Biomedical Chromatography : BMC
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Simultaneous RP-HPLC-DAD quantification of bromocriptine, haloperidol and its diazepane structural analog in rat plasma with droperidol as internal standard for application to drug-interaction pharmacokinetics.
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A simple and rapid RP-HPLC-DAD method was developed and validated for simultaneous determination of the dopamine antagonists haloperidol, its diazepane analog, and the dopamine agonist bromocriptine in rat plasma, to perform pharmacokinetic drug-interaction studies. Samples were prepared for analysis by acetonitrile (22.0 mug/mL) plasma protein precipitation with droperidol as an internal standard, followed by a double-step liquid-liquid extraction with hexane : chloroform (70:30) prior to C-18 separation. Isocratic elution was achieved using a 0.1% (v/v) trifluoroacetic acid in deionized water, methanol and acetonitri...
Source: Biomedical Chromatography : BMC - November 11, 2009 Category: Biomedical Science Authors: Billups J, Jones C, Jackson TL, Ablordeppey SY, Spencer SD Tags: Biomed Chromatogr Source Type: journals
A simple, selective and rapid validated method for estimation of anastrazole in human plasma by liquid chromatography-tandem mass spectrometry and its application to bioequivalence study.
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A rapid, simple and specific method for estimation of anastrazole in human plasma was validated using letrozole as internal standard. The analyte and internal standard were extracted from plasma using simple solid-phase extraction. The compound were separated on a reverse-phase column with an isocratic mobile phase consisting of 0.1% formic acid in water and acetonitrile (12 : 88, v/v) and detected by tandem mass spectrometry in positive ion mode. The ion transitions recorded in multiple reaction monitoring mode were m/z 294.1 --> 225.1 for anastrazole and m/z 286.1 --> 217.1 for internal standard. Linearity in p...
Source: Biomedical Chromatography : BMC - November 11, 2009 Category: Biomedical Science Authors: Jangid AG, Pudage AM, Joshi SS, Pabrekar PN, Tale RH, Vaidya VV Tags: Biomed Chromatogr Source Type: journals
Quantitative sphingosine measurement as a surrogate for total ceramide concentration-preclinical and potential translational applications.
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Biomarkers are an increasingly important constituent of the drug development process, offering the potential of increased efficiency through reduced compound attrition and earlier proof of mechanism and/or efficacy. Assays developed for compound screening that can be directly translated for clinical trials are especially valuable, but their successful adoption requires a careful balance between assay performance and implementation costs. One such 'fit-for-purpose' biomarker assay, the indirect measurement of pharmacological modulation of sphingolipid biosynthesis and disposition, is presented here. Among spingolipids, ...
Source: Biomedical Chromatography : BMC - November 11, 2009 Category: Biomedical Science Authors: Kindt E, Wetterau J, Mueller SB, Castle C, Boustany-Kari CM Tags: Biomed Chromatogr Source Type: journals
Liquid chromatography-mass spectrometry methods for urinary biomarker detection in metabonomic studies with application to nutritional studies.
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The effects of sample preparation and chromatographic method differences on the classification and recovery of metabolic biomarkers from UPLC-MS measurements on urine samples of humans exposed to different dietary interventions have been investigated. Eight volunteers consumed three high-fat meals (rich in saturated, monounsaturated and polyunsaturated fatty acids, respectively) in randomized order with a washout period in between. For each participant, urine samples were obtained prior to and at three timed intervals after each meal. Samples were processed either by dilution (1 : 4) or by liquid-liquid extraction and ...
Source: Biomedical Chromatography : BMC - November 11, 2009 Category: Biomedical Science Authors: Legido-Quigley C, Stella C, Perez-Jimenez F, Lopez-Miranda J, Ordovas J, Powell J, van-der-Ouderaa F, Ware L, Lindon JC, Nicholson JK, Holmes E Tags: Biomed Chromatogr Source Type: journals
Development of a method to measure methadone enantiomers and its metabolites without enantiomer standard compounds for the plasma of methadone maintenance patients.
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A liquid chromatography-photodiode array (LC-PDA) method using a chiral analytical column was developed to determine the plasma levels of enantiomers of methadone and its chiral metabolite, 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine (EDDP), without the standard compounds of R-form or S-form enantiomers. This method was established by the characteristics of recombinant cytochrome P-450 (CYP) isozymes, where CYP2C19 prefers to metabolize R-methadone and CYP2B6 prefers to metabolize S-methadone. We incubated the racemic methadone standard with either enzyme for 24 h. We identified the retention times of R- and S-me...
Source: Biomedical Chromatography : BMC - November 10, 2009 Category: Biomedical Science Authors: Wang SC, Ho IK, Wu SL, Liu SC, Kuo HW, Lin KM, Liu YL Tags: Biomed Chromatogr Source Type: journals
High-performance liquid chromatography with solid-phase extraction for the quantitative determination of nilotinib in human plasma.
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A simple, rapid and sensitive high-performance liquid chromatography (HPLC)-based method with ultraviolet detection was developed for the quantitation of nilotinib, a tyrosine kinase inhibitor, in human plasma. Nilotinib and the internal standard dasatinib were separated using a mobile phase of 0.5% KH(2)PO(4) (pH2.5)-acetonitrile-methanol (55:25:20, v/v/v) on a Capcell Pak MG II column (250 x 4.6 mm) at a flow rate of 0.5 mL/min and optical measurement at 250 nm. Analysis required only 100 muL of plasma and involved a rapid and simple solid-phase extraction with an Oasis HLB cartridge, which gave recoveries from 72 to...
Source: Biomedical Chromatography : BMC - November 10, 2009 Category: Biomedical Science Authors: Miura M, Takahashi N, Sawada KI Tags: Biomed Chromatogr Source Type: journals
Enantioresolution of DL-penicillamine.
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Penicillamine (PenA) is a nonproteinogenic amino acid containing a thiol group. The three functional groups in penicillamine undergo characteristic chemical reactions and differ in their ability to participate in various chemical and biochemical reactions. d-penicillamine is more active pharmacologically, while the l-isomer occurs 'naturally'. This review deals with the enantioresolution of PenA both by direct and indirect methods using liquid chromatography. HPLC separation of its diastereomers prepared with different chiral derivatizing reagents (on reversed-phase columns) and separation of the derivatives prepared w...
Source: Biomedical Chromatography : BMC - November 10, 2009 Category: Biomedical Science Authors: Bhushan R, Kumar R Tags: Biomed Chromatogr Source Type: journals
Development of a liquid chromatography-isotope dilution mass spectrometry method for quantification of fentanyl in human plasma.
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In this report, we present a simple, reliable and sensitive LC-ID/MS method for the quantification of fentanyl in human plasma. LC-ID/MS analysis was carried out on a triple quadrupole mass spectrometer operated in positive electrospray ionization multiple-reaction-monitoring using the transitions m/z 337.6 --> 187.9 for fentanyl and m/z 342.6 --> 187.9 for the internal standard (D5-fentanyl). The calibration curve covered the range 0.02-10 ng/mL. The intra- and inter-batch precision were less than 6.739 and 3.126% for fentanyl and IS, with accuracy from 94.16 to 102.0%. The lower limit of quantification was identifi...
Source: Biomedical Chromatography : BMC - November 2, 2009 Category: Biomedical Science Authors: Lu C, Jia JY, Gui YZ, Liu GY, Shi XJ, Li SJ, Yu C Tags: Biomed Chromatogr Source Type: journals
Development and validation of a HPLC method for determination of levonorgestrel and quinestrol in rat plasma.
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Levonorgestrel and quinestrol, commonly known as EP-1, has long been used in the control of wild rodents. Up to the present time, however, no method for simultaneous quantification of levonorgestrel and quinestrol in rat plasma has been reported. In the present study, a sensitive reverse-phase high-performance liquid chromatography with ultraviolet detection (RP-HPLC-UV) method for quantification of levonorgestrel and quinestrol in rat plasma has been developed. It uses a Kromasil ODS C(18) column and acetonitrile-0.1% formic acid (85 : 15, v/v) mobile phase at ambient temperature. The plasma sample was prepared by hex...
Source: Biomedical Chromatography : BMC - November 2, 2009 Category: Biomedical Science Authors: Tang T, Li P, Luo L, Shi D, Li J, Cao Y Tags: Biomed Chromatogr Source Type: journals
In vitro and in vivo studies of androst-4-ene-3,6,17-trione in horses by gas chromatography-mass spectrometry.
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This paper describes the application of gas chromatography-mass spectrometry (GC-MS) for in vitro and in vivo studies of 6-OXO in horses, with a special aim to identify the most appropriate target metabolite to be monitored for controlling the administration of 6-OXO in racehorses. In vitro studies of 6-OXO were performed using horse liver microsomes. The major biotransformation observed was reduction of one keto group at the C3 or C6 positions. Three in vitro metabolites, namely 6alpha-hydroxyandrost-4-ene-3,17-dione (M1), 3alpha-hydroxyandrost-4-ene-6,17-dione (M2a) and 3beta-hydroxyandrost-4-ene-6,17-dione (M2b) wer...
Source: Biomedical Chromatography : BMC - November 2, 2009 Category: Biomedical Science Authors: Leung GN, Tang FP, Wan TS, Wong CH, Lam KK, Stewart BD Tags: Biomed Chromatogr Source Type: journals
Isothiocyanates as derivatization reagents for amines in liquid chromatography/electrospray ionization-tandem mass spectrometry.
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The applicability of 3-pyridyl isothiocyanate, p-(dimethylamino)phenyl isothiocyanate and m-nitrophenyl isothiocyanate as the derivatization reagents for amines in high-performance liquid chromatography/electrospray ionization-tandem mass spectrometry (LC/ESI-MS/MS) was examined. The generated derivatives of amines with these reagents were favorably separated on the reversed-phase column and detected by ESI-MS/MS. The C-N bond of the generated thiourea structure was efficiently cleaved by collision-induced dissociation and gave the single and intense product ion. Among the three reagents, 3-pyridyl isothiocyanate was t...
Source: Biomedical Chromatography : BMC - November 2, 2009 Category: Biomedical Science Authors: Santa T Tags: Biomed Chromatogr Source Type: journals
Development and validation of an analytical method for the quantification of cytochrome c in skin transport studies.
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In conclusion, the HPLC method provided a fast, efficient means to quantify Cytochrome c in samples from skin transport studies. Copyright (c) 2009 John Wiley & Sons, Ltd.
PMID: 19882748 [PubMed - as supplied by publisher] (Source: Biomedical Chromatography : BMC)
Source: Biomedical Chromatography : BMC - November 2, 2009 Category: Biomedical Science Authors: Bachhav YG, Kalia YN Tags: Biomed Chromatogr Source Type: journals
A sensitive and specific liquid chromatography/tandem mass spectrometry method for quantification of nevirapine and its five metabolites and their pharmacokinetics in baboons.
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A highly sensitive and specific LC-MS/MS assay was developed and validated to quantify nevirapine (NVP) and its five metabolites [2-, 3-, 8-, 12-hydroxyl NVP (OHNVP) and 4-carboxyl NVP (CANVP)] simultaneously in baboon serum and the assay was used to characterize their pharmacokinetic studies of an oral-dose escalation study in baboon. The lower limit of quantification (LLOQ) for NVP and its four hydroxyl nevirapine metabolites was 1.0 ng/mL and for 4-CANVP was 5.0 ng/mL. The between-run and within-run precisions and accuracies at four quality control concentrations (1, 5, 50 and 500 ng/mL) were evaluated in baboon ser...
Source: Biomedical Chromatography : BMC - November 2, 2009 Category: Biomedical Science Authors: Ren C, Fan-Havard P, Schlabritz-Loutsevitch N, Ling Y, Chan KK, Liu Z Tags: Biomed Chromatogr Source Type: journals
Liquid chromatographic-tandem mass spectrometry assay for quantitation of a novel antidiabetic S002-853 in rat plasma and its application to pharmacokinetic study.
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A sensitive and selective LC-MS/MS method has been developed and validated for the estimation of novel antidiabetic synthetic flavonoid S002-853 in rat plasma using centchroman as an internal standard. The method involves a simple two-step liquid-liquid extraction with diethyl ether. The analyte was chromatographed on a Pierce Spheri-5, guard cyano column (30 x 4.6 mm i.d., 5 microm) with isocratic mobile phase consisting of methanol-ammonium acetate buffer (pH 4.6, 10 mm; 90 : 10, v/v) at a flow rate of 0.75 mL/min. The API 4000 triple-quadrupole LC-MS/MS system was operated under multiple reaction-monitoring mode. Th...
Source: Biomedical Chromatography : BMC - October 29, 2009 Category: Biomedical Science Authors: Gautam N, Singh RP, Pratap R, Singh SK Tags: Biomed Chromatogr Source Type: journals
Quantification of acetylcholine, an essential neurotransmitter, in brain microdialysis samples by liquid chromatography mass spectrometry.
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Chemical neurotransmission has been the subject of intensive investigations in recent years. Acetylcholine is an essential neurotransmitter in the central nervous system as it has an effect on alertness, memory and learning. Enzymatic hydrolysis of acetylcholine in the synaptic cleft is fast and quickly metabolizes to choline and acetate by acetylcholinesterase. Hence the concentration in the extracellular fluid of the brain is low (0.1-6 nm). Techniques such as microdialysis are routinely employed to measure acetylcholine levels in living brain systems and the microdialysis sample volumes are usually less than 50 micr...
Source: Biomedical Chromatography : BMC - October 29, 2009 Category: Biomedical Science Authors: Nirogi R, Mudigonda K, Kandikere V, Ponnamaneni R Tags: Biomed Chromatogr Source Type: journals
Irinotecan and its active metabolite, SN-38: review of bioanalytical methods and recent update from clinical pharmacology perspectives.
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The introduction of irinotecan has revolutionized the applicability of camptothecins as predominant topoisomerase I inhibitor for anti-cancer therapy. The potent anti-tumor activity of irinotecan is due to rapid formation of an in vivo active metabolite, SN-38. Therefore, irinotecan is considered as a pro-drug to generate SN-38. Over the past decade, side-by-side with the clinical advancement of the use of irinotecan in the oncology field, a plethora of bioanalytical methods have been published to quantify irinotecan, SN-38 and other metabolites. Because of the availability of HPLC, LC-MS and LC-MS/MS methods, the phar...
Source: Biomedical Chromatography : BMC - October 23, 2009 Category: Biomedical Science Authors: Ramesh M, Ahlawat P, Srinivas NR Tags: Biomed Chromatogr Source Type: journals
Supported liquid extraction in combination with LC-MS/MS for high-throughput quantitative analysis of hydrocortisone in mouse serum.
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A high-throughput LC-MS/MS bioanalytical method was developed and validated for the determination of hydrocortisone in mouse serum via supported liquid extraction (SLE) in a 96-well plate format. Although sample extracts from SLE result in similar matrix effects compared with conventional liquid-liquid extraction (LLE), greater analyte extraction recovery and much higher analysis throughput for the quantitative analysis of hydrocortisone in mouse serum were obtained. The current LC-MS/MS method was validated for a concentration range of 2.00-2000 ng/mL for hydrocortisone using a 0.100 mL volume of mouse serum. The intr...
Source: Biomedical Chromatography : BMC - October 21, 2009 Category: Biomedical Science Authors: Wu S, Li W, Mujamdar T, Smith T, Bryant M, Tse FL Tags: Biomed Chromatogr Source Type: journals
Automated precolumn derivatization system for analyzing physiological amino acids by liquid chromatography/mass spectrometry.
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An automated method for high-throughput amino acid analysis, using precolumn derivatization high-performance liquid chromatography/electrospray mass spectrometry (HPLC/ESI-MS), was developed and evaluated. The precolumn derivatization step was performed in the reaction port of a home-built auto-sampler system. Amino acids were derivatized with 3-aminopyridyl-N-hydroxysuccinimidyl carbamate, and a 3 mum Wakosil-II 3C8-100HG column (100 x 2.1 mm i.d.) was used for separation. To achieve a 13 min cycle for each sample, the derivatization and separation steps were performed in parallel. The results of the method evaluation...
Source: Biomedical Chromatography : BMC - October 12, 2009 Category: Biomedical Science Authors: Shimbo K, Kubo S, Harada Y, Oonuki T, Yokokura T, Yoshida H, Amao M, Nakamura M, Kageyama N, Yamazaki J, Ozawa SI, Hirayama K, Ando T, Miura J, Miyano H Tags: Biomed Chromatogr Source Type: journals
Micro determination of cortisol and cortisone in umbilical cord blood by chemiluminescent high-performance liquid chromatography.
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A simple, sensitive and specific chemiluminescent high-performance liquid chromatography method, based on the luminol reaction, for determination of serum cortisol and cortisone, was established. In infants, placental 11beta-hydroxysteroid dehydrogenase type 2 enzyme (11beta-HSD2) activity may affect adrenal function early after birth. The cortisol-cortisone ratio of serum concentrations in umbilical cord blood is an indicator of placental 11beta-HSD2 activity. The optimum conditions for the luminol reaction were determined to be 1.5 mM luminol, 0.6 M sodium hydroxide, 0.15 mm potassium hexacyanoferrate(III) and 200 mM...
Source: Biomedical Chromatography : BMC - October 6, 2009 Category: Biomedical Science Authors: Hasegawa T, Kubo H, Shinozaki K, Nowatari M, Ishii M Tags: Biomed Chromatogr Source Type: journals
Development and validation of RP-HPLC-fluorescence method for quantitative determination of quinidine, a probe substrate for P-glycoprotein inhibition assay using Caco-2 cell monolayer.
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A simple, sensitive and specific reverse-phase high-performance liquid chromatographic (RP-HPLC) method with fluorescence detection was developed for quantitation of quinidine from HBSS buffer. The method was applicable in the bi-directional transport assay for evaluation of the inhibitory effect of test compounds on P-glycoprotein-mediated quinidine transport; quinidine was used as a probe P-glycoprotein substrate. The calibration curve was linear (correlation coefficient >/=99) in the range 0.30-100.00 nm. The method was validated and is specific and sensitive with limit of quantitation of 300 pm for quinidine. Th...
Source: Biomedical Chromatography : BMC - October 6, 2009 Category: Biomedical Science Authors: Patil AG, Reddy D, D'Souza R, Damre A Tags: Biomed Chromatogr Source Type: journals
Determination of kynurenic acid levels in rat brain microdialysis samples and changes in kynurenic acid levels induced by N-acetylaspartic acid.
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The levels of kynurenic acid, an endogenous antagonist of alpha(7) nicotinic acetylcholine and N-methyl-D-aspartate receptors, were measured in microdialysis samples obtained from the prefrontal cortices of rats using column-switching high-performance liquid chromatography with fluorescence detection. When the perfusate was constantly infused at a rate of 1.0 mu/min, the in vitro recovery of kynurenic acid through the dialysis membrane was approximately 20.4%, and the precision was within 1.31%. Endogenous kynurenic acid in the microdialysis sample was clearly detected using column-switching high-performance liquid chr...
Source: Biomedical Chromatography : BMC - October 6, 2009 Category: Biomedical Science Authors: Tomiya M, Fukushima T, Ogaya T, Sone Y, Mitsuhashi S, Toyo'oka T Tags: Biomed Chromatogr Source Type: journals
Stability-indicating HPTLC method for quantitative estimation of silybin in bulk drug and pharmaceutical dosage form.
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In the present study a novel stability-indicating high-performance thin-layer chromatography (HPTLC) method for quantitative determination of silybin in bulk drug and nanoemulsion formulation has been developed and validated on silica using solvent chloroform-acetone-formic acid (9 : 2 : 1 v/v/v) (R(f )of silybin 0.46 +/- 0.05) in the absorbance mode at 296 nm. The method showed a good linear relationship (r(2) +/- 0.999) in the concentration range 25-1500 ng per spot. It was found to be linear, accurate, precise, specific, robust and stability-indicating and can be applied for quality control and standardization of se...
Source: Biomedical Chromatography : BMC - October 6, 2009 Category: Biomedical Science Authors: Parveen R, Ahmad S, Baboota S, Ali J, Alka A Tags: Biomed Chromatogr Source Type: journals
Sensitive LC-MS-MS method for the determination of tiopronin in human plasma.
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A highly selective and sensitive LC-MS-MS method was developed and validated to quantify tiopronin in human plasma, using fudosteine as the internal standard (IS). L-Cysteine and 1,4-dithiothreitol (DTT) were used as the reducer and the stabilizer to release and stabilify tiopronin from a dimmer and mix forms with endogenous thiols in the treatment of plasma samples. After a simple liquid-liquid extraction with ethyl acetate in acidic condition, the post-treatment samples were analyzed on a C(18) column interfaced with a triple-quadruple tandem mass spectrometer using negative electrospray ionization. Methanol and wate...
Source: Biomedical Chromatography : BMC - October 6, 2009 Category: Biomedical Science Authors: Jiang B, Xu Y, Xu F, Sun J, Li N, Luo Y, Guo Q Tags: Biomed Chromatogr Source Type: journals
Simultaneous determination of itraconazole and hydroxyitraconazole in human plasma by liquid chromatography-isotope dilution tandem mass spectrometry method.
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A rapid and sensitive liquid chromatography-isotope dilution tandem mass spectrometry method was developed and validated for quantification of itraconazole (ITZ) and its active metabolite hydroxyitraconazole (OH-ITZ ) in human plasma. The plasma samples were extracted with tert-butyl methyl ether and two isotope-labeled internal standards (D5-itraconazole and D5-hydroxyitraconazole) were used. The chromatographic separation was performed on a Capcell Pak C(18) MG III (100 x 2 mm, 5 microm, Shiseido). The protonated ions of analytes were detected in positive ionization in multiple reaction monitoring mode. The plasma me...
Source: Biomedical Chromatography : BMC - October 5, 2009 Category: Biomedical Science Authors: Jia JY, Lu C, Liu GY, Zhang MQ, Liu YM, Wang W, Weng LP, Li SJ, Yu C Tags: Biomed Chromatogr Source Type: journals
High-performance affinity chromatography method for identification of l-arginine interacting factors using magnetic nanobeads.
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In this study, we have newly developed L-arginine methyl ester (L-AME)-immobilized beads by conjugating L-AME to the surface of these nanobeads. Firstly, we showed that inducible nitric oxide synthase, which binds and uses L-arginine as a substrate, specifically bound to L-AME-immobilized beads. Secondly, we newly identified phosphofructokinase, RuvB-like 1 and RuvB-like 2 as AIFs from crude extracts of HeLa cells using this affinity chromatographic system. The data presented here demonstrate that L-AME-immobilized beads are effective tool for purification of AIFs directly from crude cell extracts. We expect that the prese...
Source: Biomedical Chromatography : BMC - October 4, 2009 Category: Biomedical Science Authors: Hiramoto M, Maekawa N, Kuge T, Ayabe F, Watanabe A, Masaike Y, Hatakeyama M, Handa H, Imai T Tags: Biomed Chromatogr Source Type: journals
A sensitive non-aqueous capillary electrophoresis-mass spectrometric method for multiresidue analyses of beta-agonists in pork.
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Non-aqueous capillary electrophoresis-mass spectrometry (NACE-MS) was developed for trace analyses of beta-agonists (i.e. clenbuterol, salbutamol and terbutaline) in pork. The NACE was in 18 mM ammonium acetate in methanol-acetonitrile-glacial acetic acid (66 : 33 : 1, v/v/v) using a voltage of 28 kV. The hyphenation of CE with a time-of-flight MS was performed by electrospray ionization interface employing 5 mM ammonium acetate in methanol-water (80 : 20, v/v) as the sheath liquid at a flow rate of 2 muL/min. Method sensitivity was enhanced by a co-injection technique (combination of hydrodynamic and electrokinetic in...
Source: Biomedical Chromatography : BMC - October 4, 2009 Category: Biomedical Science Authors: Anurukvorakun O, Buchberger W, Himmelsbach M, Klampel CW, Suntornsuk L Tags: Biomed Chromatogr Source Type: journals
Determination of dopamine, serotonin, and their metabolites in pediatric cerebrospinal fluid by isocratic high performance liquid chromatography coupled with electrochemical detection.
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A method to rapidly measure dopamine (DA), dihydroxyindolphenylacetic acid, homovanillic acid, serotonin (5-HT) and 5-hydroxyindoleacetic acid concentrations in cerebrospinal fluid (CSF) has not yet been reported. A rapid, sensitive, and specific HPLC method was therefore developed using electrochemical detection. CSF was mixed with an antioxidant solution prior to freezing to prevent neurotransmitter degradation. Separation of the five analytes was obtained on an ESA MD-150 x 3.2 mm column with a flow rate of 0.37 mL/min and an acetonitrile-aqueous (5 : 95, v/v) mobile phase with 75 mM monobasic sodium phosphate buffe...
Source: Biomedical Chromatography : BMC - October 4, 2009 Category: Biomedical Science Authors: Hubbard KE, Wells A, Owens TS, Tagen M, Fraga CH, Stewart CF Tags: Biomed Chromatogr Source Type: journals
Bioanalysis of pentoxifylline and related metabolites in plasma samples through LC-MS/MS.
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Analytical aspects related to the assay of pentoxifylline (PTX), lisofylline (M1) and carboxypropyl dimethylxanthine (M5) metabolites are discussed through comparison of two alternative analytical methods based on liquid chromatography separation and atmospheric pressure electrospray ionization tandem mass spectrometry detection. One method is based on a 'pure' reversed-phase liquid chromatography mechanism, while the second one uses the additional polar interactions with embedded amide spacers linking octadecyl moieties to the silicagel surface (C-18 Aqua stationary phase). In both cases, elution is isocratic. Both me...
Source: Biomedical Chromatography : BMC - October 4, 2009 Category: Biomedical Science Authors: Sora DI, Cristea E, Albu F, David V, Medvedovici A Tags: Biomed Chromatogr Source Type: journals
Highly sensitive determination of Schisandrin and Schisandrin B in plasma of rats after administration of Wurenchun (Fructus Schisandrae Chinensis Extracts) preparations by LC-ESI-MS/MS.
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A sensitive and specific method based on liquid chromatography-tandem mass spectrometry using electrospray ionization (LC-ESI-MS/MS) has been developed for the determination of Schisandrin and Schisandrin B in rat plasma. A 100 muL plasma sample was extracted by methyl tert-butyl ether after spiking the samples with nimodipine (internal standard) and performed on an XTerra(R)MS-C(18) column (150 mm x 2.1 mm, 3.5 mum) with the mobile phase of acetonitrile-water-formic acid (80:20:0.2, v/v) at a flow rate of 0.2 mL/min in a run time of 8.5 min. The lower limit of quantification of the method was 40 ng/mL for Schisandrin ...
Source: Biomedical Chromatography : BMC - October 4, 2009 Category: Biomedical Science Authors: Tang J, Shao B, Liu Y, Liu H, Ji H, Zhu D, Wu L Tags: Biomed Chromatogr Source Type: journals
Liquid chromatography tandem mass spectrometry method for determination of bisoprolol in human plasma using d5-bisoprolol as the internal standard.
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A simple, reliable and sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) protocol was developed and validated for quantification of bisoprolol in human plasma. The sample was pretreated with a simple procedure of protein precipitation and an isotope-labeled d5-bisoprolol was used as internal standard. The chromatographic separation was performed on a Capcell Pak C(18) MG III column (100 mm x 2.0 mm, 5 microm). The protonated ion of the analyte was detected in positive ionization by multiple reaction monitoring mode. The mass transition pairs of m/z 326.3 --> 116.3 and m/z 331.3 --> 121.3 were us...
Source: Biomedical Chromatography : BMC - October 4, 2009 Category: Biomedical Science Authors: Liu GY, Wang W, Jia JY, Lu C, Liu YM, Zhang MQ, Liu Y, Li SJ, Yu C Tags: Biomed Chromatogr Source Type: journals
Sensitivity enhancement and matrix effect evaluation during summation of multiple transition pairs-case studies of clopidogrel and ramiprilat.
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Sensitivity enhancement via summation of multiple MRM transition pairs is gaining popularity in tandem mass spectrometric assays. Numerous validation experiments describing the assays for two model substrates, clopidogrel and ramiprilat, were performed. The quantitation of clopidogrel was achieved by the summation of transition pairs m/z 322.2 to m/z 212.0 and m/z 322.2 to m/z 184.0, while that of ramiprilat was achieved by the summation of transition pairs m/z 389.2 to m/z 206.1 and m/z 389.2 to m/z156.1. The use of summation approach achieved sensitivities of >2 fold for both compounds as compared with the reporte...
Source: Biomedical Chromatography : BMC - September 29, 2009 Category: Biomedical Science Authors: Manjunath Swamy J, Kamath N, Radha Shekar AK, Srinivas NR, Kristjansson F Tags: Biomed Chromatogr Source Type: journals
On-line concentration by field-enhanced sample injection with reverse migrating micelles in micellar electrokinetic capillary chromatography for the analysis of coumarins from traditional Chinese medicine and human serum.
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In this work, a simple, reproducible and sensitive micellar electrokinetic chromatography method was developed for the separation and determination of three coumarins, imperatorin (IM), isoimperatorin (IO) and osthole (OS) from traditional Chinese medicine and human serum. Field-enhanced sample injection with reverse migrating micelles was used for on-line concentration of the coumarins. The optimum buffer contained 50 mM H(3)PO(4), 160 mM sodium dodecyl sulfate, 20% acetonitrile and 15% 2-propanol, and the pH of buffer was 2.0. The sample solution was diluted with water containing 5 mM sodium dodecyl sulfate and injec...
Source: Biomedical Chromatography : BMC - September 29, 2009 Category: Biomedical Science Authors: Jiang TF, Lv ZH, Wang YH, Yue ME Tags: Biomed Chromatogr Source Type: journals
Urinary metabolic profiling of volatile organic compounds in acute exposed volunteers after an oil spill in Republic of Korea.
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The Herbei Spirit oil spill occurred in western Korea. A large number of people who participated in the cleanup tasks of the contaminated area were exposed to crude oil component. We developed a method to monitor volatile organic compound (VOC) metabolites in urine, and evaluate the acute exposure caused by the oil spill in exposed volunteer workers (n = 100, 20.7 +/- 2.1 years, mean +/- SD). Acidified urine samples were extracted by SPE, derivatized with trimethylsilyl, and analyzed using gas chromatography-mass spectrometry. Calibration curves were found to be linear from 3 to 1000 ng/mL (r(2) > 0.993). Accuracy w...
Source: Biomedical Chromatography : BMC - September 29, 2009 Category: Biomedical Science Authors: Lee J, Kim MH, Ha M, Chung BC Tags: Biomed Chromatogr Source Type: journals
Determination of serum cholestanol by semi-micro high-performance liquid chromatography with electrochemical detection.
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In conclusion, we found this method to be both simple and useful for the determination of cholestanol in serum, helping in the diagnosis of CTX. Copyright (c) 2009 John Wiley & Sons, Ltd.
PMID: 19795364 [PubMed - as supplied by publisher] (Source: Biomedical Chromatography : BMC)
Source: Biomedical Chromatography : BMC - September 29, 2009 Category: Biomedical Science Authors: Hojo K, Hakamata H, Takahashi A, Hosokawa YY, Kusu F Tags: Biomed Chromatogr Source Type: journals
Simultaneous quantification of oleuropein and its metabolites in rat plasma by liquid chromatography electrospray ionization tandem mass spectrometry.
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In this study, a liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI MS/MS) method has been developed and validated for the quantification of OE, simultaneously with its main metabolites hydroxytyrosol, 2-(3,4-dihydroxyphenyl)acetic acid, 4-(2-hydroxyethyl)-2-methoxy-phenol or homovanillyl alcohol, 2-(4-hydroxy-3-methoxyphenyl)acetic acid or homovanillic acid, and elenolic acid in rat plasma matrix. Samples were analyzed by LC-ESI MS/MS prior to and after enzymatic treatment. A solid-phase extraction step with high mean recovery for all compounds was performed as sample pretreatment. Calibration ...
Source: Biomedical Chromatography : BMC - September 29, 2009 Category: Biomedical Science Authors: Bazoti FN, Gikas E, Tsarbopoulos A Tags: Biomed Chromatogr Source Type: journals
Determination of asperosaponin VI in rat plasma by HPLC-ESI-MS and its application to preliminary pharmacokinetic studies.
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Asperosaponin VI (also named akebia saponin D) is a typical bioactive triterpenoid saponin isolated from the rhizome of Dipsacus asper Wall (Dipsacaceae). In this work, a sensitive high-performance liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS) assay has been established for determination of asperosaponin VI in rat plasma. With losartan as the internal standard (IS), plasma samples were prepared by protein precipitation with methanol. Chromatographic separation was performed on a C(18) column with a mobile phase of 10 mm ammonium acetate buffer containing 0.05% formic acid-methanol (32 : ...
Source: Biomedical Chromatography : BMC - September 29, 2009 Category: Biomedical Science Authors: Li K, Ding L, Yang ZL, Liu EH, Qi LW, Li P, Hu YZ Tags: Biomed Chromatogr Source Type: journals
Development and validation of a rapid and sensitive HPLC method for the quantification of 5-fluorocytosine and its metabolites.
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To study the intracellular metabolism of the prodrug 5-fluorocytosine (5FC), we developed a novel reverse-phase high-performance liquid chromatography method to simultaneously detect 5FC and its four major anabolic metabolites: 5-fluorouracil, 5-fluorouridine, 5-fluorouridine-monophosphate and 5-fluoro-2'deoxyuridine-5'-monophosphate. Separation of each compound was accomplished under isocratic conditions using a C(18) column and mobile phase of formic acid-water (1 : 99 v/v). The method was validated for both accuracy and reproducibility in cell culture media. Additionally, metabolites were assessed for stability at a...
Source: Biomedical Chromatography : BMC - September 29, 2009 Category: Biomedical Science Authors: Serve KM, Yáñez JA, Remsberg CM, Davies NM, Black ME Tags: Biomed Chromatogr Source Type: journals
Development and validation of a UPLC-UV method for the determination of daptomycin in rabbit plasma.
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Daptomycin (DPT) is a lipopeptide antibiotic with potent bactericidal activity in vitro against Gram-positive bacteria, which has attracted the attention of the scientific community due to its unique mechanism of action and due to the immediate need for new antibiotics in the era of multidrug resistance. In order to assess its pharmacokinetics in rabbits a new analytical method has been developed and validated using ultra performance liquid chromatography in conjugation with ultraviolet detection for the quantitation of the antibiotic in rabbit plasma, using the internal standard methodology. The separation was achieve...
Source: Biomedical Chromatography : BMC - September 29, 2009 Category: Biomedical Science Authors: Gikas E, Bazoti FN, Fanourgiakis P, Perivolioti E, Roussidis A, Skoutelis A, Tsarbopoulos A Tags: Biomed Chromatogr Source Type: journals
Determination of intracellular glutathione and cysteine using HPLC with a monolithic column after derivatization with monobromobimane.
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An optimized high-performance liquid chromatography (HPLC) method is used to show that, as myoblasts differentiate into multinucleated muscle fibers, there is a shift to a more oxidized cell redox state. The HPLC method incorporated derivatization with monobromobimane for the determination of the reduced (GSH) and oxidized (GSSG) forms of glutathione and the reduced (Cys) and oxidized (CysSS) forms of cysteine. The derivatization was optimized to improve the sensitivity of the approach; the limits of detection for glutathione and cysteine were 3 x 10(-8) and 5 x 10(-8) M, respectively. Copyright (c) 2009 John Wiley &am...
Source: Biomedical Chromatography : BMC - September 8, 2009 Category: Biomedical Science Authors: Conlan XA, Stupka N, McDermott GP, Francis PS, Barnett NW Tags: Biomed Chromatogr Source Type: journals
Assay and stability-indicating micellar electrokinetic chromatography method for the simultaneous determination of valacyclovir, acyclovir and their major impurity guanine in pharmaceutical formulations.
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A micellar electrokinetic chromatography (MEKC) method for the simultaneous determination of the antiviral drugs acyclovir and valacyclovir and their major impurity, guanine, was developed. The influences of several factors (surfactant and buffer concentration, pH, applied voltage, capillary temperature and injection time) were studied. Using tyramine hydrochloride as internal standard, the analytes were all separated in about 4 min. The separation was carried out in reversed polarity mode at 28 degrees C, 25 kV and using hydrodynamic injection (15 s). The separation was effected in a fused-silica capillary 100 mum x 5...
Source: Biomedical Chromatography : BMC - September 7, 2009 Category: Biomedical Science Authors: Al Azzam KM, Saad B, Makahleah A, Aboul-Enein HY, Elbashir AA Tags: Biomed Chromatogr Source Type: journals
Influence of number of calibration standards within a defined range on pharmacokinetic disposition-case studies with omeprazole and clopidogrel carboxylic acid.
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While the practice of using a smaller number of non-zero standards (typically seven to eight) has not been entertained in routine bioanalytical work, it is important to innovate and be pragmatic about minimizing the number of calibration standards to promote cost-effective and speedy assessment. In this exercise, two important compounds, omeprazole and clopidogrel carboxylic acid, were considered. Additionally, both analytes offered a 1000-fold calibration curve range with eight non-zero standards to permit a systematic evaluation. Accordingly various scenarios of post-hoc analysis of the calibration data were formulat...
Source: Biomedical Chromatography : BMC - September 7, 2009 Category: Biomedical Science Authors: D'Souza HJ, Pai B, Kumar A, Shekar R, Srinivas NR, Kristjansson F Tags: Biomed Chromatogr Source Type: journals
High-performance liquid chromatographic analysis: applications to nutraceutical content and urinary disposition of oxyresveratrol in rats.
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A high-performance liquid chromatographic (HPLC) method was developed for the analysis of the stilbene, oxyresveratrol. This method involves the use of a Luna(R) C(18) column with ultraviolet detection at 320 nm. The mobile phase consisted of acetonitrile, water and formic acid (30 : 70 : 0.04 v/v) with a flow rate of 0.6 mL/min. The calibration curves were linear over the range of 0.5-100.0 mug/mL. The mean extraction efficiency was between 98.9 and 109%. The precision of the assay was 0.069-18.4% (RSD%), and within 20% at the limit of quantitation (0.5 mug/mL). The bias of the assay was <15% and within 15% at the ...
Source: Biomedical Chromatography : BMC - September 7, 2009 Category: Biomedical Science Authors: Bertram RM, Takemoto JK, Remsberg CM, Vega-Villa KR, Sablani S, Davies NM Tags: Biomed Chromatogr Source Type: journals
LC-APCI mass spectrometric method development and validation for the determination of atovaquone in human plasma.
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A newly developed LC-APCI mass spectrometric method is described for human plasma determination of atovaquone using lapachol internal standard. A single-step protein precipitation technique for plasma extraction of atovaquone achieving mean recovery of 94.17% (CV 8%) without compromising sensitivity (limit of quantitation 50.3 ng/mL) or linearity (50.3 ng/mL-23924.6 ng/mL) is delineated in this paper. Heated nebulizer in negative multiple reaction monitoring mode was employed with transitions m/z 365.2 --> m/z 337.1 and m/z 240.9 --> m/z 185.7 for atovaquone and lapachol respectively in this liquid chromatographi...
Source: Biomedical Chromatography : BMC - August 24, 2009 Category: Biomedical Science Authors: Gurule S, Goswami D, Khuroo AH, Monif T Tags: Biomed Chromatogr Source Type: journals
Quality assessment of Cortex Phellodendri by high-performance liquid chromatography coupled with electrospray ionization mass spectrometry.
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A simple method based on liquid chromatography coupled with diode array detection and electrospray ionization mass spectrometry (LC-DAD-ESI-MS) was developed for the quality assessment of Cortex Phellodendri (CP), which was mainly derived from two species of Phellodendron chinense Schneid and Phellodendron amurense Rupr. Total 41 compounds, including 14 phenols, 24 alkaloids and three liminoidal triterpenes were identified or tentatively characterized from the 75% methanol extract of CP samples by online ESI-MS(n) fragmentation and UV spectra analysis. Among them, two phenols and six alkaloids were simultaneously quant...
Source: Biomedical Chromatography : BMC - August 24, 2009 Category: Biomedical Science Authors: Hu YM, Su GH, Sze SC, Ye W, Tong Y Tags: Biomed Chromatogr Source Type: journals
A new rapid ultra-performance liquid chromatography method for the pharmacokinetic and bioavailability study of diclofenac sodium aqueous injection and lipid microsphere injection in rats.
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A novel, rapid and selective ultra performance liquid chromatography mass spectrometric method had been developed for the pharmacokinetic study of diclofenac sodium (DS) after single intravenous injection of DS aqueous injection and DS lipid microsphere (LM) injection in rats. Ketoprofen (KP) was used as internal standard. Samples were treated by a one-step liquid liquid extraction. Separation was performed on an Acquity UPLC BEH C(18) column (50 x 2.1 mm i.d., 1.7 mum). The mobile phase consisted of acetonitrile-0.1% ammonium hydroxide aqueous solution (20 : 80, v/v) initially in the gradient mode. The detection was c...
Source: Biomedical Chromatography : BMC - August 24, 2009 Category: Biomedical Science Authors: Cui Y, Lin X, Guan TT, Zhang Y, Tang X Tags: Biomed Chromatogr Source Type: journals
Study of the effect of Wuzhi tablet (Schisandra sphenanthera extract) on tacrolimus tissue distribution in rat by liquid chromatography tandem mass spectrometry method.
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A liquid chromatography/tandem mass spectrometry (LC-MS/MS) method was developed and validated for determining tacrolimus (FK506) in rat tissues to study the effect of Schisandra sphenanthera extract on FK506 tissue distribution. After a liquid-liquid extraction with ethyl acetate, FK506 and ascomycin (IS) were subjected to LC-MS/MS analysis using positive electrospray ionization under multiple reactions monitoring mode. Chromatographic separation of FK506 and ascomycin was achieved on a Hypersil BDS C(18) column with a mobile phase consisting of methanol-water (containing 2 mM ammonium acetate, 95 : 5, v/v). The intra...
Source: Biomedical Chromatography : BMC - August 18, 2009 Category: Biomedical Science Authors: Qin XL, Bi HC, Wang CX, Li JL, Wang XD, Liu LS, Chen X, Huang M Tags: Biomed Chromatogr Source Type: journals
RP-HPLC determination of phenylalkanoids and monoterpenoids in Rhodiola rosea and identification by LC-ESI-TOF.
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PMID: 19691133 [PubMed - as supplied by publisher] (Source: Biomedical Chromatography : BMC)
Source: Biomedical Chromatography : BMC - August 16, 2009 Category: Biomedical Science Authors: Avula B, Wang YH, Ali Z, Smillie TJ, Filion V, Cuerrier A, Arnason JT, Khan IA Tags: Biomed Chromatogr Source Type: journals
Determination of bencycloquidium bromide in dog plasma by liquid chromatography with electrospray ionization tandem mass spectrometry.
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A rapid, selective and sensitive liquid chromatography/tandem mass spectrometry (LC-MS/MS) method was developed and validated for determining bencycloquidium bromide (BCQB) in beagle dog plasma. The plasma sample was deproteinized with methanol which contained l-ethyl-bencycloquidium bromide as internal standard, and supernantant was assayed by LC-MS/MS. The chromatographic separation was performed on a Phenomenex C(18) column (100 x 2.0 mm, i.d., 3.0 mum) with a gradient programme mobile phase consisting of methanol and ammonium acetate (5 mm) containing 0.15% acetic acid and at a flow rate of 0.3 mL/min. Electrospray...
Source: Biomedical Chromatography : BMC - August 16, 2009 Category: Biomedical Science Authors: Jiang B, Ruan Z, Lou H, Dong X, Xie Q Tags: Biomed Chromatogr Source Type: journals
LC-MS/MS method for the simultaneous determination of ethyl gallate and its major metabolite in rat plasma.
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A simple, rapid and sensitive liquid chromatography-tandem mass spectroscopy (LC-MS/MS) method was developed and validated for the determination of ethyl gallate, a pharmacologically active constituent isolated from Lagerstroemia speciosa (Linn.) Pers. This method was used to examine the pharmacokinetics of ethyl gallate and its major metabolite gallic acid in rat plasma using propyl gallate as an internal standard. After precipitation of the plasma proteins with acetonitrile, the analytes were separated on a Zorbax SB-C(18) column (3.5 mum, 2.1 x 50 mm) with an isocratic mobile phase consisted of methanol-acetonitrile...
Source: Biomedical Chromatography : BMC - August 16, 2009 Category: Biomedical Science Authors: Gao S, Zhan Q, Li J, Yang Q, Li X, Chen W, Sun L Tags: Biomed Chromatogr Source Type: journals
Determination of dimethyl sulfoxide and dimethyl sulfone in urine by gas chromatography-mass spectrometry after preparation using 2,2-dimethoxypropane.
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A method for routinely determination of dimethyl sulfoxide (DMSO) and dimethyl sulfone (DMSO(2)) in human urine was developed using gas chromatography-mass spectrometry. The urine sample was treated with 2,2-dimethoxypropane (DMP) and hydrochloric acid for efficient removal of water, which causes degradation of the vacuum level in mass spectrometer and shortens the life-time of the column. Experimental DMP reaction parameters, such as hydrochloric acid concentration, DMP-urine ratio, reaction temperature and reaction time, were optimized for urine. Hexadeuterated DMSO was used as an internal standard. The recoveries of...
Source: Biomedical Chromatography : BMC - August 16, 2009 Category: Biomedical Science Authors: Takeuchi A, Yamamoto S, Narai R, Nishida M, Yashiki M, Sakui N, Namera A Tags: Biomed Chromatogr Source Type: journals
