc., Cincinnati, OH (United States)); Martin, T.D.; Gold, S. (Environmental Monitoring Systems Lab., Cincinnati, OH (United States))

    1992-10-01

    A unique approach is described using ion chromatography (IC) and inductively coupled plasma mass spectrometry (ICP-MS) for the determination of hexavalent chromium [Cr(VI)] in wastewater sludge incinerator emissions. Quartz fiber filters, spiked with an isotopically enriched ([sup 50]Cr or [sup 53]Cr) chromate salt, were used to collect emission particulates. The enriched Cr(VI) isotope was used to monitor the reduction of Cr(IV) during sample collection using a pseudo-first-order reaction model and to calculate the rate of deposition of native Cr(VI) on the filters. At the end of the sampling period, the Cr(VI) was extracted from the filters with 0.1 N sodium hydroxide and determined by IC using postcolumn derivatization with 1,5-diphenylcarbohydrazide. To determine the ratio of enriched Cr(VI) to the native Cr(VI) emitted from the incinerator, an additional aliquot of the sample extract was preconcentrated by IC and the isotopic composition of the Cr(VI) fraction determined by ICP-MS. 21 refs., 4 figs., 3 figs.

  1. Rapid determination of polysaccharides in BianTi Soft extract by spectrophotometry coupled with gas chromatography-mass spectrometry

    Directory of Open Access Journals (Sweden)

    Minxia Zheng

    2010-01-01

    Full Text Available A simple approach for the rapid determination of polysaccharides in BianTi Soft Extract using spectrophotometry coupled with gas chromatography-mass spectrometry (GC-MS was developed. The mixed standard solution composed of D-glucose, D-mannose, galactose and D-xylose in different proportions (1.00: 1.01: 0.12: 0.05 was prepared according to the monosaccharide composition analysis of the polysaccharides by GC-MS. The determination of polysaccharides by UV-Vis spectrophotometer was performed after 35-min color reaction, in which 1 ml 5% phenol and 4 ml sulfate was used. The assay of the method validation has shown that the method was stable, reliable and feasible. Furthermore, the proposed method was successfully applied in the preparation procedure of BianTi Soft Extract, selecting out optimal decoction conditions and suitable decoction container. It suggests that the convenient method could be useful for the quality control of BianTi Soft Extract. Meanwhile, it may be an alternative for polysaccharides determination of other formulations.

  2. Quality control evaluation of nutraceutical products from Ginkgo biloba using liquid chromatography coupled to high resolution mass spectrometry.

    Science.gov (United States)

    López-Gutiérrez, Noelia; Romero-González, Roberto; Martínez Vidal, José Luis; Garrido Frenich, Antonia

    2016-03-20

    Analysis of 11 commercial nutraceutical products obtained from ginkgo has been performed using ultra-high performance liquid chromatography coupled to single-stage Orbitrap high resolution mass spectrometry (UHPLC-Orbitrap-MS). The main phytochemicals present in these samples were detected and quantified, utilizing a database containing 65 compounds. Phytochemicals were extracted using a mixture of an aqueous solution of methanol:water (80:20, v/v) in two sequential solid-liquid extractions. Adequate validation parameters were obtained. The validated compounds exhibited suitable linearity with determination coefficients (R(2)) higher than 0.99, and intra and inter-day precision were lower than 17 and 22%, respectively. Limits of detection (LODs) and quantification (LOQs) were calculated, ranging from 2 to 10 μg L(-1), except for myricetin (LOD, 150 μg L(-1) and LOQ, 300 μg L(-1)). Results indicate that the amount of terpenoids greatly varies among samples, ranging from 1133 (C7) to 12706 mg kg(-1) (C11). This emphasizes the importance of improve quality control in ginkgo-based products. Moreover, retrospective analysis allowed the detection of some undesirable substances as ginkgolic acid in the samples evaluated. PMID:26808064

  3. Highly sensitive analysis of flavonoids by zwitterionic microemulsion electrokinetic chromatography coupled with light-emitting diode-induced fluorescence detection.

    Science.gov (United States)

    Cao, Wan; Hu, Shuai-Shuai; Li, Xing-Ying; Pang, Xiao-Qing; Cao, Jun; Ye, Li-Hong; Dai, Han-Bin; Liu, Xiao-Juan; Da, Jian-Hua; Chu, Chu

    2014-09-01

    A rapid zwitterionic microemulsion electrokinetic chromatography (ZI-MEEKC) approach coupled with light-emitting-diode-induced fluorescence (LED-IF, 480nm) detection was proposed for the analysis of flavonoids. In the optimization process, we systematically investigated the separation conditions, including the surfactants, cosurfactants, pH, buffers and fluorescence parameters. It was found that the baseline separation of the seven flavonoids was obtained in less than 5min with a running buffer consisting of 92.9% (v/v) 5mM sodium borate, 0.6% (w/v) ZI surfactant, 0.5% (w/v) ethyl acetate and 6.0% (w/v) 1-butanol. High sensitivity was obtained by the application of LED-IF detection. The limits of detection for seven flavonoids were in the range of 3.30×10(-8) to 2.15×10(-6)molL(-1) without derivatization. Ultimately, the detection method was successfully applied to the analysis of flavonoids in hawthorn plant and food products with satisfactory results. PMID:25047822

  4. Retrospective analysis of pesticide metabolites in urine using liquid chromatography coupled to high-resolution mass spectrometry.

    Science.gov (United States)

    López, Antonio; Dualde, Pablo; Yusà, Vicent; Coscollà, Clara

    2016-11-01

    A comprehensive retrospective analysis of pesticide metabolites in urine was developed, using liquid chromatography coupled to Orbitrap high-resolution mass spectrometry (UHPLC-HRMS) that includes both post-run target (suspect screening) and non-target screening. An accurate-mass database comprising 263 pesticide metabolites was built and used for the post-run screening analysis. For non-target analysis, a "fragmentation-degradation" relationship strategy was selected. The proposed methodology was applied to 49 real urine samples from pregnant women. In the post-target analysis 26 pesticide metabolites were tentatively identified, 8 of which (2-diethylamino-6-methyl-pyrimidinol; 3-ketocarbofuran; 4,6-dimethoxy-2-pyrimidinamine; 4-hydroxy-2-isporopyl-6-methylpyrimidine; diethyl malate; diethyl maleate; N-(2-Ethyl-6-methylphenyl)-2-hydroxyacetamide and propachlor oxanilic acid ) were confirmed using analytical standards. Likewise, one unknown degradation product, methyl-N-phenylcarbamate was elucidated in the non-target screening. Finally, the real urine samples were grouped according to their origin applying a metabolomic approach. PMID:27591649

  5. Retrospective screening of pesticide metabolites in ambient air using liquid chromatography coupled to high-resolution mass spectrometry.

    Science.gov (United States)

    López, Antonio; Yusà, Vicent; Millet, Maurice; Coscollà, Clara

    2016-04-01

    A new methodology for the retrospective screening of pesticide metabolites in ambient air was developed, using liquid chromatography coupled to Orbitrap high-resolution mass spectrometry (UHPLC-HRMS), including two systematic workflows (i) post-run target screening (suspect screening) and (ii) non-target screening. An accurate-mass database was built and used for the post-run screening analysis. The database contained 240 pesticide metabolites found in different matrixes such as air, soil, water, plants, animals and humans. For non-target analysis, a "fragmentation-degradation" relationship strategy was selected. The proposed methodology was applied to 31 air samples (PM10) collected in the Valencian Region (Spain). In the post-target analysis 34 metabolites were identified, of which 11 (3-ketocarburan, carbofuran-7-phenol, carbendazim, desmethylisoproturon, ethiofencarb-sulfoxide, malaoxon, methiocarb-sulfoxide, N-(2-ethyl-6-methylphenyl)-L-alanine, omethoate, 2-hydroxy-terbuthylazine, and THPAM) were confirmed using analytical standards. The semiquantitative estimated concentration ranged between 6.78 and 198.31 pg m(-3). Likewise, two unknown degradation products of malaoxon and fenhexamid were elucidated in the non-target screening. PMID:26838378

  6. Rapid Determination of Clenbuterol in Pork by Direct Immersion Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Ye, Diru; Wu, Susu; Xu, Jianqiao; Jiang, Ruifen; Zhu, Fang; Ouyang, Gangfeng

    2016-02-01

    Direct immersion solid-phase microextraction (DI-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) was developed for rapid analysis of clenbuterol in pork for the first time. In this work, a low-cost homemade 44 µm polydimethylsiloxane (PDMS) SPME fiber was employed to extract clenbuterol in pork. After extraction, derivatization was performed by suspending the fiber in the headspace of the 2 mL sample vial saturated with a vapor of 100 µL hexamethyldisilazane. Lastly, the fiber was directly introduced to GC-MS for analysis. All parameters that influenced absorption (extraction time), derivatization (derivatization reagent, time and temperature) and desorption (desorption time) were optimized. Under optimized conditions, the method offered a wide linear range (10-1000 ng g(-1)) and a low detection limit (3.6 ng g(-1)). Finally, the method was successfully applied in the analysis of pork from the market, and recoveries of the method for spiked pork were 97.4-105.7%. Compared with the traditional solvent extraction method, the proposed method was much cheaper and fast. PMID:26306572

  7. Fast carbohydrate analysis via liquid chromatography coupled with ultra violet and electrospray ionization ion trap detection in 96-well format.

    Science.gov (United States)

    Rühmann, Broder; Schmid, Jochen; Sieber, Volker

    2014-07-11

    A fast carbohydrate screening platform processible in 96-well format is described. The method is suitable for the determination of various carbohydrates out of complex mixtures as obtained by acidic hydrolysis of carbohydrates polymers. The chromatographic conditions for an efficient separation (12min) and the derivatization process with 1-phenyl-3-methyl-5-pyrazolone (PMP) were optimized for high resolution separation and simultaneous determination of deoxy-, amino-, anhydro-sugars as well as hexoses, pentoses, dimers, uronic acids and degradation products like furfural and hydroxymethylfurfural (HMF). The potential to quantify with UV- and MS-detector in the same range has been demonstrated for 20 different compounds. Finally, the matrix effects of the hydrolysis were positively evaluated. The micro scale hydrolysis and PMP-derivatization without any extraction or drying steps, both in 96-well format, result in a fast and intuitive sample preparation. In combination with a fast liquid chromatography coupled to UV and electrospray ionization ion trap detection (LC-UV-ESI-MS/MS) for the qualification and quantification of various sugars, dimers and degradation products, this method shows great performance in carbohydrate analysis. PMID:24861788

  8. Investigation of pharmaceuticals in processed animal by-products by liquid chromatography coupled to high-resolution mass spectrometry.

    Science.gov (United States)

    Nácher-Mestre, Jaime; Ibáñez, María; Serrano, Roque; Boix, Clara; Bijlsma, Lubertus; Lunestad, Bjørn Tore; Hannisdal, Rita; Alm, Martin; Hernández, Félix; Berntssen, Marc H G

    2016-07-01

    There is an on-going trend for developing more sustainable salmon feed in which traditionally applied marine feed ingredients are replaced with alternatives. Processed animal products (PAPs) have been re-authorized as novel high quality protein ingredients in 2013. These PAPs may harbor undesirable substances such as pharmaceuticals and metabolites which are not previously associated with salmon farming, but might cause a potential risk for feed and food safety. To control these contaminants, an analytical strategy based on a generic extraction followed by ultra-high performance liquid chromatography coupled to high resolution mass spectrometry (UHPLC-HRMS) using quadrupole time-of-flight mass analyzer (QTOF MS) was applied for wide scope screening. Quality control samples, consisting of PAP commodities spiked at 0.02, 0.1 and 0.2 mg/kg with 150 analytes, were injected in every sample batch to verify the overall method performance. The methodology was applied to 19 commercially available PAP samples from six different types of matrices from the EU animal rendering industry. This strategy allows assessing possible emergent risk exposition of the salmon farming industry to 1005 undesirables, including pharmaceuticals, several dyes and relevant metabolites. PMID:27058915

  9. Medicinal cannabis: Principal cannabinoids concentration and their stability evaluated by a high performance liquid chromatography coupled to diode array and quadrupole time of flight mass spectrometry method.

    Science.gov (United States)

    Citti, Cinzia; Ciccarella, Giuseppe; Braghiroli, Daniela; Parenti, Carlo; Vandelli, Maria Angela; Cannazza, Giuseppe

    2016-09-01

    In the last few years, there has been a boost in the use of cannabis-based extracts for medicinal purposes, although their preparation procedure has not been standardized but rather decided by the individual pharmacists. The present work describes the development of a simple and rapid high performance liquid chromatography method with UV detection (HPLC-UV) for the qualitative and quantitative determination of the principal cannabinoids (CBD-A, CBD, CBN, THC and THC-A) that could be applied to all cannabis-based medicinal extracts (CMEs) and easily performed by a pharmacist. In order to evaluate the identity and purity of the analytes, a high-resolution mass spectrometry (HPLC-ESI-QTOF) analysis was also carried out. Full method validation has been performed in terms of specificity, selectivity, linearity, recovery, dilution integrity and thermal stability. Moreover, the influence of the solvent (ethyl alcohol and olive oil) was evaluated on cannabinoids degradation rate. An alternative extraction method has then been proposed in order to preserve cannabis monoterpene component in final CMEs. PMID:27268223

  10. Comparison of copper labeling followed by liquid chromatography-inductively coupled plasma mass spectrometry and immunochemical assays for serum hepcidin-25 determination.

    Science.gov (United States)

    Konz, Tobias; Alonso-García, Javier; Montes-Bayón, María; Sanz-Medel, Alfredo

    2013-10-17

    Hepcidin-25 has been defined as the key biomarker in iron metabolism. This peptide binds to the iron transporter ferroportin to cause its degradation. Therefore, the need for specific, accurate and precise methods for the quantification of hepcidin-25 in biological fluids is dramatically increasing. In this regard, the use of rapid immunochemical methods that provide low limit of quantification is desired for routine clinical use. However, such fast methodologies should be first analytically evaluated and compared with alternative strategies to check for their advantages and limitations. Here we compare the use of a commercial immunochemical assay for hepcidin determination with a novel analytical approach based on Cu-labeling of the peptide followed by Cu determination using liquid chromatography (HPLC) and plasma mass spectrometry (ICP-MS). The figures of merit of both systems reveal similar analytical characteristics and both seem to be adequate for the determination of the peptide at biologically relevant concentrations in human serum samples. The analysis of a larger number of samples (n=50) by both techniques showed a good agreement in the concentrations found. Such finding permits to address the hepcidin recovery in the sample preparation procedure necessary for the HPLC-ICP-MS analysis in human serum that turn out to be 76-85%. Additionally, limitations due to cross-reactivity issues of the ELISA method could be addressed in some of the samples by using LC-ICP-MS and were confirmed by LC-Electrospray-MS. PMID:24091368

  11. Determination of eight artificial sweeteners and common Stevia rebaudiana glycosides in non-alcoholic and alcoholic beverages by reversed-phase liquid chromatography coupled with tandem mass spectrometry.

    Science.gov (United States)

    Kubica, Paweł; Namieśnik, Jacek; Wasik, Andrzej

    2015-02-01

    The method for the determination of acesulfame-K, saccharine, cyclamate, aspartame, sucralose, alitame, neohesperidin dihydrochalcone, neotame and five common steviol glycosides (rebaudioside A, rebaudioside C, steviol, steviolbioside and stevioside) in soft and alcoholic beverages was developed using high-performance liquid chromatography and tandem mass spectrometry with electrospray ionisation (HPLC-ESI-MS/MS). To the best of our knowledge, this is the first work that presents an HPLC-ESI-MS/MS method which allows for the simultaneous determination of all EU-authorised high-potency sweeteners (thaumatin being the only exception) in one analytical run. The minimalistic sample preparation procedure consisted of only two operations; dilution and centrifugation. Linearity, limits of detection and quantitation, repeatability, and trueness of the method were evaluated. The obtained recoveries at three tested concentration levels varied from 97.0 to 105.7%, with relative standard deviations lower than 4.1%. The proposed method was successfully applied for the determination of sweeteners in 24 samples of different soft and alcoholic drinks. PMID:25471292

  12. Alcohol and metal determination in alcoholic beverages through high-temperature liquid-chromatography coupled to an inductively coupled plasma atomic emission spectrometer.

    Science.gov (United States)

    Terol, Amanda; Paredes, Eduardo; Maestre, Salvador E; Prats, Soledad; Todolí, José L

    2011-06-01

    In the present work, an inductively coupled plasma atomic emission spectrometry (ICP-AES) system was used as a high temperature liquid chromatography (HTLC) detector for the determination of alcohols and metals in beverages. For the sake of comparison, a refractive index (RI) detector was also employed for the first time to detect alcohols with HTLC. The organic compounds studied were methanol, ethanol, propan-1-ol and butan-1-ol (in the 10-125 mg/L concentration range) and the elements tested were magnesium, aluminum, copper, manganese and barium at concentrations included between roughly 0.01 and 80 mg/L. Column heating temperatures ranged from 80 to 175 °C and the optimum ones in terms of peak resolution, sensitivity and column lifetime were 125 and 100 °C for the HTLC-RI and HTLC-ICP-AES couplings, respectively. The HTLC-ICP-AES interface design (i.e., spray chamber design and nebulizer type used) was studied and it was found that a single pass spray chamber provided about 2 times higher sensitivities than a cyclonic conventional design. Comparatively speaking, limits of detection for alcohols were of the same order for the two evaluated detection systems (from 5 to 25 mg/L). In contrast, unlike RI, ICP-AES provided information about the content of both organic and inorganic species. Furthermore, temperature programming was applied to shorten the analysis time and it was verified that ICP-AES was less sensitive to temperature changes and modifications in the analyte chemical nature than the RI detector. Both detectors were successfully applied to the determination of short chain alcohols in several beverages such as muscatel, pacharan, punch, vermouth and two different brands of whiskeys (from 10 to 40 g of ethanol/100 g of sample). The results of the inorganic elements studied by HTLC-ICP-AES were compared with those obtained using inductively coupled plasma mass spectrometry (ICP-MS) obtaining good agreement between them. Recoveries found for spiked samples

  13. Characterisation of Phenolic Compounds in South African Plum Fruits (Prunus salicina Lindl.) using HPLC Coupled with Diode-Array, Fluorescence, Mass Spectrometry and On-Line Antioxidant Detection

    OpenAIRE

    Dalene de Beer; Elizabeth Joubert; Alet Venter

    2013-01-01

    Phenolic compounds are abundant secondary metabolites in plums, with potential health benefits believed to be due to their antioxidant activity, amongst others. Phenolic characterisation of South African Prunus salicina Lindl. plums is necessary to fully evaluate their potential health benefits. An HPLC method using diode-array detection (DAD) for quantification of phenolic compounds was improved and fluorescence detection (FLD) was added for quantification of flavan-3-ols. Validation of the ...

  14. Quantification of ethylenediamine-N,N'-bis(hydroxysulfophenylacetic) acid regioisomers and structural characterisation of its related polycondensation products by porous graphitic carbon high-performance liquid chromatography coupled to electrospray tandem mass spectrometry.

    Science.gov (United States)

    Biasone, Alessandro; Cianci, Giusto; Di Tommaso, Donata; Piaggesi, Alberto; D'Alessandro, Nicola

    2013-10-18

    Among the commercial ethylenediamine-N,N'-bis(2-hydroxy)phenylacetic acid/iron(III) derivatives, ethylenediamine-N,N'-bis(2-hydroxy-5-sulphophenylacetic) acid/iron(III) (EDDHSA/Fe) represents one of the promising chelates for the treatment of chlorotic plants. Industrial synthesis of EDDHSA/Fe leads to relevant amounts of o,o-EDDHSA condensation products (o,o-EDDHSAcps) and other secondary products that might have important relevance from the agronomic point of view. However, their chemical structures have remained unknown to date. Analysis of iron complexes by ion-pair reversed-phase chromatography, coupled with electrospray tandem mass spectrometry revealed the presence of the meso-o,o-EDDHSA/Fe, rac-o,o-EDDHSA/Fe, o,p-EDDHSA/Fe regioisomers, the hydroxyl derivative of o,o-EDDHSA/Fe, and the three main EDDHSA condensation products chelating the iron(III) (EDDHSAcps/nFe). However, the chromatographic peaks of EDDHSAcps/Fe are not well resolved due to the large numbers of stereoisomers and the poor efficiency of the ion-pair reversed-phase separation method. An alternative chromatographic method is based on porous graphitic carbon (PGC) separation after pre-column decomplexation of the chelates with trifluoracetic acid, which was developed to allow detection of EDDHSA stereo/regioisomers, EDDHSAcps, and low-molecular-weight by-products. This extensive PGC-HPLC-ESI-MS/MS investigation provides quantitative determination of meso-o,o-EDDHSA, rac-o,o-EDDHSA and o,p-EDDHSA, in addition to characterisation of EDDHSAcps and the low-molecular-weight by-products. PGC separation coupled to a triple quadrupole ESI-MS detector allowed characterisation of free ligands using collision-induced dissociation experiments in positive and negative ionisation mode, providing comparative evaluation of EDDHSAcps in three commercial samples. For detection, the PGC-HPLC-ESI-MS/MS is the best method according to the limit of quantification and limit of detection (picomolar and sub

  15. Toxin profile of Alexandrium catenella from the Chilean coast as determined by liquid chromatography with fluorescence detection and liquid chromatography coupled with tandem mass spectrometry

    OpenAIRE

    Krock, Bernd; Seguel, Carmen Gloria; Allan D. Cembella

    2007-01-01

    The profile of tetrahydropurine neurotoxins associated with paralytic shellfish poisoning (PSP) was determined from a Chilean strain of the marine dinoflagellate Alexandrium catenella. The toxin composition was compared with that of toxic shellfish, presumably contaminated by natural blooms of A. catenella from the same region in southern Chile. Ion pair-liquid chromatography with post-column derivatization and fluorescence detection (LC-FD) was employed for relative quantitative analysis of ...

  16. Development of a method for screening spill and leakage of antibiotics on surfaces based on wipe sampling and HPLC-MS/MS analysis

    OpenAIRE

    Nygren, Olle; Lindahl, Roger

    2011-01-01

    A screening method for determination of spill and leakage of 12 different antibiotic substances has been developed. The method is based on wipe sampling where the sampling procedure has been simplified for screening purposes. After sample processing, the antibiotic substances are determined by liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS). Twelve antibiotic substances can be determined in the screening method: Cefadroxil, Cefalexin, Ciprofloxacin, Demeclocyklin HCl, D...

  17. Changes in color-related compounds in tomato fruit exocarp and mesocarp during ripening using HPLC-APcI+-mass Spectrometry

    OpenAIRE

    Carrillo-López, A.; Yahia, E.M.

    2012-01-01

    Tomato is an important agricultural crop world-wide. Their pigments are very important in many ways. They have been associated with health benefits such as lowering the risk of some chronic diseases. Quantification of chlorophylls by spectrophotometry and Identification of carotenoids using liquid chromatography coupled to mass spectrometry, and quantification by HPLC-DAD was carried out in the exocarp and mesocarp of tomato fruit during 6 different ripeness stages (mature-green, breakers, tu...

  18. Simultaneous determination of iridoid glycosides, phenethylalcohol glycosides and furfural derivatives in Rehmanniae Radix by high performance liquid chromatography coupled with triple-quadrupole mass spectrometry

    DEFF Research Database (Denmark)

    Xu, Jun; Wu, Jie; Zhu, Ling-Ying;

    2012-01-01

    In this study, a sensitive and selective method for simultaneously quantifying eight major components (four iridoid glycosides, three phenethylalcohol glycosides and one furfural derivative) of Rehmanniae Radix by high performance liquid chromatography coupled with triple-quadrupole mass spectrom......In this study, a sensitive and selective method for simultaneously quantifying eight major components (four iridoid glycosides, three phenethylalcohol glycosides and one furfural derivative) of Rehmanniae Radix by high performance liquid chromatography coupled with triple-quadrupole mass...... was validated in terms of linearity, sensitivity, precision, accuracy and stability, and successfully applied to determine the contents of the eight analytes in different batches of raw and processed Rehmanniae Radix, which confirmed that the established method was reliable and useful for “holistic” quality...... evaluation of Rehmanniae Radix. The quantitative results indicated that the quality of commercial raw or processed Rehmanniae Radix was remarkably inconsistent....

  19. Liquid chromatography coupled to on-line post column derivatization for the determination of organic compounds: A review on instrumentation and chemistries

    International Nuclear Information System (INIS)

    Graphical abstract: -- Highlights: •Review on liquid chromatography coupled to post-column derivatization. •Overview of instrumentation for post-column derivatization. •Post-column chemistries for analysis of organic compounds. -- Abstract: Analytical derivatization either in pre or post column modes is one of the most widely used sample pretreatment techniques coupled to liquid chromatography. In the present review article we selected to discuss the post column derivatization mode for the analysis of organic compounds. The first part of the review focuses to the instrumentation of post-column setups including not only fundamental components such as pumps and reactors but also less common parts such as static mixers and back-pressure regulators; the second part of the article discusses the most popular “chemistries” that are involved in post column applications, including reagent-less approaches and new sensing platforms such as the popular gold nanoparticles. Some representative recent applications are also presented as tables

  20. Towards silicon speciation in light petroleum products using gas chromatography coupled to inductively coupled plasma mass spectrometry equipped with a dynamic reaction cell

    Energy Technology Data Exchange (ETDEWEB)

    Chainet, Fabien, E-mail: fabien.chainet@ifpen.fr [IFP Energies nouvelles, Rond-point de l' échangeur de Solaize, BP 3, 69360 Solaize (France); Lienemann, Charles-Philippe; Ponthus, Jeremie [IFP Energies nouvelles, Rond-point de l' échangeur de Solaize, BP 3, 69360 Solaize (France); Pécheyran, Christophe; Castro, Joaudimir; Tessier, Emmanuel; Donard, Olivier François Xavier [LCABIE-IPREM, UMR 5254, CNRS-UPPA, Helioparc, 2 av. Pr. Angot, 64053 Pau (France)

    2014-07-01

    Silicon speciation has recently gained interest in the oil and gas industry due to the significant poisoning problems caused by silicon on hydrotreatment catalysts. The poisoning effect clearly depends on the structure of the silicon species which must be determined and quantified. The hyphenation of gas chromatography (GC) coupled to inductively coupled plasma mass spectrometry (ICP-MS) allows a specific detection to determine the retention times of all silicon species. The aim of this work is to determine the retention indices of unknown silicon species to allow their characterization by a multi-technical approach in order to access to their chemical structure. The optimization of the dynamic reaction cell (DRC) of the ICP-MS using hydrogen as reactant gas successfully demonstrated the resolution of the interferences ({sup 14}N{sup 14}N{sup +} and {sup 12}C{sup 16}O{sup +}) initially present on {sup 28}Si. The linearity was excellent for silicon compounds and instrumental detection limits ranged from 20 to 140 μg of Si/kg depending on the response of the silicon compounds. A continuous release of silicon in the torch was observed most likely due to the use of a torch and an injector which was made of quartz. A non-universal response for silicon was observed and it was clearly necessary to use response coefficients to quantify silicon compounds. Known silicon compounds such as cyclic siloxanes (D{sub 3}–D{sub 16}) coming from PDMS degradation were confirmed. Furthermore, more than 10 new silicon species never characterized before in petroleum products were highlighted in polydimethylsiloxane (PDMS) degradation samples produced under thermal cracking of hydrocarbons. These silicon species mainly consisted of linear and cyclic structures containing reactive functions such as ethoxy, peroxide and hydroxy groups which can be able to react with the alumina surface and hence, poison the catalyst. This characterization will further allow the development of innovative

  1. Development of an analytical method for the determination of polybrominated diphenyl ethers in sewage sludge by the use of gas chromatography coupled to inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Novak, Petra; Zuliani, Tea; Milačič, Radmila; Ščančar, Janez

    2016-04-01

    Polybrominated diphenyl ethers (PBDEs) are flame retardants. As a consequence of their widespread use, they have been released into the environment. PBDEs are lipophilic organic contaminants that enter wastewater treatment plants (WWTPs) from urban, agricultural and industrial discharges. Because of their low aqueous solubility and resistance to biodegradation, up to 90% of the PBDEs are accumulated in the sewage sludge during the wastewater treatment. To assess the possibilities for sludge re-use, a reliable determination of the concentrations of these PBDEs is of crucial importance. Six PBDE congeners (BDE 28, BDE 47, BDE 99, BDE 100, BDE 153 and BDE 154) are listed as priority substances under the EU Water Framework Directive. In the present work a simple analytical method with minimal sample-preparation steps was developed for a sensitive and reliable determination of the six PBDEs in sewage sludge by the use of gas chromatography coupled to inductively coupled plasma mass spectrometry (GC-ICP-MS). For this purpose an extraction procedure was optimised. Different extracting agents (methanol (MeOH), acetic acid (AcOH)/MeOH mixture (3:1) and 0.1 mol L(-1) hydrochloric acid (HCl) in MeOH) followed by the addition of a Tris-citrate buffer (co-extracting agent) and iso-octane were applied under different modes of extraction (mechanical shaking, microwave- and ultrasound-assisted extraction). Mechanical shaking or the microwave-assisted extraction of sewage sludge with 0.1 mol L(-1) HCl in MeOH and the subsequent addition of the Tris-citrate buffer and the iso-octane extracted the PBDEs from the complex sludge matrix most effectively. However, due to easier sample manipulation during the extraction step, mechanical shaking was used. The PBDEs in the organic phase were quantified with GC-ICP-MS by applying a standard addition calibration method. The spike recovery test (recoveries between 95 and 104%) and comparative analyses with the species-specific isotope

  2. Towards silicon speciation in light petroleum products using gas chromatography coupled to inductively coupled plasma mass spectrometry equipped with a dynamic reaction cell

    International Nuclear Information System (INIS)

    Silicon speciation has recently gained interest in the oil and gas industry due to the significant poisoning problems caused by silicon on hydrotreatment catalysts. The poisoning effect clearly depends on the structure of the silicon species which must be determined and quantified. The hyphenation of gas chromatography (GC) coupled to inductively coupled plasma mass spectrometry (ICP-MS) allows a specific detection to determine the retention times of all silicon species. The aim of this work is to determine the retention indices of unknown silicon species to allow their characterization by a multi-technical approach in order to access to their chemical structure. The optimization of the dynamic reaction cell (DRC) of the ICP-MS using hydrogen as reactant gas successfully demonstrated the resolution of the interferences (14N14N+ and 12C16O+) initially present on 28Si. The linearity was excellent for silicon compounds and instrumental detection limits ranged from 20 to 140 μg of Si/kg depending on the response of the silicon compounds. A continuous release of silicon in the torch was observed most likely due to the use of a torch and an injector which was made of quartz. A non-universal response for silicon was observed and it was clearly necessary to use response coefficients to quantify silicon compounds. Known silicon compounds such as cyclic siloxanes (D3–D16) coming from PDMS degradation were confirmed. Furthermore, more than 10 new silicon species never characterized before in petroleum products were highlighted in polydimethylsiloxane (PDMS) degradation samples produced under thermal cracking of hydrocarbons. These silicon species mainly consisted of linear and cyclic structures containing reactive functions such as ethoxy, peroxide and hydroxy groups which can be able to react with the alumina surface and hence, poison the catalyst. This characterization will further allow the development of innovative solutions such as trapping silicon compounds or

  3. An HPLC-ICP-MS technique for determination of cadmium–phytochelatins in genetically modified Arabidopsis thaliana

    OpenAIRE

    Sadi, Baki B.M.; Vonderheide, Anne P.; Gong, Ji-Ming; Schroeder, Julian I; Shann, Jodi R.; Caruso, Joseph A

    2007-01-01

    A reversed-phase high-performance liquid chromatographic technique was developed to separate cadmium–phytochelatin complexes (Cd-PC2, Cd-PC3, and Cd-PC4) of interest in the plant Arapidopsis thaliana. High-performance liquid chromatography (HPLC) was coupled to an inductively coupled plasma mass spectrometric (ICP-MS) system with some modification to the interface. This was done in order to sustain the plasma with optimum sensitivity for cadmium detection in the presence of the high methanol ...

  4. Usefulness of pyrolysis coupled to gas chromatography/mass spectrometry for evaluating the reproducibility of commercial samples of Cymbopogon citratus Stapf., Poaceae

    OpenAIRE

    Eduardo J. Oliveira; Enrique D. A. Alvarez; Naiana G. P. B. Lima; Rui O. Macedo

    2010-01-01

    The usefulness of pyrolysis coupled to gas chromatography/mass spectrometry (Py-GC/MS) to evaluate the identity and reproducibility of different brands and batches of commercially available samples of Cymbopogon citratus Stapf (sold as tea) was investigated. Samples of the vegetable material were extracted using hexane and the extract was pyrolysed at 450 ºC using a vertical microfurnace pyrolyser interfaced directly with a gas chromatograph/mass spectrometer operated using electron impact io...

  5. Non-target screening of organic contaminants in marine salts by gas chromatography coupled to high-resolution time-of-flight mass spectrometry

    OpenAIRE

    Serrano, Roque; Nácher-Mestre, Jaime; Portolés-Nicolau, Tania; Amat, Francisco; Hernández Hernández, Félix

    2011-01-01

    Gas chromatography coupled to time-of-flight mass spectrometry (GC-TOF MS) has been applied to characterize the organic pollution pattern of marine salt samples collected in saltworks from the Spanish Mediterranean coast. After dissolving the samples in water, a solid-phase extraction was applied reaching with a 250- preconcentration factor. The screening methodology allowed the detection of sample components without any kind of pre-selection of target pollutants. The identity of com...

  6. Separation of selenium, zinc, and copper compounds in bovine whey using size exclusion chromatography linked to inductively coupled plasma mass spectrometry.

    OpenAIRE

    Hoac, Tien; Lundh, Thomas; Purup, Stig; Onning, Gunilla; Sejrsen, Kristen; Akesson, Bjorn

    2007-01-01

    To study the role of trace elements for the quality and nutritional value of bovine milk, the distribution of selenium, zinc, and copper in whey was investigated using a method linking size exclusion chromatography to inductively coupled plasma mass spectrometry (SEC-ICP-MS). Three major peaks were detected for selenium, two peaks for zinc, and five peaks for copper. More than 65% of the selenium was found in protein fractions, mainly in fractions coinciding with the major whey proteins beta-...

  7. Extraction and Characterization of Phenolic Compounds from Rose Hip (Rosa canina L.) Using Liquid Chromatography Coupled with Electrospray Ionization - Mass Spectrometry

    OpenAIRE

    Stănilă, Andreea; Diaconeasa, Zoriţa; Roman, Ioana; Nicușor SIMA; Dănuț MĂNIUȚIU; Alin ROMAN; Rodica SIMA

    2015-01-01

    Wild berry are a rich of natural compounds which provide them high antioxidant potential. The compounds which provide them these proprieties are known to be vitamins, flavonoids, anthocyanins and phenolic acids. The aim of this study was to extract and characterize bioactive compounds from rose hip (Rosa canina L.) currently found in Romania. A qualitative high-performance liquid chromatography coupled with electrospray ionization mass spectrometric (ESI-MS) detection in positive ion mode has...

  8. Arsenic Species in Edible Seaweeds Using In Vitro Biomimetic Digestion Determined by High-Performance Liquid Chromatography Inductively Coupled Plasma Mass Spectrometry

    OpenAIRE

    Yan-Fang Zhao; Ji-Fa Wu; De-Rong Shang; Jin-Song Ning; Hai-Yan Ding; Yu-Xiu Zhai

    2014-01-01

    Arsenite [As (III)], arsenate [As (V)], methylarsonate (MMA), and dimethylarsinate (DMA) in five edible seaweeds (the brown algae Laminaria japonica, red algae Porphyra yezoensis, brown algae Undaria pinnatifida, brown algae Hizikia fusiformis, and green algae Enteromorpha prolifera) were analyzed using in vitro digestion method determined by high-performance liquid chromatography inductively coupled plasma mass spectrometry. The results showed that DMA was found in the water extracts of all ...

  9. Quantitation of motexafin lutetium in human plasma by liquid chromatography-tandem mass spectrometry and inductively coupled plasma-atomic emission spectroscopy

    OpenAIRE

    Miles, Dale; Mody, Tarak D.; Hatcher, Lori I.; Fiene, John; Stiles, Mark; Patrick P. Lin; Lee, J.W.

    2003-01-01

    Liquid chromatography-tandem mass spectrometry (LC-MS/MS) and inductively coupled plasma-atomic emission spectroscopy (ICP-AES) methods were developed and validated for the evaluation of motexafin lutetium (MLu, lutetium texaphyrin, PCI-0123) pharmacokinetics in human plasma. The LC-MS/MS method was specific for MLu, whereas the ICP-AES method measured total elemental lutetium. Both methods were fast, simple, precise, and accurate. For the LC-MS/MS method, a closely related analogue (PCI-0353...

  10. Determination of iodine and iodine compounds in marine samples by ICPMS and HPLC-ICPMS

    DEFF Research Database (Denmark)

    Hansen, Maiken Sødergreen; Lewandowski, Daniel Jacob; Rasmussen, Rie Romme;

    2014-01-01

    By now it is a well-known fact that iodine is an essential trace element for the growth and development of the human body. Because of iodine deficiency, some countries have added iodate to salt in order to increase the iodine intake. However, some people prefer iodine from more natural sources li...... chromatography (HPLC) coupled to ICPMS. These studies may be a stepping stone for further studies that can clarify the cycle and implications of iodine species in relation to the use of marine food items as iodine sources....

  11. Simultaneous Determination of Three Bioactive Compounds in Traditional Chinese Medicine Patent Prescription Zuojin Pill by HPLC

    OpenAIRE

    Cai, Jinzhang; Huang, Zhenzhen; Chen, Chan; Xu, Ren-ai; Lin, Chongliang; Lin, Guanyang; Wang, Xianqin

    2012-01-01

    A high-performance liquid chromatography (HPLC) method coupled with ultraviolet (UV) detection has been developed and validated for simultaneous quantification of berberine hydrochloride, evodiamine and rutaecarpine in Zuojin Pill. Chromatographic separation were achieved on a ODS-C18 column (250×4.6 mm i.d., 5.0 μm particle) through a 25 min gradient delivery of a mixture of A (acetonitrile) and B (0.3 % phosphoric acid-0.3 % triethylamine) at a flow rate of 0.8 mL/min at 40 °C. All of the a...

  12. Detection of biogenic amines in urine and plasma by liquid chromatography coupled to electrochemical detection HPLC-ED using microextraction in packed syringe MEPS

    OpenAIRE

    Oppolzer, David Jerónimo

    2012-01-01

    Biogenic amines are neurotransmitters involved in several physiological processes. Changes and disturbs in their function are associated to several neurological disorders or diseases, as well as consumption of psychotherapeutic or psychotropic drugs. The detection of these compounds in biological fluids is therefore of clinical and neurochemical interest. The goal of this work was to develop and validate and analytical method for the detection and quantification of the biogenic...

  13. Simultaneous Determination of Size and Quantification of Gold Nanoparticles by Direct Coupling Thin layer Chromatography with Catalyzed Luminol Chemiluminescence

    Science.gov (United States)

    Yan, Neng; Zhu, Zhenli; He, Dong; Jin, Lanlan; Zheng, Hongtao; Hu, Shenghong

    2016-04-01

    The increasing use of metal-based nanoparticle products has raised concerns in particular for the aquatic environment and thus the quantification of such nanomaterials released from products should be determined to assess their environmental risks. In this study, a simple, rapid and sensitive method for the determination of size and mass concentration of gold nanoparticles (AuNPs) in aqueous suspension was established by direct coupling of thin layer chromatography (TLC) with catalyzed luminol-H2O2 chemiluminescence (CL) detection. For this purpose, a moving stage was constructed to scan the chemiluminescence signal from TLC separated AuNPs. The proposed TLC-CL method allows the quantification of differently sized AuNPs (13 nm, 41 nm and 100 nm) contained in a mixture. Various experimental parameters affecting the characterization of AuNPs, such as the concentration of H2O2, the concentration and pH of the luminol solution, and the size of the spectrometer aperture were investigated. Under optimal conditions, the detection limits for AuNP size fractions of 13 nm, 41 nm and 100 nm were 38.4 μg L‑1, 35.9 μg L‑1 and 39.6 μg L‑1, with repeatabilities (RSD, n = 7) of 7.3%, 6.9% and 8.1% respectively for 10 mg L‑1 samples. The proposed method was successfully applied to the characterization of AuNP size and concentration in aqueous test samples.

  14. Determination of phosphodiesterase type V inhibitors in wastewater by direct injection followed by liquid chromatography coupled to tandem mass spectrometry.

    Science.gov (United States)

    Causanilles, Ana; Emke, Erik; de Voogt, Pim

    2016-09-15

    A simple, fast and reliable analytical method for the determination of phosphodiesterase type V inhibitors in wastewater was developed and validated. The method was based on direct injection followed by liquid chromatography coupled to tandem mass spectrometry with triple quadrupole as mass analyzer. Transformation products and analogues were included in the target list besides the three active pharmaceutical ingredients (sildenafil, vardenafil and tadalafil). The method performance was thoroughly investigated, including the analyte stability in wastewater and matrix effect. All target compounds presented linear fits between their LOD and 500ng/L. The quantification limits ranged from 1.6 to 30ng/L for all compounds except for n-octylnortadalafil (LOQ: 100ng/L); precision calculated as intraday repeatability was lower than 30%; accuracy calculated as procedural recovery ranged successfully between 85 and 105% in all cases. The method was applied to samples collected during three week-long monitoring campaigns performed in 2013, 2014 and 2015 in three Dutch cities. Only sildenafil and its two metabolites, desmethyl- and desethylsildenafil, were present with normalized loads ranging from LOQ to 8.3, 11.8 and 21.6mg/day/1000 inh, respectively. Two additional week-long sets of samples were collected in Amsterdam at the time that a festival event took place, bringing around 350,000 visitors to the city. The difference in drug usage patterns was statistically studied: "weekday" versus "weekend", "normal" versus "atypical" week; and results discussed. The metabolite to parent drug concentration ratio evolution during consecutive years was discussed, leading to several possible explanations that should be further investigated. Finally, wastewater-based epidemiology approach was applied to back-calculate sildenafil consumption. PMID:27161135

  15. Determination of fungicides in wine by mixed-mode solid phase extraction and liquid chromatography coupled to tandem mass spectrometry.

    Science.gov (United States)

    Carpinteiro, I; Ramil, M; Rodríguez, I; Cela, R

    2010-11-26

    A novel procedure for the determination of nine selected fungicides (metalaxyl-M, azoxystrobin, myclobutanil, flusilazole, penconazole, tebuconazole, propiconazole, diniconazole and difenoconazole) in wine samples is presented. Sample enrichment and purification is simultaneously performed using mixed-mode, anion exchange and reversed-phase, OASIS MAX solid-phase extraction (SPE) cartridges. Analytes were determined by liquid chromatography coupled to tandem mass spectrometry using atmospheric pressure electrospray ionization (LC-ESI-MS/MS). Parameters affecting the chromatographic determination and the extraction-purification processes were thoroughly investigated. Under optimized conditions, 10 mL of wine were firstly diluted 1:1 with ultrapure water and then passed through the mixed-mode SPE cartridge at a flow of ca. 5 mLmin(-1). After a washing step with 5 mL of an aqueous NH(4)OH solution (5%, w:v), analytes were recovered with just 1 mL of methanol and injected in the LC-MS/MS system without any additional purification. The selective extraction process avoided significant changes in the ionization efficiency for red and white wine extracts in comparison with pure standards in methanol. Performance of the method was good in terms of precision (RSDs72%, determined against pure standards in methanol) reporting method LOQs in the range of 0.01-0.79 ngmL(-1) for target compounds, which are far below the EU maxima residue levels (MRLs) for fungicides in vinification grapes and wine. Several commercial wines from different geographic areas in Spain were analyzed. In most samples, metalaxyl-M and azoxystrobin were found at concentrations up to several ngmL(-1). PMID:20971470

  16. Microextraction Techniques Coupled to Liquid Chromatography with Mass Spectrometry for the Determination of Organic Micropollutants in Environmental Water Samples

    Directory of Open Access Journals (Sweden)

    Mª Esther Torres Padrón

    2014-07-01

    Full Text Available Until recently, sample preparation was carried out using traditional techniques, such as liquid–liquid extraction (LLE, that use large volumes of organic solvents. Solid-phase extraction (SPE uses much less solvent than LLE, although the volume can still be significant. These preparation methods are expensive, time-consuming and environmentally unfriendly. Recently, a great effort has been made to develop new analytical methodologies able to perform direct analyses using miniaturised equipment, thereby achieving high enrichment factors, minimising solvent consumption and reducing waste. These microextraction techniques improve the performance during sample preparation, particularly in complex water environmental samples, such as wastewaters, surface and ground waters, tap waters, sea and river waters. Liquid chromatography coupled to tandem mass spectrometry (LC/MS/MS and time-of-flight mass spectrometric (TOF/MS techniques can be used when analysing a broad range of organic micropollutants. Before separating and detecting these compounds in environmental samples, the target analytes must be extracted and pre-concentrated to make them detectable. In this work, we review the most recent applications of microextraction preparation techniques in different water environmental matrices to determine organic micropollutants: solid-phase microextraction SPME, in-tube solid-phase microextraction (IT-SPME, stir bar sorptive extraction (SBSE and liquid-phase microextraction (LPME. Several groups of compounds are considered organic micropollutants because these are being released continuously into the environment. Many of these compounds are considered emerging contaminants. These analytes are generally compounds that are not covered by the existing regulations and are now detected more frequently in different environmental compartments. Pharmaceuticals, surfactants, personal care products and other chemicals are considered micropollutants. These

  17. High temperature liquid chromatography-inductively coupled plasma mass spectrometry for the determination of arsenosugars in biological samples.

    Science.gov (United States)

    Terol, Amanda; Ardini, Francisco; Grotti, Marco; Todolí, José Luis

    2012-11-01

    The potential of high temperature liquid chromatography (HTLC) with detection by inductively coupled plasma mass spectrometry (ICP-MS) for the determination of arsenosugars in marine organisms was examined for the first time. The retention behavior of four naturally occurring dimethylarsinoylribosides was studied on a graphite column using plain water as mobile phase. An aqueous solution of pH 8, ionic strength 13.8mM and containing 2% (v/v) of methanol, along with a column temperature of 120°C and a liquid flow rate of 1.0 mL/min, were selected as the optimal conditions, as they allowed the separation of the four arsenosugars in less than 18 min, without any interferences due to other common arsenic species (arsenite, arsenate, dimethylarsinate, methylarsonate and arsenobetaine). The run time could be further decreased to 12 min by working at 1.5 mL/min, although with a 3-4 times loss of sensitivity. The procedural limits of detection were 0.03-0.04 μg As/g dry mass, and the precision of the procedure ranged from 4% for arsenosugar glycerol to 18% for arsenosugar sulfate (RSD%, n=5). The developed method was applied to a number of representative biological samples, such as algae and crustaceans, providing results consistent with previous studies. In the red algae samples, the most of extracted arsenic was as arsenosugars (81-97%), mainly arsenosugar phosphate (56-94%). On the other hand, lower concentrations of these compounds were found in the crustacean, accounting for about 15% of the extracted arsenic. PMID:22995196

  18. Characterizations of the hydrolyzed products of ginkgolide A and ginkgolide B by liquid chromatography coupled with mass spectrometry.

    Science.gov (United States)

    Lan, Ke; Li, Xue-Jing; Du, Gang; Xu, Liang

    2016-01-25

    Ginkgolides are diterpenoid trilactones responsible for the neuromodulatory properties of Ginkgo biloba extracts. They are to be hydrolyzed in aqueous solutions as mixed carboxylate forms potentially including three monocarboxylates, three dicarboxylates and one tricarboxylate. Characterizations of the hydrolyzed products are challenging because there is no way to prepare them individually. In this work, the major hydrolyzed products of ginkgolide A (GA) and ginkgolide B (GB) including all three monocarboxyaltes have been produced in buffers and subjected to liquid chromatography coupled with triple quadrupole MS and LTQ Orbitrap MS analysis. With the comparative analysis of the trilactone of GA and GB, it was highlighted a unique charge-driven fragmentation pathway of twice neutral losses of CO on the lactone-C. The monocarboxylates were accordingly identified based on the construction of their fragmentation pathways cross-linked with those of the trilactone. In brief, the lactone-C hydrolyzed product is characteristic of the absence of product ions between [M-H](-) and [M-H-C2H2O3](-) (m/z 351 for GA and m/z 367 for GB). The featured fragmentation pathway of the lactone-F hydrolyzed product is the cleavage of ring-A, yielding a fragment (m/z 295 for GA and m/z 309 for GB) followed with twice (GA) or triple (GB) neutral losses of CO. The most characteristic fragment of the lactone-E hydrolyzed product is [M-H-H2O-CO2-2CO](-) (m/z 307 for GA and m/z 323 for GB) in contrast to the other two monocarboxylates. The knowledge gained in this work was of special uses to investigate the biological fates and the corresponding pharmacological mechanisms of ginkgolides. PMID:26540626

  19. Rapid and sensitive hormonal profiling of complex plant samples by liquid chromatography coupled to electrospray ionization tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    Müller Maren

    2011-11-01

    Full Text Available Abstract Background Plant hormones play a pivotal role in several physiological processes during a plant's life cycle, from germination to senescence, and the determination of endogenous concentrations of hormones is essential to elucidate the role of a particular hormone in any physiological process. Availability of a sensitive and rapid method to quantify multiple classes of hormones simultaneously will greatly facilitate the investigation of signaling networks in controlling specific developmental pathways and physiological responses. Due to the presence of hormones at very low concentrations in plant tissues (10-9 M to 10-6 M and their different chemistries, the development of a high-throughput and comprehensive method for the determination of hormones is challenging. Results The present work reports a rapid, specific and sensitive method using ultrahigh-performance liquid chromatography coupled to electrospray ionization tandem spectrometry (UPLC/ESI-MS/MS to analyze quantitatively the major hormones found in plant tissues within six minutes, including auxins, cytokinins, gibberellins, abscisic acid, 1-amino-cyclopropane-1-carboxyic acid (the ethylene precursor, jasmonic acid and salicylic acid. Sample preparation, extraction procedures and UPLC-MS/MS conditions were optimized for the determination of all plant hormones and are summarized in a schematic extraction diagram for the analysis of small amounts of plant material without time-consuming additional steps such as purification, sample drying or re-suspension. Conclusions This new method is applicable to the analysis of dynamic changes in endogenous concentrations of hormones to study plant developmental processes or plant responses to biotic and abiotic stresses in complex tissues. An example is shown in which a hormone profiling is obtained from leaves of plants exposed to salt stress in the aromatic plant, Rosmarinus officinalis.

  20. Analysis of plant hormones by microemulsion electrokinetic capillary chromatography coupled with on-line large volume sample stacking.

    Science.gov (United States)

    Chen, Zongbao; Lin, Zian; Zhang, Lin; Cai, Yan; Zhang, Lan

    2012-04-01

    A novel method of microemulsion electrokinetic capillary chromatography (MEEKC) coupled with on-line large volume sample stacking was developed for the analysis of six plant hormones including indole-3-acetic acid, indole-3-butyric acid, indole-3-propionic acid, 1-naphthaleneacetic acid, abscisic acid and salicylic acid. Baseline separation of six plant hormones was achieved within 10 min by using the microemulsion background electrolyte containing a 97.2% (w/w) 10 mM borate buffer at pH 9.2, 1.0% (w/w) ethyl acetate as oil droplets, 0.6% (w/w) sodium dodecyl sulphate as surfactant and 1.2% (w/w) 1-butanol as cosurfactant. In addition, an on-line concentration method based on a large volume sample stacking technique and multiple wavelength detection was adopted for improving the detection sensitivity in order to determine trace level hormones in a real sample. The optimal method provided about 50-100 fold increase in detection sensitivity compared with a single MEEKC method, and the detection limits (S/N = 3) were between 0.005 and 0.02 μg mL(-1). The proposed method was simple, rapid and sensitive and could be applied to the determination of six plant hormones in spiked water samples, tobacco leaves and 1-naphthylacetic acid in leaf fertilizer. The recoveries ranged from 76.0% to 119.1%, and good reproducibilities were obtained with relative standard deviations (RSDs) less than 6.6%. PMID:22363931

  1. Simultaneous Determination of Size and Quantification of Gold Nanoparticles by Direct Coupling Thin layer Chromatography with Catalyzed Luminol Chemiluminescence

    Science.gov (United States)

    Yan, Neng; Zhu, Zhenli; He, Dong; Jin, Lanlan; Zheng, Hongtao; Hu, Shenghong

    2016-01-01

    The increasing use of metal-based nanoparticle products has raised concerns in particular for the aquatic environment and thus the quantification of such nanomaterials released from products should be determined to assess their environmental risks. In this study, a simple, rapid and sensitive method for the determination of size and mass concentration of gold nanoparticles (AuNPs) in aqueous suspension was established by direct coupling of thin layer chromatography (TLC) with catalyzed luminol-H2O2 chemiluminescence (CL) detection. For this purpose, a moving stage was constructed to scan the chemiluminescence signal from TLC separated AuNPs. The proposed TLC-CL method allows the quantification of differently sized AuNPs (13 nm, 41 nm and 100 nm) contained in a mixture. Various experimental parameters affecting the characterization of AuNPs, such as the concentration of H2O2, the concentration and pH of the luminol solution, and the size of the spectrometer aperture were investigated. Under optimal conditions, the detection limits for AuNP size fractions of 13 nm, 41 nm and 100 nm were 38.4 μg L−1, 35.9 μg L−1 and 39.6 μg L−1, with repeatabilities (RSD, n = 7) of 7.3%, 6.9% and 8.1% respectively for 10 mg L−1 samples. The proposed method was successfully applied to the characterization of AuNP size and concentration in aqueous test samples. PMID:27080702

  2. [Determination of fructooligosaccharides in milk powder using high performance anion-exchange chromatography coupled with pulsed amperometric detection].

    Science.gov (United States)

    Geng, Lijuan; Huang, Junrong; Feng, Feng; Jiang, Pingping; Chu, Xiaogang; Zhang, Feng; Ling, Yun

    2014-12-01

    Fructooligosaccharides (FOS) are usually added in milk powder as a kind of prebiotic. Thus, quantitative analysis of the FOS is very important for the quality control of milk powder. In this study, a simple method for the simultaneous determination of three FOS components with degrees of polymerization (DP) 3-5 in milk powder was developed by high performance anion-exchange chromatography coupled with pulsed amperometric detection (HPAEC-PAD). The samples were extracted with 50% (v/v) ethanol aqueous solution and defatted by an On Guard RP pretreatment column. The separation was performed on a CarboPac PA200 column by gradient elution using deionized water, 0. 2 mol/L NaOH solution and 0. 4 mol/L NaAc solution as the mobile phases. The flow rate was 0. 4 mL/min. The column temperature was 30 °C; and the injection volume was 25 µL. Good linear response was observed in the concentration range of 0.05-10 mg/L (r2 >0. 9993). The limits of quantification were 0. 02, 0. 005 and 0. 02 mg/L for 1-kestose, nystose and fructofuranosyl-nystose, respectively. The mean recoveries varied from 86. 0% to 114. 0% at three spiked levels of 0. 5, 1. 0 and 5. 0 mg/L. The short-chain fructooligosaccharides from inulooligosaccharides (IOS) were successfully separated by the developed HPAEC-PAD method. The method is simple, accurate, sensitive, and helpful for the quality control of milk powder. PMID:25902647

  3. Microextraction techniques coupled to liquid chromatography with mass spectrometry for the determination of organic micropollutants in environmental water samples.

    Science.gov (United States)

    Padrón, Ma Esther Torres; Afonso-Olivares, Cristina; Sosa-Ferrera, Zoraida; Santana-Rodríguez, José Juan

    2014-01-01

    Until recently, sample preparation was carried out using traditional techniques, such as liquid-liquid extraction (LLE), that use large volumes of organic solvents. Solid-phase extraction (SPE) uses much less solvent than LLE, although the volume can still be significant. These preparation methods are expensive, time-consuming and environmentally unfriendly. Recently, a great effort has been made to develop new analytical methodologies able to perform direct analyses using miniaturised equipment, thereby achieving high enrichment factors, minimising solvent consumption and reducing waste. These microextraction techniques improve the performance during sample preparation, particularly in complex water environmental samples, such as wastewaters, surface and ground waters, tap waters, sea and river waters. Liquid chromatography coupled to tandem mass spectrometry (LC/MS/MS) and time-of-flight mass spectrometric (TOF/MS) techniques can be used when analysing a broad range of organic micropollutants. Before separating and detecting these compounds in environmental samples, the target analytes must be extracted and pre-concentrated to make them detectable. In this work, we review the most recent applications of microextraction preparation techniques in different water environmental matrices to determine organic micropollutants: solid-phase microextraction SPME, in-tube solid-phase microextraction (IT-SPME), stir bar sorptive extraction (SBSE) and liquid-phase microextraction (LPME). Several groups of compounds are considered organic micropollutants because these are being released continuously into the environment. Many of these compounds are considered emerging contaminants. These analytes are generally compounds that are not covered by the existing regulations and are now detected more frequently in different environmental compartments. Pharmaceuticals, surfactants, personal care products and other chemicals are considered micropollutants. These compounds must be

  4. Determination of Estrogens in Milk Samples by Magnetic-Solid-Phase Extraction Technique Coupled With High-Performance Liquid Chromatography.

    Science.gov (United States)

    Wang, Juan; Cheng, Chunsheng; Yang, Yaling

    2015-12-01

    A magnetic-solid-phase extraction method coupled with high-performance liquid chromatography and diode array detection has been developed for simultaneous determination of 3 estrogens in milk samples. In this work, Fe3O4 NPs were synthesized by a simple chemical co-precipitation reaction, and the surface of Fe3O4 was modified with cetyltrimethyl ammonium bromide (CTAB; designed as Fe3O4@CTAB). The synthesized Fe3O4@CTAB NPs were characterized by Fourier transformed infrared spectroscopy, scanning electron microscopy, and transmission electron microscope. Fe3O4@CTAB NPs have high binding affinity toward estrone (E1), 17β-estradiol (17β-E2), and diethylstilbestrol (DES). Fe3O4@CTAB NPs can be easily separated from sample solutions using an external magnet due to the high super-paramagnetic property. The separation, preconcentration procedure is fast and will be completed in 2 min. Estrogens linear dynamic ranges were achieved in the range of 10 to 1000 ng/mL with regression coefficients (R(2)) higher than 0.9992. The limits of detection were between 0.26 and 0.61 ng/mL. Parameters influencing the recoveries were investigated and optimized. The proposed method was used for the determination of E1, 17β-E2, and DES in milk samples, and recoveries were ranged from 91.3% to 105.0%, with the relative standard deviations in the range of 2.7% to 4.0%. PMID:26488134

  5. Fast determination of phenoxy acid herbicides in carrots and apples using liquid chromatography coupled triple quadrupole mass spectrometry.

    Science.gov (United States)

    Santilio, Angela; Stefanelli, Patrizia; Dommarco, Roberto

    2009-08-01

    A fast, simple and inexpensive method has been developed for the analysis of phenoxy acid herbicides: 2,4-dichlorophenoxyacetic acid (2,4-D), 4-chloro-2-methylphenoxyacetic acid (MCPA), 2-(4-chloro-o-tolyloxy)propionic acid (MCPP), 2-(4-aryloxyphenoxy)propionic acid (Fluazifop) and 2-(4-aryloxyphenoxy)propionic acid (Haloxyfop) in carrots and apples by liquid chromatography coupled to triple quadrupole mass spectrometry (LC/MS/MS). The compounds were analyzed by QuEChERS (quick, easy, cheap, effective, rugged, safe) methodology without cleanup. The recoveries were performed at two spiked levels (0.05 and 0.5 mg/kg) for both matrices with six replicates for each level. The mean recoveries ranged from 70-92% for both apples and carrots. The precision of the method expressed as relative standard deviation (RSD%) was found to be in the range 3-15%. For all compounds, good linearity (r(2) > 0.99) was obtained over the range of concentration from 0.05 micro g/mL to 0.5 micro g/mL, corresponding to the pesticide concentrations of 0.05 mg/kg and 0.5 mg/kg, respectively. The determination limits (LOQs) ranged from 0.01 ng/mL to 1.3 ng/mL in solvent, whereas, the LOQs calculated in matrix ranged from 0.05 ng/g to 21.0 ng/g for apples and from 0.06 ng/g to 10.2 ng/g for carrots. The developed methodology combines the advantages of both QuEChERS and LC/MS/MS producing a very rapid, sensitive and cheap method useful for the routine analytical laboratories. PMID:20183066

  6. Quantitative multi-residue method for determination antibiotics in chicken meat using turbulent flow chromatography coupled to liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Bousova, Katerina; Senyuva, Hamide; Mittendorf, Klaus

    2013-01-25

    A multi-class method for identification and quantification of 36 antibiotics from seven different chemical classes (aminoglycosides, macrolides, lincosamides, sulfonamides, tetracyclines, quinolones and trimethoprim) has been developed by using liquid chromatography-mass spectrometry. The method was optimised for detection of antibiotics in chicken meat. Sample preparation including extraction with a mixture of acetonitrile:2% trichloroacetic acid (45:55, v/v), centrifugation and filtration was followed by on-line clean-up using turbulent flow chromatography. Using this automated on-line technique enabled a larger number of samples to be analysed per day than with a traditional clean-up technique (e.g. solid phase extraction). The optimised method was validated according to the European Commission Directive 2002/657/EC. In-house validation was performed by fortifying the blank matrix at three levels 0.5, 1.0 and 1.5 MRL (maximum residue limit), or respectively, at concentrations as low as possible for substances without an MRL. Precision in terms of repeatability standard deviation ranged from 3 to 28% and recovery values were between 80 and 120% in most cases. All calculated validation parameters including CCα and CCβ were in the compliance with the legislative requirements. PMID:23298848

  7. Comparative studies on performance of CCC and preparative RP-HPLC in separation and purification of steroid saponins from Dioscorea zingiberensis C.H.Wright

    OpenAIRE

    Zhang, Xinxin; Liang, Jinru; Zhang, Yongmin; Liu, Jianli; Sun, Wenji; Ito, Yoichiro

    2015-01-01

    Steroid saponins from Dioscorea zingiberensis C.H.Wright were separated for the first time using two chromatographic methods for comparison: counter-current chromatography (CCC) coupled with evaporative light scattering detector (ELSD) and preparative reversed phase high-performance liquid chromatography (RP-HPLC) with an ultraviolet detector. Ethyl acetate-n-butanol-methanol-water (4:1:2:4, v/v) was chosen as the two-phase solvent system for CCC, while the acetonitrile-water (25:75 for the f...

  8. Speciation of butyltin compounds in environmental and biological samples using headspace single drop microextraction coupled with gas chromatography-inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Xiao, Qin; Hu, Bin; He, Man

    2008-11-21

    A method based on headspace single drop microextraction (HS-SDME) in combination with gas chromatography-inductively coupled plasma mass spectrometry (GC-ICP-MS) was proposed for the speciation analysis of butyltin compounds in environmental and biological samples. The sodium tetraethylborate (NaBEt4) and sodium tetrahydroborate (NaBH4) were used as the derivatizing reagent for in situ derivatization of the butyltins. For the two derivatizations, the HS-SDME parameters such as organic solvent, drop volume, sample pH, stirring rate, temperature, extraction time and the ionic strength were examined systematically. The analytical performance including the linearity ranges, limits of detection (LODs) and reproducibilities of the two derivatizations were compared under the respective optimized conditions. Derivatization with NaBEt(4) proved to be more sensitive and robust than that with NaBH4, leading to the LODs of 1.4 ng/L for MBT, 1.8 ng/L for DBT and 0.8 ng/L for TBT. The reproducibilities, expressed as relative standard deviations (RSDs), were in the range of 1.1-5.3% (c=1 microg/L, n=3). With tripropyltin (TPrT) as internal standard, HS-SDME-GC-ICP-MS with NaBEt(4) derivatization was applied for the speciation analysis of butyltins in real seawater and shellfish samples. The butyltins found in the real-world samples are 31ng/L MBT, 79 ng/L DBT and 32 ng/L TBT for seawater, and 11.6-30.4 ng/g MBT, 11.8-8.9 ng/g DBT and 12.8-52.6 ng/g TBT for different shellfish samples. For validation, the developed method was also employed for the speciation analysis of butyltins in certified reference material (CRM) of PACS-2 sediment, and the determined values are in a good agreement with the certified values. The developed method is simple, rapid, sensitive, and cost-effective and provides an attractive alternative for butyltins speciation in biological and environmental samples with complex matrix. PMID:18922539

  9. Simultaneous multi-mycotoxin determination in nutmeg by ultrasound-assisted solid-liquid extraction and immunoaffinity column clean-up coupled with liquid chromatography and on-line post-column photochemical derivatization-fluorescence detection.

    Science.gov (United States)

    Kong, Wei-Jun; Liu, Shu-Yu; Qiu, Feng; Xiao, Xiao-He; Yang, Mei-Hua

    2013-05-01

    A simple and sensitive analytical method based on ultrasound-assisted solid-liquid extraction and immunoaffinity column clean-up coupled with high performance liquid chromatography and on-line post-column photochemical derivatization-fluorescence detection (USLE-IAC-HPLC-PCD-FLD) has been developed for simultaneous multi-mycotoxin determination of aflatoxins B1, B2, G1, G2 (AFB1, AFB2, AFG1, AFG2) and ochratoxin A (OTA) in 13 edible and medicinal nutmeg samples marketed in China. AFs and OTA were extracted from nutmeg samples by ultrasonication using a methanol : water (80 : 20, v/v) solution, followed by an IAC clean-up step. Different USL extraction conditions, pre-processing ways for nutmeg sample and clean-up columns for mycotoxins, as well as HPLC-PCD-FLD parameters (mobile phase, column temperature, elution procedure, excitation and emission wavelengths) were optimized. This method, which was appraised for analyzing nutmeg samples, showed satisfactory results with reference to limits of detection (LODs) (from 0.02 to 0.25 μg kg(-1)), limits of quantification (LOQs) (from 0.06 to 0.8 μg kg(-1)), linear ranges (up to 30 ng mL(-1) for AFB1, AFG1 and OTA and 9 ng mL(-1) for AFB2 and AFG2), intra- and inter-day variability (all <2%) and average recoveries (from 79.6 to 90.8% for AFs and from 93.6 to 97.3% for OTA, respectively). The results of the application of developed method in nutmeg samples have elucidated that four samples were detected with contamination of AFs and one with OTA. AFB1 was the most frequently found mycotoxin in 30.8% of nutmeg samples at contamination levels of 0.73-16.31 μg kg(-1). At least two different mycotoxins were co-occurred in three samples, and three AFs were simultaneously detected in one sample. PMID:23486692

  10. Comprehensive Two-Dimensional Hydrophilic Interaction Chromatography (HILIC) × Reversed-Phase Liquid Chromatography Coupled to High-Resolution Mass Spectrometry (RP-LC-UV-MS) Analysis of Anthocyanins and Derived Pigments in Red Wine.

    Science.gov (United States)

    Willemse, Chandré M; Stander, Maria A; Vestner, Jochen; Tredoux, Andreas G J; de Villiers, André

    2015-12-15

    Changes in anthocyanin chemistry represent some of the most important transformations involved in red wine aging. However, accurate analysis of the derived pigments, as required to study the evolution of anthocyanins and tannins during aging, is hampered by their extreme structural diversity, low levels, and the fact that many of these compounds have identical mass spectral characteristics. In this context, chromatographic separation is critical. In this contribution, the application of online hydrophilic interaction chromatography (HILIC) × reversed-phase liquid chromatography (RP-LC) separation coupled to high-resolution mass spectrometry (MS) is described for the detailed characterization of anthocyanins and their derived pigments in aged red wine. A systematic approach was followed for the optimization of HILIC × RP-LC separation parameters using a capillary liquid chromatography (LC) system in the first dimension and an ultrahigh-pressure LC system in the second dimension to ensure maximum sensitivity and performance. Ninety four (94) anthocyanin-derived pigments were tentatively identified in one- and six-year-old Pinotage wines using accurate mass and fragmentation information obtained using quadrupole-time-of-flight mass spectrometry (Q-TOF-MS). Online HILIC × RP-LC-MS was found to offer high-resolution separation, because of the combination of two different separation modes, while the structured elution order observed improved the certainty in compound identification. Therefore, this approach shows promise for the detailed elucidation of the chemical alteration of anthocyanins during wine aging. PMID:26554292

  11. Two-dimensional turbulent flow chromatography coupled on-line to liquid chromatography-mass spectrometry for solution-based ligand screening against multiple proteins.

    Science.gov (United States)

    Zhou, Jian-Liang; An, Jing-Jing; Li, Ping; Li, Hui-Jun; Jiang, Yan; Cheng, Jie-Fei

    2009-03-20

    We present herein a novel bioseparation/chemical analysis strategy for protein-ligand screening and affinity ranking in compound mixtures, designed to increase screening rates and improve sensitivity and ruggedness in performance. The strategy is carried out by combining on-line two-dimensional turbulent flow chromatography (2D-TFC) with liquid chromatography-mass spectrometry (LC-MS), and accomplished through the following steps: (1) a reversed-phase TFC stage to separate the protein/ligand complex from the unbound free molecules, (2) an on-line dissociation process to release the bound ligands from the complexes, and (3) a second mixed-mode cation-exchange/reversed-phase TFC stage to trap the bound ligands and to remove the proteins and salts, followed by LC-MS analysis for identification and determination of the binding affinities. The technique can implement an ultra-fast isolation of protein/ligand complex with the retention time of a complex peak in about 5s, and on-line prepare the "clean" sample to be directly compatible with the LC-MS analysis. The improvement in performance of this 2D-TFC/LC-MS approach over the conventional approach has been demonstrated by determining affinity-selected ligands of the target proteins acetylcholinesterase and butyrylcholinesterase from a small library with known binding affinities and a steroidal alkaloid library composed of structurally similar compounds. Our results show that 2D-TFC/LC-MS is a generic and efficient tool for high-throughput screening of ligands with low-to-high binding affinities, and structure-activity relationship evaluation. PMID:19203758

  12. On-line coupling of counter-current chromatography and macroporous resin chromatography for continuous isolation of arctiin from the fruit of Arctium lappa L.

    Science.gov (United States)

    Guo, Mengzhe; Liang, Junling; Wu, Shihua

    2010-08-13

    In this work, we have developed a novel hybrid two-dimensional counter-current chromatography and liquid chromatography (2D CCC x LC) system for the continuous purification of arctiin from crude extract of Arctium lappa. The first dimensional CCC column has been designed to fractionalize crude complex extract into pure arctiin effluent using a one-component organic/salt-containing system, and the second dimensional LC column has been packed with macroporous resin for on-line adsorption, desalination and desorption of arctiin which was effluent purified from the first CCC dimension. Thus, the crude arctiin mixture has been purified efficiently and conveniently by on-line CCC x LC in spite of the use of a salt-containing solvent system in CCC separation. As a result, high purity (more than 97%) of arctiin has been isolated by repeated injections both using the ethyl acetate-8% sodium chloride aqueous solution and butanol-1% sodium chloride aqueous solution. By contrast with the traditional CCC processes using multi-component organic/aqueous solvent systems, the present on-line CCC x LC process only used a one-component organic solvent and thus the solvent is easier to recover and regenerate. All of used solvents such as ethyl acetate, n-butanol and NaCl aqueous solution are low toxicity and environment-friendly. Moreover, the lower phase of salt-containing aqueous solution used as mobile phase, only contained minor organic solvent, which will save much organic solvent in continuous separation. In summary, our results indicated that the on-line hybrid 2D CCC x LC system using one-component organic/salt-containing aqueous solution is very promising and powerful tool for high-throughput purification of arctiin from fruits of A. lappa. PMID:20619844

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

    International Nuclear Information System (INIS)

    A new IC-ESI-MS/MS method, with simple sample preparation procedure, has been developed for quantification and confirmation of perchlorate (ClO4-) anions in water, fresh and canned food, wine and beer samples at low part-per-trillion (ng l-1) levels. To the best of our knowledge, this is the first time an analytical method is used for determination of perchlorate in wine and beer samples. The IC-ESI-MS/MS instrumentation consisted of an ICS-2500 ion chromatography (IC) system coupled to either an API 2000TM or an API 3200TM mass spectrometer. The IC-ESI-MS/MS system was optimized to monitor two pairs of precursor and fragment ion transitions, i.e., multiple reaction monitoring (MRM). All samples had oxygen-18 isotope labeled perchlorate internal standard (ISTD) added prior to extraction. Chlorine isotope ratio (35Cl/37Cl) was used as a confirmation tool. The transition of 35Cl16O4- (m/z 98.9) into 35Cl16O3- (m/z 82.9) was monitored for quantifying the main analyte; the transition of 37Cl16O4- (m/z 100.9) into 37Cl16O3- (m/z 84.9) was monitored for examining a proper isotopic abundance ratio of 35Cl/37Cl; and the transition of 35Cl18O4- (m/z 107.0) into 35Cl18O3- (m/z 89.0) was monitored for quantifying the internal standard. The minimum detection limit (MDL) for this method in de-ionized water is 5 ng l-1 (ppt) using the API 2000TM mass spectrometer and 0.5 ng l-1 using the API 3200TM mass spectrometer. Over 350 food and beverage samples were analyzed mostly in triplicate. Except for four, all samples were found to contain measurable amounts of perchlorate. The levels found ranged from 5 ng l-1 to 463.5 ± 6.36 μg kg-1 using MRM 98.9 → 82.9 and 100 μl injection

  14. Dispersive liquid-phase microextraction with solidification of floating organic droplet coupled with high-performance liquid chromatography for the determination of Sudan dyes in foodstuffs and water samples.

    Science.gov (United States)

    Chen, Bo; Huang, Yuming

    2014-06-25

    Dispersive liquid-phase microextraction with solidification of floating organic drop (SFO-DLPME) is one of the most interesting sample preparation techniques developed in recent years. In this paper, a new, rapid, and efficient SFO-DLPME coupled with high-performance liquid chromatography (HPLC) was established for the extraction and sensitive detection of banned Sudan dyes, namely, Sudan I, Sudan II, Sudan III, and Sudan IV, in foodstuff and water samples. Various factors, such as the type and volume of extractants and dispersants, pH and volume of sample solution, extraction time and temperature, ion strength, and humic acid concentration, were investigated and optimized to achieve optimal extraction of Sudan dyes in one single step. After optimization of extraction conditions using 1-dodecanol as an extractant and ethanol as a dispersant, the developed procedure was applied for extraction of the target Sudan dyes from 2 g of food samples and 10 mL of the spiked water samples. Under the optimized conditions, all Sudan dyes could be easily extracted by the proposed SFO-DLPME method. Limits of detection of the four Sudan dyes obtained were 0.10-0.20 ng g(-1) and 0.03 μg L(-1) when 2 g of foodstuff samples and 10 mL of water samples were adopted, respectively. The inter- and intraday reproducibilities were below 4.8% for analysis of Sudan dyes in foodstuffs. The method was satisfactorily used for the detection of Sudan dyes, and the recoveries of the target for the spiked foodstuff and water samples ranged from 92.6 to 106.6% and from 91.1 to 108.6%, respectively. These results indicated that the proposed method is simple, rapid, sensitive, and suitable for the pre-concentration and detection of the target dyes in foodstuff samples. PMID:24894629

  15. Separation, concentration and determination of chloramphenicol in environment and food using an ionic liquid/salt aqueous two-phase flotation system coupled with high-performance liquid chromatography.

    Science.gov (United States)

    Han, Juan; Wang, Yun; Yu, Cuilan; Li, Chunxiang; Yan, Yongsheng; Liu, Yan; Wang, Liang

    2011-01-31

    Ionic liquid-salt aqueous two-phase flotation (ILATPF) is a novel, green, non-toxic and sensitive samples pretreatment technique. ILATPF coupled with high-performance liquid chromatography (HPLC) was developed for the analysis of chloramphenicol, which combines ionic liquid aqueous two-phase system (ILATPS) based on imidazolium ionic liquid (1-butyl-3-methylimidazolium chloride, [C(4)mim]Cl) and inorganic salt (K(2)HPO(4)) with solvent sublation. In ILATPF systems, phase behaviors of the ILATPF were studied for different types of ionic liquids and salts. The sublation efficiency of chloramphenicol in [C(4)mim]Cl-K(2)HPO(4) ILATPF was influenced by the types of salts, concentration of K(2)HPO(4) in aqueous solution, solution pH, nitrogen flow rate, sublation time and the amount of [C(4)mim]Cl. Under the optimum conditions, the average sublation efficiency is up to 98.5%. The mechanism of ILATPF contains two principal processes. One is the mechanism of IL-salt ILATPS formation, the other is solvent sublation. This method was practical when applied to the analysis of chloramphenicol in lake water, feed water, milk, and honey samples with the linear range of 0.5-500 ng mL(-1). The method yielded limit of detection (LOD) of 0.1 ng mL(-1) and limit of quantification (LOQ) of 0.3 ng mL(-1). The recovery of CAP was 97.1-101.9% from aqueous samples of environmental and food samples by the proposed method. Compared with liquid-liquid extraction, solvent sublation and ionic liquid aqueous two-phase extraction, ILATPF can not only separate and concentrate chloramphenicol with high sublation efficiency, but also efficiently reduce the wastage of IL. This novel technique is much simpler and more environmentally friendly and is suggested to have important applications for the concentration and separation of other small biomolecules. PMID:21168562

  16. Selenium speciation in radix puerariae using ultrasonic assisted extraction combined with reversed phase high performance liquid chromatography-inductively coupled plasma-mass spectrometry after magnetic solid-phase extraction with 5-sulfosalicylic acid functionalized magnetic nanoparticles

    Science.gov (United States)

    Cao, Yupin; Yan, Lizhen; Huang, Hongli; Deng, Biyang

    2016-08-01

    A new method for determination of selenium species in radix puerariae was described. The method consists of sample enrichment with 5-sulfosalicylic acid (SSA)-functionalized silica-coated magnetic nanoparticles (SMNPs), high performance liquid chromatography (HPLC) separation, and online detection using inductively coupled plasma mass spectrometry (ICP-MS). The selenium species were extracted using ultrasonic extraction system with a mixture of protease K and lipase. The SSA-SMNPs were used to enrich trace amounts of selenite [Se(IV)], selenate [Se(VI)], selenomethionine (SeMet), and selenocystine (SeCys2) from lower selenium containing samples. Under the optimal conditions, the limits of detection (3σ) for SeCys2, Se(IV), SeMet and Se(VI) were observed as 0.0023, 0.0015, 0.0043, and 0.0016 ng mL- 1, respectively. The RSD values (n = 6) of method for intraday were observed between 0.5% and 0.9%. The RSD values of method for interday were less than 1.3%. The linear concentration ranges for SeCys2, Se(IV), SeMet and Se(VI) were 0.008-1000, 0.005-200, 0.015-500 and 0.006-200 ng mL- 1, respectively. The detection limits of this method were improved by 10 times due to the enrichment with the SSA-SMNP extraction. The contents of SeCys2, Se(IV), SeMet, and Se(VI) in radix puerariae were determined as 0.0140, 0.171, 0.0178, and 0.0344 μg g- 1, respectively. The recoveries were in the range of 95.6%-99.4% and the RSDs (n = 6) of recoveries were less than 1.5%.

  17. Multiresidue analysis of 88 polar organic micropollutants in ground, surface and wastewater using online mixed-bed multilayer solid-phase extraction coupled to high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Huntscha, Sebastian; Singer, Heinz P; McArdell, Christa S; Frank, Carolin E; Hollender, Juliane

    2012-12-14

    An automated multiresidue method consisting of an online solid-phase extraction step coupled to a high performance liquid chromatography-tandem mass spectrometer (online-SPE-HPLC-MS/MS method) was developed for the determination of 88 polar organic micropollutants with a broad range of physicochemical properties (logD(OW) (pH 7): -4.2 to 4.2). Based on theoretical considerations, a single mixed-bed multilayer cartridge containing four different extraction materials was composed for the automated enrichment of water samples. This allowed the simultaneous analysis of pesticides, biocides, pharmaceuticals, corrosion inhibitors, many of their transformation products, and the artificial sweetener sucralose in three matrices groundwater, surface water, and wastewater. Limits of quantification (LOQs) were in the environmentally relevant concentration range of 0.1-87 ng/L for groundwater and surface water, and 1.5-206 ng/L for wastewater. The majority of the compounds could be quantified below 10 ng/L in groundwater (82%) and surface water (80%) and below 100 ng/L in wastewater (80%). Relative recoveries were largely between 80 and 120%. Intraday and inter-day precision, expressed as relative standard deviation, were generally better than 10% and 20%, respectively. 50 isotope labeled internal standards were used for quantification and accordingly, relative recoveries as well as intraday and inter-day precision were better for compounds with corresponding internal standard. The applicability of this method was shown during a sampling campaign at a riverbank filtration site for drinking water production with travel times of up to 5 days. 36 substances of all compound classes investigated could be found in concentrations between 0.1 and 600 ng/L. The results revealed the persistence of carbamazepine and sucralose in the groundwater aquifer as well as degradation of the metamizole metabolite 4-acetamidoantipyrine. PMID:23137864

  18. Determination of CMPO using HPLC -UV

    Energy Technology Data Exchange (ETDEWEB)

    Gracy Elias; Gary S. Groenewold; Bruce J. Mincher; Stephen P. Mezyk

    2012-06-01

    Octyl(phenyl)-N,N-diisobutylcarbamoylmethylphosphine oxide (CMPO) is an extractant proposed for selective separation of radionuclide metals from used nuclear fuel solutions using solvent extraction. Radiolysis reactions can degrade CMPO and reduce separation performance and hence methods for measuring concentration of CMPO and identifying degradation products are needed. A novel high performance liquid chromatography (HPLC) method employing ultraviolet detection (UV) was developed to detect and quantitate CMPO in dodecane. Some radiolysis products in gamma and alpha irradiated CMPO solutions were identified using HPLC/electrospray ionization-mass spectrometry (ESI-MS). Validation data indicated that the HPLC-UV method for CMPO determination provided good linearity, sensitivity, procedure accuracy and system precision. CMPO-nitric acid complexes were also identified, that account for the apparent loss of CMPO in acidic environment, independent of irradiation.

  19. Speciation of four selenium compounds using high performance liquid chromatography with on-line detection by inductively coupled plasma mass spectrometry or flame atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Pedersen, Gitte Alsing; Larsen, Erik Huusfeldt

    1997-01-01

    with an aqueous solution of 6 mmol L-1 of salicylate ion at pH 8.5 as the mobile phase which allowed the isocratic separation of the four selenium analytes within 8 minutes. The separated selenium species were detected on-line by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma mass...... spectrometry (ICP-MS). The signal-to-noise ratio of the FAAS detector was optimized using a hydrogen-argon entrained-air flame and a slotted-tube atom trap (STAT) in the flame. The limit of detection (3 sigma) achieved by the HPLC-FAAS system was 1 mg L-1 of selenium (100 mu L injections) for each of the four...

  20. Determination of aflatoxin B1 in cereals by homogeneous liquid-liquid extraction coupled to high performance liquid chromatography-fluorescence detection.

    Science.gov (United States)

    Sheijooni-Fumani, Neda; Hassan, Jalal; Yousefi, Seyed R

    2011-06-01

    A simple and rapid method based on homogeneous liquid-liquid extraction coupled to HPLC with fluorescence detection was developed for the determination of aflatoxin B1 (AFB1) in the rice and grain samples after post-column derivatization. The proposed method eliminated the use of immunoaffinity columns for clean-up in the determination of AFB1. The parameters affecting recovery and preconcentration such as type and volume of organic solvent, volume ratio of water/methanol, concentration of phase separator reagent and extraction time were optimized. Under the optimized conditions, the calibration graph was linear in the concentration range of 0.01-1.0 ng/g with the detection limit of 0.003 ng/g. This method was successfully applied for the analysis of AFB1 in different cereal samples. PMID:21491592

  1. Determination of rare-earth elements in geological materials by ion-exchange chromatography separation and induction coupled plasma emission spectroscopy

    International Nuclear Information System (INIS)

    A methodology for the analysis of Rare-Earth elements in geological samples has been developed. Ion exchange chromatography for the separation and induction coupled plasma emission spectroscopy for the analysis have been used. The columns with cationic resin were calibrated with radioactive elements. With complexes matrices, the instrument's data must be corrected for the presence of majors elements (CEM) and for the interferences of the Rare-earth elements (CETR). The accuracy and precision are evaluated critically with respect to the convenience and efficiency of this methodology in the analysis of rare-Earth elements i geological samples. (author)

  2. Analyses of nitrobenzene,benzene and aniline in environmental water samples by headspace solid phase micro-extraction coupled with gas chromatography-mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    CHEN Ming; YIN Yongguang; TAI Chao; ZHANG Qinghua; LIU Jiyan; HU Jingtian; JIANG Guibin

    2006-01-01

    A headspace solid phase microextraction coupled with gas chromatography mass spectrometry (HS-SPME/GC-MS) method was established for analyzing nitrobenzene, benzene and aniline in environmental water samples simultaneously.Factors affecting extraction efficiency (SPME fiber selection, acidity, temperature, salt addition, extraction time, headspace, etc) were verified. Under optimal extraction conditions, the detection limits are 0.50, 0.11 and 1.00 μg/L for nitrobenzene, benzene and aniline, respectively. The results indicate that this method is capable of making sensitive and accuracy analyses on nitrobenzene, benzene and aniline in environmental water samples.

  3. Metabonomic Study of Biochemical Changes in Human Hair of Heroin Abusers by Liquid Chromatography Coupled with Ion Trap-Time of Flight Mass Spectrometry.

    Science.gov (United States)

    Xie, Pu; Wang, Tie-jie; Yin, Guo; Yan, Yan; Xiao, Li-he; Li, Qing; Bi, Kai-shun

    2016-01-01

    Hair analysis is with the advantage of non-invasive collection and long surveillance window. The present study employed a sensitive and reliable liquid chromatography coupled with ion trap-time of flight mass spectrometry method to study the metabonomic characters in the hair of 58 heroin abusers and 72 non-heroin abusers. Results indicated that certain endogenous metabolites, such as sorbitol and cortisol, were accelerated, and the level of arachidonic acid, glutathione, linoleic acid, and myristic acid was decreased in hair of heroin abusers. The metabonomic study is helpful for further understanding of heroin addiction and clinical diagnosis. PMID:26445826

  4. Separation of seven arsenic compounds by high-performance liquid chromatography with on-line detection by hydrogen–argon flame atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, S. H.; Larsen, E. H.; Pritzl, G.;

    1992-01-01

    of mixtures of arsenic standards into the HPLC system were: arsenite, As(III) 1.1; arsenate, As(V) 1.4; MMA 1.4; DMA 0.7; AsB 0.3; AsC 0.5; and the TMAs 0.4. The HPLC-AAS system was used for the analysis of arsenic species in aqueous extracts of soil samples from a polluted land site. Only arsenate was found......Seven molecular forms of arsenic were separated by anion- and cation-exchange high-performance liquid chromatography (HPLC) with on-line detection by flame atomic absorption spectrometry (FAAS). The interfacing was established by a vented poly(tetrafluoroethylene) capillary tubing connecting...... the HPLC column to the nebulizer of the atomic absorption spectrometer. Arsenite, arsenate, monomethylarsonate (MMA) and dimethylarsinate (DMA) were separated from each other and from the co-injected cationic arsenic compounds, arsenobetaine (AsB), arsenocholine (AsC) and the tetramethylarsonium ion (TMAs...

  5. Separation of seven arsenic compounds by high performance liquid chromatography with on-line detection by hydrogen-argon flame atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, S. H.; Larsen, Erik Huusfeldt; Pritzl, G.;

    1992-01-01

    of mixtures of arsenic standards into the HPLC system were: arsenite, As(III) 1.1; arsenate, As(V) 1.4; MMA 1.4; DMA 0.7; AsB 0.3; AsC 0.5; and the TMAs 0.4. The HPLC-AAS system was used for the analysis of arsenic species in aqueous extracts of soil samples from a polluted land site. Only arsenate was found......Seven molecular forms of arsenic were separated by anion- and cation-exchange high-performance liquid chromatography (HPLC) with on-line detection by flame atomic absorption spectrometry (FAAS). The interfacing was established by a vented poly(tetrafluoroethylene) capillary tubing connecting...... the HPLC column to the nebulizer of the atomic absorption spectrometer. Arsenite, arsenate, monomethylarsonate (MMA) and dimethylarsinate (DMA) were separated from each other and from the co-injected cationic arsenic compounds, arsenobetaine (AsB), arsenocholine (AsC) and the tetramethylarsonium ion (TMAs...

  6. Arsenic-containing fatty acids and hydrocarbons in marine oils - Determination using reversed-phase HPLC-ICP-MS and HPLC-qTOF-MS

    DEFF Research Database (Denmark)

    Sele, Veronika; Sloth, Jens Jørgen; Holmelid, Bjarte;

    2014-01-01

    concentrations from 1.6 to 12.5 mg kg-1 oil, were analyzed for arsenolipids using reversed-phase high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry (HPLC-ICP-MS). The arsenolipids were quantified using three different arsenic-containing calibration standards......Arsenolipids are the major arsenic species present in marine oils. Several structures of arsenolipids have been elucidated the last 5 years, demonstrating the chemical complexity of this trace element in the marine environment. Several commercial fish oils and marine oils, ranging in total arsenic...... for the quantification of arsenolipids, with recoveries between 91% and 104% compared to total arsenic measurements in the same extracts. A range of marine oils was investigated, including oils of several fish species, cod liver and seal, as well as three commercial fish oils. The AsHCs - C17H38AsO, C19H42AsO and C23H38...

  7. Determination of polar pesticides in olive oil and olives by hydrophilic interaction liquid chromatography coupled to tandem mass spectrometry and high resolution mass spectrometry.

    Science.gov (United States)

    Nortes-Méndez, Rocío; Robles-Molina, José; López-Blanco, Rafael; Vass, Andrea; Molina-Díaz, Antonio; Garcia-Reyes, Juan F

    2016-09-01

    This article reports the development of two HPLC-MS methods for the determination of polar pesticides in olive oil and olive samples by hydrophilic interaction liquid chromatography (HILIC) separation followed by mass spectrometry detection with tandem mass spectrometry using a triple quadrupole instrument operated in multiple reaction monitoring mode (HILIC-MS/MS) or electrospray time-of-flight mass spectrometry (HILIC-TOFMS). The selected polar pesticides included in the study were: amitrol, cyromazine, diquat, paraquat, mepiquat, trimethylsulfonium (trimesium, glyphosate counterion) and fosetyl aluminium. The simple sample treatment procedure was based on liquid partitioning with methanol. The performance of the sample extraction was evaluated in terms of recovery rates and matrix effects in both olive oil and olives matrices. The results obtained for olive oil were satisfactory while, due to the high complexity of olives, poor recovery rates were obtained for the extraction of diquat, paraquat and amitrol, although with a reasonable precision enabling its use in routine analysis. Similarly, matrix effects were minor in the case of olive oil (ca. 20% suppression average), while significantly higher suppression was observed for olives (30-50% suppression average). The studied approaches were found to be useful for the determination of the pesticides studied in olive oil and olives with limits of quantitation below 5µgkg(-1) in most cases when tandem mass spectrometry was used, thus being in compliance with MRLs set by current EU regulation. PMID:27343599

  8. Biological Fingerprinting Analysis of Interaction Between Taxoids in Taxus and Microtubule Protein by Microdialysis Coupled with High-performance Liquid Chromatography/Mass Spectrometry for Screening Antimicrotubule Agents

    Institute of Scientific and Technical Information of China (English)

    LEI Xiao-yuan; KONG Liang; SU Xing-ye; GUO Ming; ZOU Han-fa

    2008-01-01

    Some natural products,such as traditional Chinese medicines(TCMs),contain compounds with anticancer activity and have attracted a great interest in recent years as alternative anticancer therapies,A quick and convenient assay for screening antimicrotubule compounds in which in vitro microdialysis/high-performance liquid chromatography(HPLC) is used to monitor the binding of the compounds extracted from TCM Taxus cuspidata Siebold & Zucc(Taxus)to microtubules is reported,It was observed that the extract of Taxus contains at least five compounds which have affinity interaction with microtubules by biological fingerprinting analysis,and they were identified as the taxoids of taxol,baccatin Ⅲ,10-deacetylbaccatin Ⅲ(10-DAB),cephalomannine and 7-epi-10-deacetyltaxol (7-epi-10-DAT) based on the comparison of their high-performance liquid chromatographic/mass spectrometric and UV spectra with those of the standard samples,both assembly-promoting and disassembly-inhibiting characteristics of those compounds were evaluated,It was observed that baccatin Ⅲ and 10-DAB bound to microtubules and the binding degrees were influenced by GTP,Competitive binding behavior of taxol with other four taxoids to microtubules was also investigated.

  9. Development of the H-point standard additions method for coupled liquid-chromatography and UV-visible spectrophotometry

    International Nuclear Information System (INIS)

    This work establishes the fundamentals of the H-point standard additions method for liquid chromatography for the simultaneous analysis of binary mixtures with overlapped chromatographic peaks. The method was compared with the deconvolution method of peak suppression and the second derivative of elution profiles. Different mixtures of diuretics were satisfactorily resolved. (author). 21 refs.; 9 figs.; 2 tabs

  10. Signal and Charge Enhancement for Protein Analysis by Liquid Chromatography-Mass Spectrometry with Desorption Electrospray Ionization

    OpenAIRE

    Liu, Yan; Miao, Zhixin; Lakshmanan, Rajeswari; Ogorzalek Loo, Rachel R.; Loo, Joseph A.; Chen, Hao

    2012-01-01

    We recently reported the use of desorption electrospray ionization (DESI) as a novel interface to couple high-performance liquid chromatography (HPLC) with mass spectrometry (MS) (Chem. Commun. 2011, 47, 4171). One of the benefits of such an interface is that post-column derivatization of separated analytes can be integrated with ionization via a “reactive” DESI approach in which a derivatizing reagent is doped into the spray solvent. The reactive DESI interface allows analyte desorption/ioni...

  11. Simultaneous analysis of eight bioactive compounds in Danning tablet by HPLC-ESI-MS and HPLC-UV.

    Science.gov (United States)

    Liu, Runhui; Zhang, Jiye; Liang, Mingjin; Zhang, Weidong; Yan, Shikai; Lin, Min

    2007-02-19

    A high performance liquid chromatography (HPLC) coupled with electrospray tandem mass spectrometry (ESI-MS) and ultraviolet detector (UV) has been developed for the simultaneous analysis of eight bioactive compounds in Danning tablet (including hyperin, hesperidin, resveratrol, nobiletin, curcumine, emodin, chrysophanol, and physcion), a widely used prescription of traditional Chinese medicine (TCM). The chromatographic separation was performed on a ZORBAX Extend C(18) analytical column by gradient elution with acetonitrile and formate buffer (containing 0.05% formic acid, adjusted with triethylamine to pH 5.0) at a flow rate of 0.8 ml/min. The eight compounds in Danning tablet were identified and their MS(n) fractions were elucidated by using HPLC-ESI-MS, and the contents of these compounds were determined by using HPLC-UV method. The standard calibration curves were linear between 5.0 and 100 microg/ml for hyperin, 10-200 microg/ml for hesperidin, 1.0-150 microg/ml for resveratrol, 2.0-120 microg/ml for nobiletin, 2.0-225 microg/ml for curcumine, 20-300 microg/ml for emodin, 2.0-200 microg/ml for chrysophanol, and 20-250 microg/ml for physcion with regression coefficient r(2)>0.9995. The intra-day and inter-day precisions of this method were evaluated with the R.S.D. values less than 0.7% and 1.3%, respectively. The recoveries of the eight investigated compounds were ranged from 99.3% to 100.2% with R.S.D. values less than 1.5%. This method was successfully used to determine the 8 target compounds in 10 batches of Danning tablet. PMID:17079108

  12. Automated derivatization and fluorimetric determination of biogenic amines in milk by zone fluidics coupled to liquid chromatography.

    Science.gov (United States)

    Notou, Maria; Zotou, Anastasia; Tzanavaras, Paraskevas D; Themelis, Demetrius G

    2014-08-22

    A novel zone-fluidics/high pressure liquid chromatographic (ZF-HPLC) method is described for the simultaneous determination of six biogenic monoamines, in the presence of hexylamine as internal standard. Automated on-line derivatization of the analytes with naphthalene-2,3-dicarboxaldehyde/cyanide ions was performed using the ZF concept and the derivatives were injected on the HPLC column for separation/detection. The influence of the ZF operation conditions on the derivatization reaction was investigated. The isoindoles formed were separated on a Kromasil C18 column (250 mm × 4 mm i.d., 5 μm), using an isocratic mobile phase of methanol/water (80:20, v/v) at a flow rate of 1.0 mL min(-1). Monitoring and quantification was carried out by fluorescence detection at 424/494 nm. The limits of detection were at the pg level with a sample volume of 20 μL. The whole procedure was evaluated and fully validated for the determination of biogenic amines in milk samples. PMID:24986070

  13. A High Performance Liquid Chromatography-Mass Spectrometry (HPLC-MS) Qualitative Detection Method Developed for In Vivo Analyses of Toxin Orellanine from the Cortinarius orellanus Fr.—Part II

    OpenAIRE

    Ilia Brondz; Anton Brondz

    2012-01-01

    The high-performance liquid chromatography—mass spectrometry (HPLC-MS) qualitative analysis method in negative mode of detection was used to record the presence of orellanine in the stomach contents of rats after ingestion of Cortinarius orellanus. Intoxication with orellanine causes acute renal failure (ARF), which is characterized by sudden loss of the ability of the kidneys to excrete wastes. The detection method presented here can be used as a platform for future development of analytical...

  14. High performance liquid chromatography-charged aerosol detection applying an inverse gradient for quantification of rhamnolipid biosurfactants.

    Science.gov (United States)

    Behrens, Beate; Baune, Matthias; Jungkeit, Janek; Tiso, Till; Blank, Lars M; Hayen, Heiko

    2016-07-15

    A method using high performance liquid chromatography coupled to charged-aerosol detection (HPLC-CAD) was developed for the quantification of rhamnolipid biosurfactants. Qualitative sample composition was determined by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). The relative quantification of different derivatives of rhamnolipids including di-rhamnolipids, mono-rhamnolipids, and their precursors 3-(3-hydroxyalkanoyloxy)alkanoic acids (HAAs) differed for two compared LC-MS instruments and revealed instrument dependent responses. Our here reported HPLC-CAD method provides uniform response. An inverse gradient was applied for the absolute quantification of rhamnolipid congeners to account for the detector's dependency on the solvent composition. The CAD produces a uniform response not only for the analytes but also for structurally different (nonvolatile) compounds. It was demonstrated that n-dodecyl-β-d-maltoside or deoxycholic acid can be used as alternative standards. The method of HPLC-ultra violet (UV) detection after a derivatization of rhamnolipids and HAAs to their corresponding phenacyl esters confirmed the obtained results but required additional, laborious sample preparation steps. Sensitivity determined as limit of detection and limit of quantification for four mono-rhamnolipids was in the range of 0.3-1.0 and 1.2-2.0μg/mL, respectively, for HPLC-CAD and 0.4 and 1.5μg/mL, respectively, for HPLC-UV. Linearity for HPLC-CAD was at least 0.996 (R(2)) in the calibrated range of about 1-200μg/mL. Hence, the here presented HPLC-CAD method allows absolute quantification of rhamnolipids and derivatives. PMID:27283098

  15. Extraction and characterization of polysaccharides from Semen Cassiae by microwave-assisted aqueous two-phase extraction coupled with spectroscopy and HPLC.

    Science.gov (United States)

    Chen, Zhi; Zhang, Wei; Tang, Xunyou; Fan, Huajun; Xie, Xiujuan; Wan, Qiang; Wu, Xuehao; Tang, James Z

    2016-06-25

    A novel and rapid method for simultaneous extraction and separation of the different polysaccharides from Semen Cassiae (SC) was developed by microwave-assisted aqueous two-phase extraction (MAATPE) in a one-step procedure. Using ethanol/ammonium sulfate system as a multiphase solvent, the effects of MAATPE on the extraction of polysaccharides from SC such as the composition of the ATPS, extraction time, temperature and solvent-to-material ratio were investigated by UV-vis analysis. Under the optimum conditions, the yields of polysaccharides were 4.49% for the top phase, 8.80% for the bottom phase and 13.29% for total polysaccharides, respectively. Compared with heating solvent extraction and ultrasonic assisted extraction, MAATPE exhibited the higher extraction yields in shorter time. Fourier-transform infrared spectra showed that two polysaccharides extracted from SC to the top and bottom phases by MAATPE were different from each other in their chemical structures. Through acid hydrolysis and PMP derivatization prior to HPLC, analytical results by indicated that a polysaccharide of the top phases was a relatively homogeneous homepolysaccharide composed of dominant gucose glucose while that of the bottom phase was a water-soluble heteropolysaccharide with multiple components of glucose, xylose, arabinose, galactose, mannose and glucuronic acid. Molar ratios of monosaccharides were 95.13:4.27:0.60 of glucose: arabinose: galactose for the polysaccharide from the top phase and 62.96:14.07:6.67: 6.67:5.19:4.44 of glucose: xylose: arabinose: galactose: mannose: glucuronic acid for that from the bottom phase, respectively. The mechanism for MAATPE process was also discussed in detail. MAATPE with the aid of microwave and the selectivity of the ATPS not only improved yields of the extraction, but also obtained a variety of polysaccharides. Hence, it was proved as a green, efficient and promising alternative to simultaneous extraction of polysaccharides from SC. PMID

  16. Screening and analyzing the potential bioactive components from reduning injection, using macrophage cell extraction and ultra-high performance liquid chromatography coupled with mass spectrometry.

    Science.gov (United States)

    Li, Yonghui; Wang, Peixiang; Xiao, Wei; Zhao, Li; Wang, Zhenzhong; Yu, Li

    2013-01-01

    In this paper, a useful method for screening and analyzing the potential bioactive components from Reduning Injection was developed using macrophage cell extraction and ultra-high performance liquid chromatography coupled with Q-TOF/MS spectrometry. In addition, the protective effects on macrophage cell damage induced by LPS in vitro were also investigated. The results showed that chlorogenic acid, 3, 4-dicaffeoylquinic acid, 3, 5-dicaffeoylquinic acid and 4, 5-dicaffeoylquinic acid significantly inhibited the prostaglandin E(2) (PGE(2)) release and reversed the interleukin-6 (IL-6) secretion of macrophages (p extraction coupled with UPLC-MS technology is feasible, rapid and useful for screening and analyzing potential bioactive components from TCM injection. PMID:23336518

  17. Coupling of size-exclusion chromatography to liquid chromatography/mass spectrometry for determination of trace levels of thifensulfuron-methyl and tribenuron-methyl in cottonseed and cotton gin trash.

    Science.gov (United States)

    Stry, J J; Amoo, J S; George, S W; Hamilton-Johnson, T; Stetser, E

    2000-01-01

    Size-exclusion chromatography (SEC) was coupled to reversed-phase liquid chromatography/mass spectrometry for the determination of thifensulfuron-methyl and tribenuron-methyl in cottonseed and cotton gin trash. The limit of quantitation was 20 parts per billion (ppb), and the limit of detection was 6 ppb. The analytes were extracted by homogenization in a buffer solution. The extracts underwent a solvent exchange into methanol and were injected onto an SEC column. As the analytes eluted from the SEC column, the eluate was diverted onto a reversed-phase column for additional separation of the analytes and their detection via mass spectrometry. This method is unique because the samples are not cleaned up before analysis, the analytes are injected in methanol, and the entire analysis is completed in 30 min. Average recoveries and standard deviations for thifensulfuronmethyl and tribenuron-methyl in cotton gin trash were 91 +/- 6% and 88 +/- 5%, respectively. Average recoveries and standard deviations for thifensulfuron-methyl and tribenuron-methyl in cottonseed were 91 +/- 11% and 99 +/- 12%, respectively. This is an effective method for the detection and determination of thifensulfuron-methyl and tribenuron-methyl in cotton. PMID:10868588

  18. Quantification of appetite suppressing steroid glycosides from Hoodia gordonii in dried plant material, purified extracts and food products using HPLC-UV and HPLC-MS methods

    NARCIS (Netherlands)

    H.-G. Janssen; C. Swindells; P. Gunning; W. Wang; C. Grün; K. Mahabir; V.J. Maharaj; P.J. Apps

    2008-01-01

    High-performance liquid chromatography (HPLC)-UV and HPLC-Mass Spectrometry (MS) methods were developed for the quantitative analysis of the family of Hoodia gordonii steroid glycosides with appetite suppressing properties in dried plant material, in purified and enriched extracts and in various pro

  19. Analysis of volatile organic compounds in pleural effusions by headspace solid-phase microextraction coupled with cryotrap gas chromatography and mass spectrometry.

    Science.gov (United States)

    Huang, Zhongping; Zhang, Jie; Zhang, Peipei; Wang, Hong; Pan, Zaifa; Wang, Lili

    2016-07-01

    Headspace solid-phase microextraction coupled with cryotrap gas chromatography and mass spectrometry was applied to the analysis of volatile organic compounds in pleural effusions. The highly volatile organic compounds were separated successfully with high sensitivity by the employment of a cryotrap device, with the construction of a cold column head by freezing a segment of metal capillary with liquid nitrogen. A total of 76 volatile organic compounds were identified in 50 pleural effusion samples (20 malignant effusions and 30 benign effusions). Among them, 34 more volatile organic compounds were detected with the retention time less than 8 min, by comparing with the normal headspace solid-phase microextraction coupled with gas chromatography and mass spectrometry method. Furthermore, 24 volatile organic compounds with high occurrence frequency in pleural effusion samples, 18 of which with the retention time less than 8 min, were selected for the comparative analysis. The results of average peak area comparison and box-plot analysis showed that except for cyclohexanone, 2-ethyl-1-hexanol, and tetramethylbenzene, which have been reported as potential cancer biomarkers, cyclohexanol, dichloromethane, ethyl acetate, n-heptane, ethylbenzene, and xylene also had differential expression between malignant and benign effusions. Therefore, the proposed approach was valuable for the comprehensive characterization of volatile organic compounds in pleural effusions. PMID:27159330

  20. Circulating ultrasound-assisted extraction, countercurrent chromatography, and liquid chromatography for the simultaneous extraction, isolation, and analysis of the constituents of Uncaria tomentosa.

    Science.gov (United States)

    Zhang, Yuchi; Liu, Chunming; Qi, Yanjuan; Li, Sainan; Pan, Yan; Li, Yuchun

    2015-04-01

    A hyphenated automated technique for the online extraction, isolation, analysis, and identification of natural organic compounds was established. Circulating ultrasound-assisted extraction (CUAE) was coupled with countercurrent chromatography (CCC), high performance liquid chromatography (HPLC), and a diode array detector (DAD). This approach was applied to the fractionation and purification of alkaloids from Uncaria tomentosa. A biphasic solvent system of chloroform-methanol-water (6:4:5, v:v:v) was used for the CUAE and CCC separation of compounds from 500 g of U. tomentosa. Two CUAE/CCC/HPLC/DAD modes were established. Either the upper aqueous phase or the lower organic phase of the solvent system could be used as the extraction solvent. The target compounds were extracted by CUAE, and the extract was pumped into a sample loop before being directly injected into the CCC column, or pre-purified using a flash chromatography column before injection. The target compounds were eluted using either the organic or aqueous phase of the solvent system and the fractions were monitored using a UV detector. The target fractions were collected by a sample loop via a six-port valve, and analyzed by HPLC/DAD for purity and structural identification. This system isolated of 8.2mg, 7.4 mg, and 12.9 mg of rhynchophylline, corynoxine, and corynoxine B with HPLC purities of 96.15%, 95.34%, and 95.49%, respectively via the first mode; and isolated 26.6 mg, 24.6 mg, and 45.3mg of rhynchophylline, corynoxine, and corynoxine B with a HPLC purities of 98.22%, 97.18%, and 97.93% via the second mode. PMID:25725954

  1. Determination of occluded oxygen, nitrogen and hydrogen in zircalloy-4 by vacuum extraction coupled to gas chromatography

    International Nuclear Information System (INIS)

    The technique of vacuum extraction at high temperatures was used for the liberation of gases from zircalloy-4 samples; oxygen, nitrogen and hydrogen were quantitatively analysed by gas chromatography. Two different sets of zircalloy-4 samples were examined. The results for O2, N2 and H2 quantitative analyses satisfy the requirements for the characterization of the zircalloy-4 quality. (C.L.B.)

  2. Quantification of the antifungal lipopeptide iturin A by high performance liquid chromatography coupled with aqueous two-phase extraction.

    Science.gov (United States)

    Yuan, Jun; Raza, Waseem; Huang, Qiwei; Shen, Qirong

    2011-09-15

    Iturin A, a powerful antifungal surfactant, is a kind of bacterial lipopeptide produced by Bacillus strains. This study addresses the use of an aqueous two-phase system (ATPS) using ethanol/ammonium sulfate to extract iturin A from Bacillus amyloliquefaciens NJN-6 fermentation broth and the quantification of iturin A by HPLC. Baseline separation of iturin A homologues was performed using an RP-C(18) column with a mixture of water and acetonitrile. The results showed that the correlation coefficient between integral area and concentration was 0.9961 within the range of 20-140 mg/l. The RSD of the retention time and the peak area were 1.29% and 1.45%, respectively. The effects of some operating parameters in ATPS, e.g., pH, temperature and centrifugation time, were also studied. This method can be successfully used for the rapid quantification of iturin A. PMID:21872538

  3. Vortex-Assisted Dispersive Micro-Solid Phase Extraction Using CTAB-Modified Zeolite NaY Sorbent Coupled with HPLC for the Determination of Carbamate Insecticides.

    Science.gov (United States)

    Salisaeng, Pawina; Arnnok, Prapha; Patdhanagul, Nopbhasinthu; Burakham, Rodjana

    2016-03-16

    A vortex-assisted dispersive micro-solid phase extraction (VA-D-μ-SPE) based on cetyltrimethylammonium bromide (CTAB)-modified zeolite NaY was developed for preconcentration of carbamate pesticides in fruits, vegetables, and natural surface water prior to analysis by high performance liquid chromatography with photodiode array detection. The small amounts of solid sorbent were dispersed in a sample solution, and extraction occurred by adsorption in a short time, which was accelerated by vortex agitation. Finally, the sorbents were filtered from the solution, and the analytes were subsequently desorbed using an appropriate solvent. Parameters affecting the VA-D-μ-SPE performance including sorbent amount, sample volume, desorption solvent ,and vortex time were optimized. Under the optimum condition, linear dynamic ranges were achieved between 0.004-24.000 mg kg(-1) (R(2) > 0.9946). The limits of detection (LODs) ranged from 0.004-4.000 mg kg(-1). The applicability of the developed procedure was successfully evaluated by the determination of the carbamate residues in fruits (dragon fruit, rambutan, and watermelon), vegetables (cabbage, cauliflower, and cucumber), and natural surface water. PMID:26915268

  4. HPLC-DAD-ESI-MS analysis of phenolic compounds during ripening in exocarp and mesocarp of tomato fruit.

    Science.gov (United States)

    Carrillo-López, Armando; Yahia, Elhadi

    2013-12-01

    Identification of phenolic compounds was done by means of liquid chromatography (HPLC) coupled to mass spectrometry (MS) using the electrospray ionization interface (ESI). Quantification of phenolic compounds was carried out by using HPLC with diode array detector (DAD) in exocarp and mesocarp of tomato fruit at 6 different ripeness stages (mature-green, breakers, turning, pink, light-red, and red). Several phenolic compounds were identified including chlorogenic acid, caffeic acid, p-coumaric acid, ferulic acid, and rutin and some combined phenolic acids were tentatively identified, mainly glycosides, such as caffeoyl hexose I, caffeoyl hexose II, caffeoylquinic acid isomer, dicaffeoylquinic acid, p-coumaroyl hexose I, p-coumaroyl hexose II, feruloyl hexose I, feruloyl hexose II, siringyl hexose, and caffeoyl deoxyhexose hexose. Fruit exocarp had higher quantities of total soluble phenolics (TSP) compared to mesocarp. During ripening, TSP increased in both exocarp and mesocarp, mainly in exocarp. While rutin increased, chlorogenic acid decreased in both tissues: exocarp and mesocarp. PMID:24171765

  5. Simultaneous determination of arsenic, selenium and antimony species using HPLC/ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Lindemann, T.; Prange, A.; Neidhart, B. [GKSS-Forschungszentrum Geesthacht GmbH (Germany). Inst. fuer Physikalische und Chemische Analytik; Dannecker, W. [Univ. of Hamburg (Germany). Inst. for Inorganic and Applied Chemistry

    1999-07-01

    A new method for the simultaneous separation and determination of four arsenic species [As(III), As(V), monomethylarsonic acid and dimethylarsinic acid], three selenium species [Se(IV), Se(VI) and selenomethionine] as well as Sb(III) and Sb(V) is presented. The speciation was achieved by on-line coupling of anion exchange high-performance liquid chromatography (HPLC) with inductively coupled plasma mass spectrometry (ICP-MS). Chromatographic parameters such as the composition and pH of the mobile phase were optimised. Limits of detection are below 4.5 {mu}g L{sup -1} (as element) for Sb(III) and the selenium species and below 0.5 {mu}g L{sup -1} for the other species. Precisions of retention times were better than 2% RSD and of peak areas better than 8% RSD for all the species investigated. (orig.) With 5 figs., 3 tabs., 41 refs.

  6. A quantitative assay for reductive metabolism of a pesticide in fish using electrochemistry coupled with liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Bussy, Ugo; Chung-Davidson, Yu-Wen; Li, Ke; Li, Weiming

    2015-04-01

    This is the first study to use electrochemistry to generate a nitro reduction metabolite as a standard for a liquid chromatography-mass spectrometry-based quantitative assay. This approach is further used to quantify 3-trifluoromethyl-4-nitrophenol (TFM) reductive metabolism. TFM is a widely used pesticide for the population control of sea lamprey (Petromyzon marinus), an invasive species of the Laurentian Great Lakes. Three animal models, sea lamprey, lake sturgeon (Acipenser fulvescens), and rainbow trout (Oncorhynchus mykiss), were selected to evaluate TFM reductive metabolism because they have been known to show differential susceptibilities to TFM toxicity. Amino-TFM (aTFM; 3-trifluoromethyl-4-aminophenol) was the only reductive metabolite identified through liquid chromatography-high-resolution mass spectrometry screening of liver extracts incubated with TFM and was targeted for electrochemical synthesis. After synthesis and purification, aTFM was used to develop a quantitative assay of the reductive metabolism of TFM through liquid chromatography and tandem mass spectrometry. The concentrations of aTFM were measured from TFM-treated cellular fractions, including cytosolic, nuclear, membrane, and mitochondrial protein extracts. Sea lamprey extracts produced the highest concentrations (500 ng/mL) of aTFM. In addition, sea lamprey and sturgeon cytosolic extracts showed concentrations of aTFM substantially higher than those of rainbow trout. However, other fractions of lake sturgeon extracts tend to show aTFM concentrations similar to those of rainbow trout but not with sea lamprey. These data suggest that the level of reductive metabolism of TFM may be associated with the sensitivities of the animals to this particular pesticide. PMID:25730707

  7. Identification of Perfluorooctanoic Acid Release from Commercial Coated Cooking Pans by Liquid Chromatography Coupled to Electrospray Ionization Tandem Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Monica Bononi

    2007-01-01

    Full Text Available Salts of perfluorooctanoic acid (PFOA can be used in the manufacture of fluoropolymers employed for coating pans; moreover, PFOA can be formed as a byproduct of thermolysis of the aforesaid fluoropolymers. This study was carried out to evaluate PFOA migration into food cooked in fluoropolymer-coated pans. The pans were purchased from a local retailer and subjected to cooking conditions. Used oil was extracted with a methanol/water solution and analyzed by liquid chromatography tandem mass spectrometry (LC/MS/MS. We found that PFOA can enter cooked food during a container's first phases of use, not only in containers already abused by kitchen tools or otherwise scratched.

  8. Determination of aflatoxins in food by immunoaffinity chromatography-high performance liquid chromatography fluorescence detector coupled with post-column photochemical derivatization%免疫亲和柱净化-高效液相色谱柱后光化学衍生-荧光检测器检测食品中黄曲霉毒素

    Institute of Scientific and Technical Information of China (English)

    薛昆鹏; 郭会琴; 余冲; 汪超; 蓝凯; 赵岳星

    2015-01-01

    ABSTRACT:Objective To establish an immunoaffinity chromatography-high performance liquid chromatography (HPLC) fluorescence detector coupled with post-column photochemical derivatization method for determination of the aflatoxin B1, B2, G1, and G2 in food.Methods The sample was tested by HPLC with fluorescence detector after being homogenizer extracted from methanol-water (70:30,V:V), purified by immunoaffinity chromatography column of aggregated aflatoxin, separated by Welch Ultimate®XB-C18 HPLC column, eluted with a mobile phase consisting of methanol and waters (45:55,V:V) and derived from post column photochemical derivative reactor. The content of aflatoxin B1, B2, G1, and G2 in food was measured using peak area external standard method.ResultsThe calibration curves showed a good linearity in each concentration range with correlation coefficient greater than 0.999 within linear range 0.3~50.0 µg/L. The limits of detection (LODs) were 0.15, 0.05, 0.15 and 0.05μg/kg for the aflatoxins B1, B2, G1, and G2 in food, respectively. The recovery rate was within 80.7 %~92.6 % at 3 adding levels with the relative standard deviation (RSDs) of 2.04~3.87%.ConclusionThis method is sensitive, accurate and precise, which is in accordance with technical standards of the aflatoxins detection. It is proper for routine detection of the aflatoxins B1, B2, G1, and G2 in food.%目的:建立一种免疫亲和固相萃取柱净化-高效液相色谱柱后光化学衍生-荧光检测器同时测定食品中黄曲霉毒素B1、B2、G1和G2的方法。方法以甲醇-水(70:30, V:V)为提取溶剂,采用高速均质提取,并经过黄曲霉毒素免疫亲和柱净化。结果经月旭公司Welch Ultimate® XB-C18色谱柱(250 mm×4.6 mm,5μm)分离后使用光化学衍生器进行柱后衍生,并采用带荧光检测器的高效液相色谱仪检测,流动相为甲醇/水(45:55,V:V)。黄曲霉毒素B1、B2、G1和G2线性范围在0.3~50.0µg/L之

  9. Trace amounts of rare earth elements in high purity samarium oxide by sector field inductively coupled plasma mass spectrometry after separation by HPLC

    International Nuclear Information System (INIS)

    Today there is an increasing need for high purity rare earth compounds in various fields, the optical, the electronics, the ceramic, the nuclear and geochemistry. Samarium oxide has special uses in glass, phosphors, lasers and thermoelectric devices. Calcium chloride crystals treated with samarium have been employed in lasers, which produce light beams intense enough to burn metal. In general, the inductively coupled plasma mass spectrometry (ICP-MS) presents some advantages for trace element analysis, due to high sensitivity and resolution, when compared with other analytical techniques such as ICP optical emission spectrometry (ICP-OES). In this work, sector field inductively coupled plasma mass spectrometry was used. Sixteen elements (Sc, Y and 14 lanthanides) were determined selectively with the ICP-MS system using a concentration gradient method. The detection limits with the ICP-MS system were about 0.2 (La) pg mL-1 to 8 (Gd) pg mL-1. The %R.S.D. of the methods varying between 0.9 and 1.5% for a set of five (n = 5) replicates was found for the IPEN's material and for the certificate reference sample. Determination of trace REEs in two high pure samarium oxides samples (IPEN and JMC) was performed. IPEN's material is highly pure (>99.99%) and was successfully analyzed without spectral interference (MO+ and MOH+)

  10. Detection in superheated water chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Chienthavorn, O

    1999-11-01

    Superheated water has been used successfully as an eluent in liquid chromatography and has been coupled to various modes of detection, ultraviolet (UV), fluorescence, and nuclear magnetic resonance spectroscopy (NMR) and mass spectrometry (MS). A number of compounds were examined on poly(styrene-divinylbenzene) (PS-DVB), polybutadiene (PBD), and octadecylsilyl bonded silica (ODS) column with isothermal and temperature programmes. The PS-DVB column was mostly used throughout the project as it was the most stable. Not only pure water could serve as superheated water mobile phase; inorganic buffered water and ion-pairing reagent with a concentration of 1-3 mM of the buffer and reagent were also exploited. It was shown that the pH could be controlled during the separation without salt precipitation and the separations followed a conventional reversed-phase HPLC method. Results from fluorescence detection showed good separation of a series of vitamins, such as pyridoxine, riboflavin, thiamine, and some analgesics. The relationship of riboflavin using the detection was linear and the detection limit was seven times higher than that of a conventional method. Simultaneous separation and identification using superheated water chromatography-NMR was demonstrated. With using a stop flow method, NMR spectra of model drugs, namely barbiturates, paracetamol, caffeine and phenacetin were obtained and the results agreed with reference spectra, confirming a perfect separation. A demonstration to obtain COSY spectrum of salicylamide was also performed. The method was expanded to the coupling of superheated water LC to NMR-MS. Results from the hyphenated detection method showed that deuteration and degradation happened in the superheated water conditions. The methyl group hydrogens of pyrimidine ring of sulfonamide and thiamine were exchanged with deuterium. Thiamine was decomposed to 4-methyl-5-thiazoleethanol and both were deuterated under the conditions. (author)

  11. Detection in superheated water chromatography

    International Nuclear Information System (INIS)

    Superheated water has been used successfully as an eluent in liquid chromatography and has been coupled to various modes of detection, ultraviolet (UV), fluorescence, and nuclear magnetic resonance spectroscopy (NMR) and mass spectrometry (MS). A number of compounds were examined on poly(styrene-divinylbenzene) (PS-DVB), polybutadiene (PBD), and octadecylsilyl bonded silica (ODS) column with isothermal and temperature programmes. The PS-DVB column was mostly used throughout the project as it was the most stable. Not only pure water could serve as superheated water mobile phase; inorganic buffered water and ion-pairing reagent with a concentration of 1-3 mM of the buffer and reagent were also exploited. It was shown that the pH could be controlled during the separation without salt precipitation and the separations followed a conventional reversed-phase HPLC method. Results from fluorescence detection showed good separation of a series of vitamins, such as pyridoxine, riboflavin, thiamine, and some analgesics. The relationship of riboflavin using the detection was linear and the detection limit was seven times higher than that of a conventional method. Simultaneous separation and identification using superheated water chromatography-NMR was demonstrated. With using a stop flow method, NMR spectra of model drugs, namely barbiturates, paracetamol, caffeine and phenacetin were obtained and the results agreed with reference spectra, confirming a perfect separation. A demonstration to obtain COSY spectrum of salicylamide was also performed. The method was expanded to the coupling of superheated water LC to NMR-MS. Results from the hyphenated detection method showed that deuteration and degradation happened in the superheated water conditions. The methyl group hydrogens of pyrimidine ring of sulfonamide and thiamine were exchanged with deuterium. Thiamine was decomposed to 4-methyl-5-thiazoleethanol and both were deuterated under the conditions. (author)

  12. A reversed-phase high performance liquid chromatography coupled with resonance Rayleigh scattering detection for the determination of four tetracycline antibiotics

    International Nuclear Information System (INIS)

    A new reversed-phase high performance liquid chromatography with resonance Rayleigh scattering detection (HPLC-RRS) was developed for simultaneous separation and determination of four tetracycline antibiotics (TCs). A good chromatographic separation among the compounds was achieved using a Synergi Fusion-RP column (150 mm x 4.6 mm; 4 μm) and a mobile phase consisting of methanol-acetonitrile-oxalic acid (5 mM) at the flow rate of 0.8 mL min-1. Column temperature was 30 deg. C. The RRS signal was detected at λex = λem = 370 nm. The recoveries of sample added standard ranged from 95.3% to 103.5%, and the relative standard deviation was below 2.79%. A detection limit of 2.12-5.12 μg mL-1 was reached and a linear range was found between peak height and concentration in the range of 10.36-518.0 μg mL-1 for oxytetracycline (OTC), 12.11-605.5 μg mL-1 for tetracycline (TC), 11.79-589.5 μg mL-1 for chlortetracycline (CTC) and 10.32-516.0 μg mL-1 for doxycycline (DC). The linear regression coefficients were all above 0.999. The method has been applied successfully to the determination of OTC, TC, CTC, DC in pharmaceutical formulations and in honey. The method was simple, rapid and showed a better linear relation and high repeatability

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

    Directory of Open Access Journals (Sweden)

    Yu-Ling Wang

    2011-03-01

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

  14. Molecularly imprinted sol-gel nanofibers based solid phase microextraction coupled on-line with high performance liquid chromatography for selective determination of acesulfame.

    Science.gov (United States)

    Moein, Mohammad Mahdi; Javanbakht, Mehran; Karimi, Mohammad; Akbari-adergani, Behrouz

    2015-03-01

    Sol-gel based molecularly imprinted polymer (MIP) nanofiber was successfully fabricated by electrospinning technique on the surface of a stainless steel bar. The manufactured tool was applied for on-line selective solid phase microextraction (SPME) and determination of acesulfame (ACF) as an artificial sweetener with high performance liquid chromatography (HPLC). The selective ability of method for the extraction of ACF was investigated in the presence of some selected sweeteners such as saccharine (SCH), aspartame (ASP) and caffeine (CAF). Electrospinning of MIP sol-gel solution on the stainless steel bar provided an unbreakable sorbent with high thermal, mechanical, and chemical stability. Moreover, application of the MIP-SPME tool revealed a unique approach for the selective microextraction of the analyte in beverage samples. In this work, 3-(triethoxysilyl)-propylamine (TMSPA) was chosen as a precursor due to its ability to imprint the analyte by hydrogen bonding, Van der Walls, and dipole-dipole interactions. Nylon 6 was also added as a backbone and support for the precursor in which sol could greatly growth during the sol-gel process and makes the solution electrospinable. Various effective parameters in the extraction efficiency of the MIP-SPME tool such as loading time, flow rate, desorption time, selectivity, and the sample volume were evaluated. The linearity for the ACF in beverage sample was in the range of 0.78-100.5 ng mL(-1). Limit of detection (LOD) and quantification (LOQ) were 0.23 and 0.78 ng mL(-1) respectively. The RSD values (n=5) were all below 3.5%at the 20 ng mL(-1) level. PMID:25618677

  15. A reversed-phase high performance liquid chromatography coupled with resonance Rayleigh scattering detection for the determination of four tetracycline antibiotics

    Energy Technology Data Exchange (ETDEWEB)

    Wang Lifeng [School of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China); Peng Jingdong [School of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China)], E-mail: hxpengjd@swu.edu.cn; Liu Limin [School of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China)

    2008-12-07

    A new reversed-phase high performance liquid chromatography with resonance Rayleigh scattering detection (HPLC-RRS) was developed for simultaneous separation and determination of four tetracycline antibiotics (TCs). A good chromatographic separation among the compounds was achieved using a Synergi Fusion-RP column (150 mm x 4.6 mm; 4 {mu}m) and a mobile phase consisting of methanol-acetonitrile-oxalic acid (5 mM) at the flow rate of 0.8 mL min{sup -1}. Column temperature was 30 deg. C. The RRS signal was detected at {lambda}{sub ex} = {lambda}{sub em} = 370 nm. The recoveries of sample added standard ranged from 95.3% to 103.5%, and the relative standard deviation was below 2.79%. A detection limit of 2.12-5.12 {mu}g mL{sup -1} was reached and a linear range was found between peak height and concentration in the range of 10.36-518.0 {mu}g mL{sup -1} for oxytetracycline (OTC), 12.11-605.5 {mu}g mL{sup -1} for tetracycline (TC), 11.79-589.5 {mu}g mL{sup -1} for chlortetracycline (CTC) and 10.32-516.0 {mu}g mL{sup -1} for doxycycline (DC). The linear regression coefficients were all above 0.999. The method has been applied successfully to the determination of OTC, TC, CTC, DC in pharmaceutical formulations and in honey. The method was simple, rapid and showed a better linear relation and high repeatability.

  16. Possible interferences of mercury sulfur compounds with ethylated and methylated mercury species using HPLC-ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Wilken, R.D.; Nitschke, F.; Falter, R. [ESWE-Institute for Water Research Water Technology at Mainz University, Kurfuerstenstr. 6, 65203, Wiesbaden (Germany)

    2003-09-01

    The HPLC-ICP-MS coupling technique is able to separate and detect methyl, ethyl and inorganic mercury isotopes specifically. An identification of ethyl mercury(+) is not possible when the widely used sodium tetraethylborate derivatisation method in combination with GC-AFS/AAS or ICP-MS techniques is performed because it contains ethyl groups. An unidentified compound with the same retention time as ethyl mercury was found in the HPLC chromatograms of industrial sewage samples and humic-rich soils of microcosm experiments after applying water vapour distillation. We also observed such unidentified peaks in samples of heavily contaminated sites in Eastern Germany, separated by HPLC fractionation only. In the experiments described, different mercury sulfur adducts were synthesised and tested for their retention times in the HPLC-ICP-MS system. It was found that the compound CH{sub 3}-S-Hg{sup +} showed the same retention time as the ethyl mercury standard. It is therefore possible that ethyl mercury detected in chromatography by comparison of the retention time could also be due to an adduct of a sulfur compound and a mercury species. CH{sub 3}-S-Hg{sup +}should be tested in other chromatographic mercury speciation methods for this effect. This work can also be regarded as a contribution to the discussion of artificially occurring methyl mercury in sediments during sample preparation. (orig.)

  17. Possible interferences of mercury sulfur compounds with ethylated and methylated mercury species using HPLC-ICP-MS

    International Nuclear Information System (INIS)

    The HPLC-ICP-MS coupling technique is able to separate and detect methyl, ethyl and inorganic mercury isotopes specifically. An identification of ethyl mercury(+) is not possible when the widely used sodium tetraethylborate derivatisation method in combination with GC-AFS/AAS or ICP-MS techniques is performed because it contains ethyl groups. An unidentified compound with the same retention time as ethyl mercury was found in the HPLC chromatograms of industrial sewage samples and humic-rich soils of microcosm experiments after applying water vapour distillation. We also observed such unidentified peaks in samples of heavily contaminated sites in Eastern Germany, separated by HPLC fractionation only. In the experiments described, different mercury sulfur adducts were synthesised and tested for their retention times in the HPLC-ICP-MS system. It was found that the compound CH3-S-Hg+ showed the same retention time as the ethyl mercury standard. It is therefore possible that ethyl mercury detected in chromatography by comparison of the retention time could also be due to an adduct of a sulfur compound and a mercury species. CH3-S-Hg+should be tested in other chromatographic mercury speciation methods for this effect. This work can also be regarded as a contribution to the discussion of artificially occurring methyl mercury in sediments during sample preparation. (orig.)

  18. Chromatographic behavior of 12 polar pteridines in hydrophilic interaction chromatography using five different HILIC columns coupled with tandem mass spectrometry.

    Science.gov (United States)

    Xiong, Xin; Liu, Yanmeng

    2016-04-01

    Retention characteristic of 5 hydrophilic interaction chromatography (HILIC) columns, containing neutral and possibly negatively charged support (silica, diol and amide), cationic phase (triazole) and zwitterionic phase (sulfobetaine), that are commercially available were studied for the separation of a group of 12 polar pteridines. The main factors influencing the retention and selectivity of pteridines for these different HILIC systems have been studied in liquid chromatography-tandem mass spectrometry (LC-MS/MS) conditions: mobile phase composition, buffer type, pH and concentration and the separation mechanism was also investigated. Results of the effects of organic modifier, buffer pH and ion strength indicate that the retention mechanism is a mixed-mode of adsorption and ion exchange, and optimization of HILIC analyses depends on the ionization state of the analytes. For silica, diol, amide and sulfobetaine phases, hydrophilic partitioning mainly contributes to the retention, while electrostatic interactions and hydrogen-bonding should be considered to understand the elution orders for triazole phase. An zwitterionic phase (ZIC-HILIC) provided the stronger retention for all pteridines than other tested columns. PMID:26838435

  19. Simultaneous determination of herbicide residues in tobacco using ultraperformance convergence chromatography coupled with solid-phase extraction.

    Science.gov (United States)

    Guo, Weiyun; Bian, Zhaoyang; Zhang, Daohong; Tang, Gangling; Liu, Wei; Wang, Jianlong; Li, Zhonghao; Yang, Fei

    2015-03-01

    A time-saving and organic solvent efficient method to simultaneously determine six kinds of herbicide residues in tobacco using solid-phase extraction for sample clean-up and preconcentration and the highly sensitive ultraperformance convergence chromatography method was developed. Parameters for ultraperformance convergence chromatography, including the choice of stationary phase and modifiers, autobackpressure regulator pressure, column temperature, and the flow rate of mobile solvents, were optimized. The herbicide residues of napropamide, alachlor, quizalofop-ethyl, diphenamid, metolachlor, and clomazone in tobacco samples were successfully separated and detected at levels as low as 0.0043-0.0086 mg/kg within 5 min using a nonpolar high strength silica C18 selectivity for bases column and methanol as the cosolvent of the mobile phase of carbon dioxide (75-99.9%, v/v). Analysis of tobacco samples had recoveries of 69.8-95.0%, limit of quantitation of 0.0127-0.0245 mg/kg, limit of detection of 0.0043-0.0086 mg/kg, and correlation coefficient of >0.9990. Results support this method as an efficient alternative to current methodologies for the determination of herbicide residues in tobacco. PMID:25546570

  20. PEG precipitation coupled with chromatography is a new and sufficient method for the purification of botulinum neurotoxin type B [corrected].

    Directory of Open Access Journals (Sweden)

    Yao Zhao

    Full Text Available Clostridium botulinum neurotoxins are used to treat a variety of neuro-muscular disorders, as well as in cosmetology. The increased demand requires efficient methods for the production and purification of these toxins. In this study, a new purification process was developed for purifying type B neurotoxin. The kinetics of C.botulinum strain growth and neurotoxin production were determined for maximum yield of toxin. The neurotoxin was purified by polyethylene glycol (PEG precipitation and chromatography. Based on design of full factorial experiment, 20% (w/v PEG-6000, 4 °C, pH 5.0 and 0.3 M NaCl were optimal conditions to obtain a high recovery rate of 87% for the type B neurotoxin complex, as indicated by a purification factor of 61.5 fold. Furthermore, residual bacterial cells, impurity proteins and some nucleic acids were removed by PEG precipitation. The following purification of neurotoxin was accomplished by two chromatography techniques using Sephacryl™ S-100 and phenyl HP columns. The neurotoxin was recovered with an overall yield of 21.5% and the purification factor increased to 216.7 fold. In addition, a mouse bioassay determined the purified neurotoxin complex possessed a specific toxicity (LD(50 of 4.095 ng/kg.