BIOMEDICAL CHROMATOGRAPHY
·
2019
·Vol. 33
·期 9
·e4555
·
IF 1.748
Ke-ke Cui,Yue-ting Cao,Jia-feng Shao,Zheng-yu Lu,Long-hu Wang
Bufadienolides are the main bioactive components of Venenum Bufonis (VB) and have been widely used to treat different types of human cancers for decades. The bufadienolide content in VB varies significantly in materials from different geographical origins. In this work, a new strategy for the quality assessment of VB was developed through quantitative analysis of multi-components by single marker (QAMS). Cinobufagin was selected as the internal reference substance; seven bufadienolides were separated and simultaneously determined based on relative correction factors. The correlation coefficient value ( r ≥ 0.9936) between QAMS and the normal external standard method proved the consistency of the two methods. According to the outcomes of 30 batches of VB samples, the contents of the seven bufadienolides were used for further chemometric analysis. All of the samples of VB from various geographical origins were divided into three categories based on hierarchical cluster analysis and radar plot, which indicated the crucial influence of geographical origins on VB. This study showed that QAMS combined with chemometristry could be used to comprehensively evaluate and effectively control the quality of VB from different geographical origins.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2019
·Vol. 33
·期 12
·e4688
·
IF 1.748
MingNa Sun,Lu Yu,Zhou Tong,Xu Dong,Yue Chu,Mei Wang,TongChun Gao,JinSheng Duan
Phenamacril is a new broad-spectrum fungicide that is commonly used for the control of fungal diseases in wheat and rice. In this study, ultra-high-performance liquid chromatography–tandem mass spectrometry was used to establish a method for analyzing the residual phenamacril in flour and rice based on the improved QuEChERS ( qu ick, e asy, ch eap, e ffective, r ugged and s afe) method using Z-Sep+ as the adsorbent in the pre-treatment process. The average recovery of phenamacril in flour and rice was 82.2–96.0%, the relative standard deviation was 2.1–5.6% and the limit of quantification was 0.5 μg/kg. The accuracy and sensitivity of this method meet the requirements for residue analysis. The method was applied to commercially available flour and rice samples, and the detected concentrations of phenamacril were 0.005–0.033 mg/kg. This method provides technical support for the safety evaluation of phenamacril.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 32
·期 10
·e4306
·
IF 1.688
Jie Yang,Zhi Sun,Duolu Li,Fei Duan,Zhuolun Li,Jingli Lu,Yingying Shi,Tanye Xu,Xiaojian Zhang
Shenkang injection is a traditional Chinese formula with good curative effect on chronic renal failure. In this paper, a novel, rapid and sensitive ultra-high-performance liquid chromatography coupled with Q Exactive hybrid quadrupole Orbitrap high-resolution accurate mass spectrometry was developed and validated for simultaneous determination of seven bioactive constituents of Shenkang injection in rat plasma and tissues after intravenous administration. Acetonitrile was used as a protein precipitation agent in biological samples disposal with carbamazepine as internal standard. The chromatographic separation was carried out on a C 18 column with a gradient mobile phase consisting of acetonitrile and water (containing 0.1% formic acid). The MS analysis was performed in the full-scan positive and negative ion mode. The lower limits of quantification for the seven analytes in rat plasma and tissues were 0.1–10 ng/mL. The validated method was successfully applied to tissue distribution and pharmacokinetic studies of Shenkang injection after intravenous administration. The results of the tissue distribution study showed that the high concentrations of seven constituents were primarily in the kidney tract. This is the first report of the application of Q-Orbitrap with full-scan mass spectrometry in tissue distribution and pharmacokinetic studies of Shenkang injection.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 32
·期 8
·e4256
·
IF 1.688
Fugeng Zhang,Xiaoli Qiao,Hui Lu,Shaoqiang Zhang,Wuxun Du,Xuefeng Xiao
Yiqifumai Injection is a lyophilized powder preparation widely used to treat coronary heart disease. However, its in vivo bioactive components and pharmacokinetic behavior remain unknown. Therefore a sensitive and specific LC–MS/MS was developed and validated for the simultaneous quantification of eight saponins and four lignans in beagle dog plasma. The plasma samples were pretreated by protein precipitation with methanol–acetonitrile (1:1, v /v). Chromatographic separation of all the 12 analytes and estazolam (internal standard, IS) was successfully accomplished on an Ultimate® XB-C 8 column (100 × 2.1 mm, 3 μm) with a gradient elution system. The total running time was 8 min with a flow rate of 0.40 mL/min. Acquisition of mass spectrometric data was performed via positive electrospray ionization in multiple reaction monitoring mode. The assay was fully validated in terms of selectivity, linear range, lower limit of quantitation, precision, accuracy, matrix effect, recovery and stability. This validated method was successfully applied to the pharmacokinetics of 12 bioactive components after intravenous administration of Yiqifumai Injection to beagle dogs at a dose of 0.541 g/kg.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 32
·期 9
·e4281
·
IF 1.688
Peng-Cheng Guo,Hua-Dan Shen,Jiang-Ji Fang,Tian-Ming Ding,Xiao-Ping Ding,Jun-Feng Liu
An on-line high-performance liquid chromatography–biochemical detection (HPLC-BCD) method, in which compounds separated by HPLC were on-line reacted with enzyme and substrate solutions delivered by flow injection and the enzyme inhibition signal was collected by UV detection, was developed to rapidly screen α -glucosidase inhibitors from green tea extracts in this study. The chromatographic fingerprints and enzyme inhibition profiles of the different brands of green tea could be simultaneously detected by the on-line HPLC-BCD method. Enzyme inhibition profiles were detected by the UV detector at 415 nm based on the reaction of α -glucosidase and p -nitrophenyl α - d -glucopyranoside (PNPG). PNPG (1.25 m m ), α -glucosidase (0.4 U/mL) and the flow rate 0.07 mL/min were applied as optimized parameters to detect α -glucosidase inhibitors in green tea. Four components in green tea showed α -glucosidase inhibition action and three of them were identified as HHDP-galloyl glucose, (−)-epigallocatechin-3-gallate and (−)-epicatechin-3-gallate by HPLC–fourier-transform mass spectrometry (HPLC-FTMS). Two brands of green tea derived from Mengding and Enshi mountainous areas might be superior to the other samples in the prevention and treatment of diabetes owing to their stronger activities of enzyme inhibitors. The proposed on-line HPLC-BCD method could be used to rapidly identify the potential enzyme inhibitors in complex matrixes.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 33
·期 4
·e4454
·
IF 1.688
Jing-Xian Zhang,Mei-Juan Qi,Mei-Zhi Shi,Jun-Jun Chen,Xiang-Qi Zhang,Jiao Yang,Ke-Zhi Zhang,Yong-Long Han,Cheng Guo
Danhong injection (DHI) is made from Salvia miltiorrhiza Bunge. and Carthamus tinctorius L. extract and is widely used in the clinical treatment of cardiovascular and cerebrovascular diseases. This study aimed to evaluate the effect of DHI on cytochrome P450 (CYP450) enzymes in vitro to predict drug–drug interactions based on CYP450 as combination therapy. To assess the inhibitory effect of DHI on CYP450, we detected the IC 50 value of DHI on CYP450 in vitro by liquid chromatography/tandem mass spectrometry (LC–MS/MS). Simultaneously, the induction effect of DHI on CYP450s was also evaluated. The relative induction ratios of DHI on CYP1A2, CYP2B6 and CYP3A4 activity were calculated by LC–MS/MS. The expression level of CYP3A4 mRNA was determined by reverse transcription PCR (RT-PCR). The LC–MS/MS data showed DHI intensively inhibit CYP2A6 activity and the intensity of inhibition was followed by CYP2C8, CYP3A4, CYP2C19, CYP2B6, CYP2D6, CYP1A2, CYP2E1 and CYP2C9 in vitro . The results of RT-PCR showed that there is a certain induction of DHI on CYP3A4 mRNA in human primary hepatocytes in vitro . The study suggested that drug–drug interactions might occur in clinical co-administration of drugs owing to the CYP2A6 inhibition and CYP3A4 induction.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 32
·期 11
·e4338
·
IF 1.688
Dan Huang,Qing-Song Jiang,Jun-Qing Yang,Ting Cui,Nian-Ru Wang,Ting-Ting Du,Xin-Hui Jiang
The determination of amino acids and monoamine with actions like neurotransmitters or modulators has become increasingly important for studying the relationship between the dysfunction of neurotransmitters and the pathogenesis of diabetic encephalopathy. Here, a high-performance liquid chromatography with fluorescence detection method was developed to simultaneously determine nine monoamines and amino acids including three excitatory neurotransmitters (aspartate, glutamate, and serotonin), four inhibitory neurotransmitters (glycine, γ -aminobutyric acid, taurine, dopamine), a precursor of 5-HT (tryptophan) and methionine using homoserine as the internal standard. The separation was performed on a BDS column with methanol-buffer solution of 35 mmol/L sodium acetate and 5 mmol/L citric acid (pH 6.0) using a simple gradient elution. Several parameters including specificity, precision, and recovery were validated after optimization of the analytical conditions. The developed method was successfully applied to determine the cortex and the hippocampus samples from Sprague–Dawley rats. Our results showed that various neurotransmitters involved in diabetes mellitus may tend to be differentially modulated and present a different alteration tendency at different time course, which might be associated with the duration of diabetes mellitus.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 33
·期 2
·e4400
·
IF 1.688
Lihua Zuo,Zhi Sun,Zhenhui Wang,Daling Ding,Tanye Xu,Liwei Liu,Li Gao,Shuzhang Du,Jian Kang,Xiaojian Zhang
Xuebijing injection (XBJI) is a traditional Chinese medicine prescription extracted from five Chinese herbs. Hydroxysafflor yellow A, oxypaeoniflorin, ferulic acid and benzoylpaeoniflorin are the main bioactive ingredients of XBJI. This paper presents an application of ultra-high-performance liquid chromatography–Q–exactive hybrid quadrupole–Orbitrap high-resolution mass spectrometry (UHPLC–Q–Orbitrap HRMS) to quantify four compounds of XBJI in rats various tissues for tissue distribution studies. The analytes were separated on a Waters Acquity UHPLC ® BEH C 18 column with a gradient mobile phase consisting of acetonitrile–water (containing 0.1% formic acid) at a flow rate of 0.2 mL/min. Mass spectrometric detection was performed by parallel reaction monitoring via a heated electrospray ionization source under the negative ionization mode. The method was validated in various tissue samples, and has demonstrated great performance for rapidity, accuracy, high sensitivity and selectivity. It was successfully applied to the tissue distribution studies of XBJI after intravenous administration to rats. It was also the first study to investigate the tissue distribution of XBJI in rats and we found that the concentrations of four compounds were high in kidney, liver, stomach and intestine. The clinical use of XBJI should focus on its pharmacodynamics and safety studies in these tissues.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2019
·Vol. 33
·期 9
·e4581
·
IF 1.748
Zheng Zhang,Yuqing Tang,Bocheng Yu,Jiaming Ying,Bingchu Wu,Jinyi Wu,Jinshun Zhao,Zhenjun Chen,Jinyan Xu,Chunlan Tang
The chemical fingerprinting and metabolite profile in a rat plasma sample after intragastric administration of Yangyin qingfei decoction (YYQFD, 14 g/kg) were investigated. First, YYQFD was analyzed by UPLC/Q-TOF MS to establish the chemical composition database by comparing their retention behavior, accurate molecular mass and MS 2 data with those of references or known compounds in the literature. In this database, 100 chemical constituents with information on retention time, molecular mass, molecular formula, MS 2 data and compound name were identified, which can provide compound information for further metabolite profiling studies. Furthermore, 64 compounds including 37 prototypes and 27 metabolites were detected in the dosed rat plasma sample, and the metabolic pathways of YYQFD were hydrolyzation, hydroxylation, dehydrogenation, glucuronidation, glucosylation, sulfation and mixed modes. Among the five component herbs in the YYQFD, Glycyrrhizae Radix et Rhizome and Fritillariae Thunbergii bulbs were actively metabolized, contributing 16 and 7 metabolites, respectively. It is suggested that chemical characterization and metabolite profiling studies are valuable to elucidate the material basis of herbal preparations.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2019
·Vol. 33
·期 9
·e4568
·
IF 1.748
Liping Zhou,Hexiang Liu,Zhongyong Xu,Su Guan,Lei Zhang
Febuxostat is a novel nonpurine type of highly selective xanthine oxidoreductase inhibitor. A rapid and sensitive ultra-high-performance liquid chromatography–quadrupole time-of-flight mass spectrometry method for simultaneous separation and determination of febuxostat and its metabolites in rat serum and urine was developed at various time points after oral administration to the rats. The febuxostat metabolites were predicted by biotransformation software and transformed to a personal compound database to quickly determine the possible metabolites from the MS1 data. The possibility of the MS/MS fragmentation was calculated by the Molecular Structure Correlator software. As a result, five phase I and two phase II metabolites in rat serum, and seven phase I and three phase II metabolites in rat urine were identified, of which four metabolites (M2, M5, M6, M7) have not been reported before. The metabolite toxicities are predicted, and the results are helpful for the design of new xanthine oxidoreductase inhibitors.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 32
·期 8
·e4250
·
IF 1.688
Lin-Hu Ye,Xin-Qian Zhao,Ling-Ti Kong,Li-Sha Wang,Xue Tao,Hui Wu,Mei He,Qi Chang
Danhong Injection (DHI) as a Chinese patent medicine is mainly used to treat ischemic encephalopathy and coronary heart disease in combination with other chemotherapy. However, the information on DHI's potential drug interactions is limited. The goal of this work was to examine the potential P450-mediated metabolism drug interaction arising from DHI and its active components. The results showed that DHI inhibited CYP2C19, CYP2D6, CYP3A4, CYP2E1 and CYP2C9 with IC 50 values of 1.26, 1.42, 1.63, 1.10 and 1.67% ( v /v), respectively. Danshensu and rosmarinic acid inhibited CYP2E1 and CYP2C9 with IC 50 values of 36.63 and 75.76 μ m , and 34.42 and 76.89 μ m , respectively. Salvianolic acid A and B inhibited CYP2D6, CYP2E1 and CYP2C9 with IC 50 values of 33.79, 21.64 and 31.94 μ m , and 45.47, 13.52 and 24.15 μ m , respectively. The study provides some useful information for safe and effective use of DHI in clinical practice.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2015
·Vol. 30
·期 4
·601-605
·
IF 1.723
Zhaoli Ling,Ping Xu,Zeyu Zhong,Fan Wang,Nan Shu,Ji Zhang,Xiange Tang,Li Liu,Xiaodong Liu
A new pre-column derivative high-performance liquid chromatography (HPLC) method for determination of d -glucose with 3- O -methyl- d -glucose (3-OMG) as the internal standard was developed and validated in order to study the gluconeogenesis in HepG2 cells. Samples were derivatized with 1-phenyl-3-methy-5-pyrazolone at 70°C for 50 min. Glucose and 3-OMG were extracted by liquid–liquid extraction and separated on a YMC-Triart C 18 column, with a gradient mobile phase composed of acetonitrile and 20 m m ammonium acetate solution containing 0.09% tri-ethylamine at a flow rate of 1.0 mL/min. The eluate were detected using a UV detector at 250 nm. The assay was linear over the range 0.39–25 μ m ( R 2 = 0.9997, n = 5) and the lower limit of quantitation was 0.39 μ m (0.070 mg/mL). Intra- and inter-day precision and accuracy were <15% and within ±3%, respectively. After validation, the HPLC method was applied to investigate the gluconeogenesis in Dulbecco's modified Eagle medium (DMEM) cultured HepG2 cells. Glucose concentration was determined to be about 1–2.5 μ m in this gluconeogenesis assay. In conclusion, this method has been shown to determine small amounts of glucose in DMEM successfully, with lower limit of quantitation and better sensitivity when compared with common commercial glucose assay kits. Copyright © 2015 John Wiley & Sons, Ltd.
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