Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Impact Factor & Information

Publisher: Elsevier

Journal description

The Journal of Chromatography B. addresses advancements in and applications of analytical methodologies related to drugs, other pharmacologically active compounds, metabolites, as well as to bio-polymers such as proteins and nucleic acids. The areas considered include: clinical analysis, therapeutic drug monitoring, pharmaceutical analysis and novel approaches to sample preparation in bioanalysis; the qualitative and quantitative analysis of proteins, peptides and their post-translational modifications as well as nucleic acids; the screening and profiling of body fluids and tissues related to monitoring the level of active substances, including metabolites, biomarkers and toxicants; the comparative analysis of biological systems and proteomics and genomics including novel ways of data handling and interpretation; analytical techniques covered include the various facets of chromatography, electrophoresis and related methods, including mass spectrometry and affinity-based methodologies.

Current impact factor: 2.69

Impact Factor Rankings

2015 Impact Factor Available summer 2015
2013 / 2014 Impact Factor 2.694
2012 Impact Factor 2.487
2011 Impact Factor 2.888
2010 Impact Factor 2.971
2009 Impact Factor 2.777
2008 Impact Factor 2.5
2007 Impact Factor 2.935
2006 Impact Factor 2.647
2005 Impact Factor 2.391
2004 Impact Factor 2.176
2003 Impact Factor 2.085
2002 Impact Factor 1.913
1996 Impact Factor 1.341
1995 Impact Factor 1.255
1994 Impact Factor 1.209

Impact factor over time

Impact factor
Year

Additional details

5-year impact 0.00
Cited half-life 6.60
Immediacy index 0.36
Eigenfactor 0.04
Article influence 0.73
Website Journal of Chromatography B website
ISSN 1873-376X

Publisher details

Elsevier

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    • NIH Authors articles will be submitted to PubMed Central after 12 months
    • Publisher last contacted on 18/10/2013
  • Classification
    ​ green

Publications in this journal

  • [Show abstract] [Hide abstract]
    ABSTRACT: In this work, a simple, sensitive and fast ultra performance liquid chromatography with tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for the quantitative determination of vortioxetine in rat plasma. Plasma samples were processed with a protein precipitation. The separation was achieved by an Acquity UPLC BEH C18 column (2.1mm×50mm, 1.7μm) column with a gradient mobile phase consisting of 0.1% formic acid in water and acetonitrile. Detection was carried out using positive-ion electrospray tandem mass spectrometry via multiple reaction monitoring (MRM). The validated method had an excellent linearity in the range of 0.05-20ng/mL (R(2)>0.997) with a lower limit of quantification (0.05ng/mL). The extraction recovery was in the range of 78.3-88.4% for vortioxetine and 80.3% for carbamazepine (internal standard, IS). The intra- and inter-day precision was below 8.5% and accuracy was from -11.2% to 9.5%. No notable matrix effect and astaticism was observed for vortioxetine. The method has been successfully applied to a pharmacokinetic study of vortioxetine in rats for the first time, which provides the basis for the further development and application of vortioxetine. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 08/2015; 997. DOI:10.1016/j.jchromb.2015.05.010
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    ABSTRACT: Multi-analytes simultaneous monitoring of amino acid and monoamine neurotransmitters (NTs) has important scientific significance for their related pathology, physiology and drug screening. In this work, in virtue of a mass spectrometry sensitizing reagent 10-ethyl-acridone-3-sulfonyl chloride (EASC) as derivatization reagent, an Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry (UHPLC-MS/MS) method was developed and validated for simultaneous determination of six amino acid NTs, two monoamine ones and its one metabolite. The simple and rapid derivatization reaction was innovatively combined with plasma preparation by using EASC acetonitrile solution as protein precipitant. This interesting combination brought the advantages of speediness, simpleness and high-throughput in a cost-effective way. Under the optimized conditions, LODs (0.004-3.80nM) and LOQs (0.014-13.3nM) of EASC derivatized-NTs were calculated and found to be significantly lower than those of direct UHPLC-MS/MS detection about 11.5-275.0 and 14.4-371.4 times, respectively. Moreover, EASC derivatization significantly improved chromatographic resolution and matrix effect when compared with direct UPLC-MS/MS detection method without derivatization. Meanwhile, it also brought acceptable precision (3.0-13.0%, peak area CVs%), accuracy (86.4-112.9%), recovery (88.3-107.8%) and stability (3.8-8.5%, peak area CVs%) results. This method was successfully applied for the antiparkinsonian effect evaluation of levodopa and Ginsenoside Rg1 using PC12 cells and rats models by measuring multiple NTs. This provided a new method for the NTs related studies in the future. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 07/2015; 995. DOI:10.1016/j.jchromb.2015.05.017
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    ABSTRACT: In the present study, the modification of a polysulfone hollow fiber membrane with in situ molecularly imprinted sol-gel process (as a novel and one-step method) was prepared and investigated. 3-(propylmethacrylate)trimethoxysilane (3PMTMOS) as an inorganic precursor was used for preparation of molecularly imprinted sol-gel. The modified molecularly imprinted sol-gel hollow fiber membrane (MSHM) was used for the liquid-phase microextraction (LPME) of hippuric acid (HA) in human plasma and urine samples. MSHM as a selective, robust, and durable tool was used for at least 50 extractions without significant decrease in the extraction efficiency. The non-molecularly imprinted sol-gel hollow fiber membrane (NSHM) as blank hollow fiber membrane was prepared by the same process, only without HA. To achieve the best condition, influential parameters on the extraction efficiency were thoroughly investigated. The capability of this robust, green, and simple method for extraction of HA was successfully accomplished with LC/MS/MS. The limits of detection (LOD) and quantification (LOQ) in human plasma and urine samples were 0.3 and 1.0nmolL(-1), respectively. The standard calibration curves were obtained within the concentration range 1-2000nmolL(-1) for HA in human plasma and urine. The coefficients of determination (r(2)) were ≥0.998. The obtained data exhibited recoveries were higher than 89% for the extraction of HA in human plasma and urine samples. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 07/2015; 995. DOI:10.1016/j.jchromb.2015.05.005
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    ABSTRACT: The main objective of this work was to develop a method to measure Leucine (Leu) and β-hydroxymethylbutyrate (HMB) at basal levels in serum, urine, milk and brain microdialysates in rats. Ultrahigh performance liquid chromatography-electrospray-tandem mass spectrometry (UHPLC-ESI-MS/MS) was used as analytical technique. The sample treatment was simple and consisted of dilution with methanol and centrifugation for serum and urine, dilution with water and filtration with an Amicon filter for milk, and treatment with formic acid with no further dilution for microdialyzates. The procedures for sampling and the UHPLC-MS/MS parameters were accurately optimized to achieve the highest recoveries and to enhance the analytical characteristics of the method. For chromatographic separation, an Acquity UPLC BEH Amide column using acetonitrile-water gradient with formic acid as additive was used. The total run time was 4min. The analytical characteristics (accuracy, selectivity and sensitivity) of the proposed method were evaluated. The limits of detection (LODs) obtained ranged from 0.4 to 7ngmL(-1) and the limits of quantification (LOQs) from 1 to 22ngmL(-1). Precision, expressed as relative standard deviation (% RSD), was lower than 15% in all cases, and the determination coefficient (R(2)) was equal or higher than 99.0% with a residual deviation for each calibration point lower than ±25%. Mean recoveries were between 85 and 115%. The method was successfully applied to these matrices being able to detect significant differences between physiological situations, strains and stages of life. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 07/2015; 995. DOI:10.1016/j.jchromb.2015.05.013
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    ABSTRACT: A rapid and sensitive liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed and validated for the simultaneous determination of acetylpuerarin (AP) and its major metabolite puerarin (PUE) in rat plasma using genistein as the internal standard (IS). Plasma samples were pretreated by protein precipitation with a mixture of methanol and acetonitrile. Chromatographic separation was performed on a CAPCELL PAK C18 MGШ column with a mixture of 0.1% formic acid in water and methanol (35:65, v/v) as the mobile phase. The analytes were detected using a tandem mass spectrometer in the positive ionization and multiple-reaction monitoring mode. The ion transition of m/z 669.4→627.3, 417.5→297.6 and 271.3→153.0 was utilized to quantify AP, PUE and the IS, respectively. The calibration curves showed good linearity over the plasma concentration range of 1-2000ng/mL for AP and 2.5-5000ng/mL for PUE. The intra- and inter-day precisions (RSD %) for each analyte were less than 6.91%, and the accuracies ranged from -2.17% to 2.93%. The validated LC-MS/MS method was further successfully applied to a pharmacokinetic study of AP and PUE in rats following intravenous and oral administration. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 07/2015; 995. DOI:10.1016/j.jchromb.2015.05.009
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    ABSTRACT: A simple and efficient technique based on liquid phase extraction with CH2Cl2 solvent followed by derivatization with (C2H5)2O·BF3 solution and confirmation analysis with GC-MS analytical method was developed for detecting the bensulfuron-methyl (BSM) residues in water. Box-Behnken response surface methodology was employed for optimization of the derivatization efficiency. According to the optimization model, the derivatization time of 45min, derivatization temperature at 55°C and 0.2mL (C2H5)2O·BF3 solvent were selected as the optimal derivatization condition for obtaining the maximum desirability of response. Method validation was performed at 6 working standard levels (0.05, 0.1, 0.2, 0.5, 1.0, 5.0μg/mL) and the linearity of the calibration curve was linear well over the 6 fortification levels with the squared correlation coefficient of determination r(2)=0.998 and the LOD was found to be 0.1μg/L for BSM herbicide. The mean value of BSM was detected from 0.0414 to 4.7542μg/mL at levels from 0.05 to 5μg/mL with the recoveries remained at the acceptable level (42.8-95.0%) with the RSD values from 3.5% to 6.2%, which is more accptable and desirable than the results obtained by LC methods. Moreover, the method allowed the determination of BSM residue in real paddy field water samples at concentrations between 0.0902 and 3.4605μg/L. Average recovery rates of the BSM spiked at levels 0.1, 0.2, 0.5, 1.0μg/mL into thirty water samples ranged from 74.1% and 94.1% with the relative standard derivation (RSD) values from 1.9% to 6.7%. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 07/2015; 995. DOI:10.1016/j.jchromb.2015.05.008
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    ABSTRACT: Fetal lung maturity is estimated using the lecithin/sphingomyelin ratio (L/S ratio) in amniotic fluid and it is commonly measured with thin-layer chromatography (TLC). The TLC method is time consuming and technically difficult; however, it is widely used because there is no alternative. We evaluated a novel method for measuring the L/S ratio, which involves a tip-column with a cation-exchange resin and mass spectrometry. Phospholipids in the amniotic fluid were extracted using methanol and chloroform. Choline-containing phospholipids such as lecithin and sphingomyelin were purified by passing them through the tip-column. LC-MS/MS and MALDI-TOF were used to directly analyze the purified samples. The L/S ratio by mass spectrometry was calculated from the sum peak intensity of the six lecithin, and that of sphingomyelin 34:1. In 20 samples, the L/S ratio determined with TLC was significantly correlated with that obtained by LC-MS/MS and MALDI-TOF. There was a 100% concordance between the L/S ratio by TLC and that by LC-MS/MS (kappa value=1.0). The concordance between the L/S ratio by TLC and that by MALDI-TOF was also 100% (kappa value=1.0). Our method provides a faster, simpler, and more reliable assessment of fetal lung maturity. The L/S ratio measured by LC-MS/MS and MALDI-TOF offers a compelling alternative method to traditional TLC. Copyright © 2015. Published by Elsevier B.V.
    Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 07/2015; 993. DOI:10.1016/j.jchromb.2015.05.012
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    ABSTRACT: Camellianin A is a major active constituent of Adinandra nitida. A LC-MS/MS method for the determination of camellianin A and its metabolite (camellianin B) in rat plasma and tissues was developed and applied to a pharmacokinetics and tissue distribution study. Samples were separated on a Waters HSS T3 column with a mobile phase consisted of methanol and water (containing 0.1% formic acid). MS/MS detection was carried out on a triple-quadruple mass spectrometer under negative ESI mode. Pharmacokinetics study showed that camellianin A was rapidly eliminated with a t1/2 of 92.6±41.4h and CL of 3.19±0.471L/min/kg. Additionally, camellianin A showed a low oral bioavailability of 2.99% and a narrow tissue distribution; however, camellianin B was proved to have a wide tissue distribution with brain penetration. The data presented in this study provides useful information for the further applications of A. nitida and camellianin A. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 06/2015; 997. DOI:10.1016/j.jchromb.2015.06.012
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    ABSTRACT: Two chromatographic methods for the quantitative analysis of uridine diphosphate (UDP) sugars involved in hyaluronan pathway of Streptococcus zooepidemicus (SEZ) were developed and compared. The sample preparation protocol using centrifugation and extraction in hot ethanol was employed prior to the analyses. Separation was achieved using an anion exchange Spherisorb SAX column or a Shodex QA-825 column connected with a photodiode array (PDA) detector. To increase the throughput of the chromatography method employing the Spherisorb SAX column, the solid phase extraction (SPE) procedure was introduced. Method validation results displayed that limits of detection (LODs) of UDP-glucose (UDP-Glc), UDP-N-acetylglucosamine (UDP-GlcNAc) and UDP-glucuronic acid (UDP-GlcA) calculated according to QC Expert software were in the low micromolar range and the coefficient of correlation (R(2)) was above 0.997. However, the analytical technique using the Spherisorb SAX column resulted in 80-90% recoveries and low LODs (≤6.19μM), the Shodex QA-825 column showed better long-term stability and reproducible chromatographic properties (RSD≤5.60%). The Shodex QA-825 column was successfully used to monitor UDP-sugar levels during the growth rate of SEZ cells. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 06/2015; 997. DOI:10.1016/j.jchromb.2015.05.038
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    ABSTRACT: Herein, we report an on-line two-dimensional system constructed by counter-current chromatography (CCC) coupling with preparative high-performance liquid chromatography (prep-HPLC) for the separation and purification of polar natural products. The CCC was used as the first dimensional isolation column, where an environmental friendly polar two-phase solvent system of isopropanol and 16% sodium chloride aqueous solution (1:1.2, v/v) was introduced for low toxicity and favorable resolution. In addition, by applying the stop-and-go flow technique, effluents pre-fractionated by CCC was further purified by a preparative column packed with octadecyl silane (ODS) as the second dimension. The interface between the two dimensions was comprised of a 6-port switching valve and an electronically controlled 2-position 10-port switching valve connected with two equivalent holding columns. To be highlighted here, this rationally designed interface for the purpose of smooth desalination, absorption and desorption, successfully solved the solvent compatibility problem between the two dimensional separation systems. The present integrated system was successfully applied in a one-step preparative separation and identification of 10 pure compounds from the water extracts of Tieguanyin tea (Chinese oolong tea). In short, all the results demonstrated that the on-line 2D CCC×LC method is an efficient and green approach for harvesting polar targets in a single step, which showed great promise in drug discovery. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 06/2015; 997:179-186. DOI:10.1016/j.jchromb.2015.06.011
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    ABSTRACT: Herein, an aptamer-based affinity chromatography method for rapid and single step purification of Concanavalin A is developed and validated. We have used a 41ntssDNA aptamer of Con A (Con A aptabody) as an affinity reagent in the developed aptamer-affinity chromatography. Stationary phase of the method consists of surface functionalized agarose beads carrying covalently immobilized Con A-aptabody. Affinity purification of Con A from jack bean (Canavalia ensiformis) seed using developed aptamer-affinity columns has resulted in ≥66% recovery with 90% purity and 336-fold purification of Con A. The developed aptamer-affinity chromatography has shown efficient scalability and consistent purification when analysed over 13mm, 20mm and 25mm diameter columns having a bed height of 60mm each. Also, the developed aptamer-agarose columns were found to be reusable with recovery decrease of 12.9% in seven sequential cycles of purification. Therefore, the developed aptamer-affinity chromatography provides a novel, efficient and single-step methodology for isolation and purification of Con A. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 06/2015; 997. DOI:10.1016/j.jchromb.2015.06.003
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    ABSTRACT: Removal of the wool-bearing skin around a young lamb's rump (mulesing) provides long term health benefits for the animal, and the use of a sedative and analgesic agent such as xylazine may assist with pain relief to reduce discomfort and stress. Sensitive analytical methods are essential for monitoring pharmaceuticals and their metabolites in animals destined for human consumption. The following work reports a method that is 200 times more sensitive for xylazine detection than previously published methods, with lower limits of quantitation for xylazine and its primary metabolite in animals of 0.5pg and 2pg on-column, respectively. The use of a square wave solvent gradient immediately prior to analyte elution resulted in larger MS/MS peaks and a reduction in baseline noise, allowing reliable detection of lower analyte concentrations. The method uses as little as 1mL of plasma which allows replication within a sample if required, and requires simple sample preparation, minimising the introduction of matrix components into the MS/MS. Crown Copyright © 2015. Published by Elsevier B.V. All rights reserved.
    Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 06/2015; 997. DOI:10.1016/j.jchromb.2015.06.005
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    ABSTRACT: Hypoglycin A has been recently identified has the causal agent of atypical myopathy (AM) in horses. Its identification and quantification in equine's biological fluids is thus a major concern to confirm maple poisoning and to provide insight into the poorly understood mechanism of hypoglycin A intoxication. Quantification of hypoglycin A has been achieved with the aTRAQ kit for amino acid analysis of physiological fluids (AB Sciex). Acquisition method on mass spectrometer has been updated to record the hypoglycin A specific MRM transition. Outlined accuracy profiles demonstrated very reliable data. A good linearity was observed from 0.09 to 50μmol/L and precision was very good with coefficient of variation below 8%. Fifty-five samples collected from 25 confirmed AM horses revealed significant hypoglycin A concentrations, while toxin was not found in serum of 8 control animals. The described aTRAQ variant method has been analytically and clinically validated. The reliability of our approach is thus demonstrated into the workup of atypical myopathy. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 06/2015; 997:75-80. DOI:10.1016/j.jchromb.2015.06.004
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    ABSTRACT: An ultra-high performance liquid chromatographic-tandem mass spectrometry (UHPLC-MS/MS) method for quantification of potato steroidal alkaloids, namely α-solanine, α-chaconine, solanidine and demissidine was developed and validated. Three different column chemistries, i.e. ethylene bridged hybrid (BEH) C18, hydrophilic lipophilic interaction and amide columns, were assessed. The BEH C18 column showed best separation and sensitivity for the alkaloids. Validation data (inter-day and intra-day combined) for accuracy and recovery ranged from 94.3 to 107.7% and 97.0 to 103.5%, respectively. The accuracy data were within the acceptable range of 15% as outlined in the United States Food and Drug Administration (USFDA) guidelines. The recovery data were consistent and reproducible with a coefficient of variation (CV) ranging from 6.2 to 9.7%. In addition, precision of the method also met the criteria of the USFDA with CV values lower than 15% even at lower limit of quantification (LLOQ), while the permissible variation is considered acceptable below 20%. The limit of detection and LLOQ of the four alkaloids were in the range of 0.001-0.004μg/mL whereas the linearities of the standard curves were between 0.980 and 0.995. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 06/2015; 997. DOI:10.1016/j.jchromb.2015.05.033
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    ABSTRACT: A reversed-phase HPLC-UV method was developed, optimized, and validated for the separation and quantitation of six target alkaloids from leaves of Nicotiana species (nicotine, nornicotine, anatabine, anabasine, myosmine, and cotinine). A bidentate reversed-phase C18 column was used as stationary phase and an alkaline ammonium formate buffer and acetonitrile as mobile phase. The alkaloids were well separated in a short run time of 13min with mobile phase pH 10.5 and a small gradient of 9-13% acetonitrile, and detected using UV at 260nm. Peak parameters were acceptable for all six closely related alkaloids. The proposed method has enough linearity with correlation coefficient >0.999 within the investigated range for all tested alkaloids. Satisfactory precision was achieved for both intra- and inter-day assay, with RSD less than 2% for all alkaloid standards. Reproducibility was also within the acceptable range of RSD <2%. Limit of detection was 1.6μg/mL for nicotine and below 1μg/mL for all other alkaloids. The limit of quantification was 2.8 and 4.8μg/mL for nornicotine and nicotine respectively, and below 2μg/mL for all other alkaloids. The method was successfully applied for simultaneous analysis of alkaloids in leaves of Nicotiana benthamiana. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 06/2015; 997. DOI:10.1016/j.jchromb.2015.06.006
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    ABSTRACT: UTL-5g is a novel small-molecule TNF-α inhibitor under investigation as both a chemoprotective and radioprotective agent. Animal studies showed that pretreatment of UTL-5g protected kidney, liver, and platelets from cisplatin-induced toxicity. In addition, UTL-5g reduced liver and lung injuries induced by radiation in vivo. Although a number of preclinical studies have been conducted, a validated bioanalytical method for UTL-5g in human plasma has not been published. In this work, a sensitive and reproducible reverse-phase liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) assay was developed and validated for the determination of UTL-5g and its metabolites, 5-methylisoxazole-3-carboxylic acid (ISOX) and 2,4-dichloroaniline (DCA), in human plasma. The method involves a simple methanol precipitation step followed by injection of the supernatant onto a Waters 2695 HPLC system coupled with a Waters Quattro Micro™ triple quadrupole mass spectrometer. Chromatographic separation was accomplished using a Waters Nova-Pak C18 column maintained at 30°C, running at gradient mode with mobile phase consisting of 0.1% formic acid in water and 0.1% formic acid in methanol at a flow rate of 0.2mL/min. The analytes were monitored under positive electrospray ionization (ESI). Quantitation of these compounds in plasma was linear from 0.05 to 10μM. The lower limit of quantitation (LLOQ) was 0.05, 0.1, and 0.2μM for UTL-5g, ISOX and DCA, respectively. The accuracy and intra-and inter-day precisions were within the generally accepted criteria for bioanalytical method (<15%). This method provides a practical tool to measure and characterize the plasma concentration-time profiles for UTL-5g and its metabolites, ISOX and DCA. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 06/2015; 991. DOI:10.1016/j.jchromb.2015.04.015
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    ABSTRACT: In this study, a method for the quantitation of SK5474 in rat plasma was developed and validated using high performance liquid chromatography (HPLC). The plasma samples were prepared by deproteinization, and sildenafil was used as an internal standard. Chromatographic separation was achieved using a reversed-phase (C18) column. The mobile phase, 0.02M ammonium acetate buffer:acetonitrile (48:52, v/v), was run at a flow rate of 1.0mL/min, and the column eluent was monitored using an ultraviolet detector at 254nm at room temperature. The retention times of sildenafil and SK5474 were approximately 5.8 and 7.2min, respectively. The quantitation limit of SK5474 in rat plasma was 0.03μg/mL. Pharmacokinetic parameters of SK5474 was evaluated after intravenous (i.v.; at doses of 15mg/kg) and oral (p.o.; at doses of 30mg/kg) administration of SK5474 in rats. After p.o. administration (30mg/kg) of SK5474, F (fraction absorbed) value was approximately 46.0%. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 06/2015; 991. DOI:10.1016/j.jchromb.2015.04.010
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    ABSTRACT: Peroxiredoxins (Prxs) are a family of thiol peroxidases, which have been suggested to serve as biomarkers for diseases caused by oxidative stress. In this study, we established a high performance liquid chromatography (HPLC) method for quantifying the amount of Prx2 in red blood cells (RBCs). RBC proteins were separated using HPLC, and a single peak was detected that matched that produced by recombinant Prx2. Under improved conditions, the calibration curve for Prx2 (reduced form) was linear over the range of 0.5-20.0μg with a correlation coefficient of 0.999. The minimum detectable level of the recombinant Prx2 was 0.2μg, with a signal-to-noise ratio of 3 per 20μl of injection volume. SDS-PAGE and mass spectrometric analysis showed that the proteins comprising the peak were almost exclusively Prx2. Further high-resolution analysis using nanoLC-MS/MS demonstrated that the oxidation sensitive, Cys-51 was carbamidomethylated by iodoacetamide-alkylation during in-gel digestion but was not modified with sulfinic acid (-SO2H) or sulfonic acid (-SO3H). These results indicated that the separated Prx2 was the reduced form and not the hyperoxidized form. These basic experiments allowed us to determine the relative amounts of native Prx2 in RBCs taken from healthy subjects. The average levels of Prx2 in male and female subjects were 7.28ng/mg and 8.29ng/mg, respectively, and no significant difference was observed between the sexes. Therefore, the HPLC method with UV detection described herein offers a convenient method to quantitatively determine the levels of reduced form of Prx2 and its oxidative decrease in human RBCs. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 06/2015; 997. DOI:10.1016/j.jchromb.2015.06.007
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    ABSTRACT: Cnidilin is one of the major bioactive constituents of Radix Angelicae dahuricae. The present study was designed to characterize and interpret the structures of metabolites in rats after oral administration of cnidilin at a dose of 48mg/kg body weight. Metabolite identification was accomplished using a predictive multiple reaction monitoring-information-dependent acquisition-enhanced product ion (pMRM-IDA-EPI) scan and precursor ion scan-information-dependent acquisition-enhanced product ion (PREC-IDA-EPI) scan in positive ion mode. Comparing the changes in protonated molecular masses, MS/MS spectra and retention times with the parent drug, 18 metabolites were identified. The result shows that the metabolic pathways contain deisopentenyl, combination with glucose, hydroxylation, oxidation, demethylation and addition reaction. The study identified 18 metabolites, analyzed and summarized the fragmentation regularities of mass spectra of 8-methoxy-5-hydroxy psoralen. The study provides a new pathway to discovery new compounds, new fragmentation regularities and the mode of metabolites. Copyright © 2015 Elsevier B.V. All rights reserved.
    Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 05/2015; 995-996C:85-92. DOI:10.1016/j.jchromb.2015.05.002