CHROMATOGRAPHIA
·
2025
·
IF 1.3
Jiang Qiaoling,Wu Qiaoli,Chen Shuhang,Zeng Tianfu,Tong Xiaoyi
This study introduces a rapid LC–MS/MS method designed to simultaneously quantify 14 water-soluble vitamins and their metabolites in human serum. The protein precipitation with metaphosphoric acid and stable isotope dilution techniques are utilized in this method. An Agilent XDB C18 column and dynamic ionization mode switching are adopted, enabling the completion of a single sample analysis within 5 min. The method has undergone rigorous validation. The lower limits of quantification (LLOQs) range from 0.3 to 400 ng/mL, with recovery rates between 80 and 120%. Intra-day and inter-day relative standard deviations (RSDs) are below 15%. The matrix effects are controlled within ± 15%, and the analyte carryover is less than 20% of the LLOQ. The stability tests have demonstrated that samples remain stable at room temperature (25 °C) for 10 h, at − 20 °C for 7 days, and can withstand one freeze–thaw cycle. Extracted samples are stable in the autosampler (4 °C) for 24 h. The method was applied to serum samples from 150 healthy individuals. Non-parametric statistical analysis was carried out to establish clinical reference intervals, which provides valuable data for the clinical evaluation of vitamin and metabolite levels in serum.
研究领域:
临床医学
·
分析化学
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产品关联
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2023
·
IF 3.4
Bingqing Zhang,Xueyong Li,Yiying Chen,Bo Chen,Yu Cheng,Hailing Lin,Wancai Que,Maobai Liu,Lili Zhou,Hui Zhang,Hongqiang Qiu,Chaoyang Wu
Polymyxin B (PB) is currently one of the last resort treatment options against carbapenem-resistant gram-negative bacterial pathogens. Pharmacokinetics/pharmacodynamics (PK/PD) guided therapeutic drug monitoring (TDM) of antibiotics is critical for optimizing dosage regimens to maximize efficacy, minimize toxicity, and delay the emergence of resistance. Currently, methods for determining PB in human plasma and epithelial lining fluid (ELF) are limited. In this study, we developed and validated a simple method for PB determination in human plasma and ELF using LC-MS/MS. Protein precipitation of the sample was conducted with 0.1% formic acid-acetonitrile. Polymyxin B1 and B2 were separated on a C 18 column and detected within 4 min by the mass spectrometer in the positive mode coupled with multiple reaction monitoring. The calibration curve range was 0.156–10.0 and 0.0156–1.00 μg/mL in the plasma for polymyxin B1 and B2, respectively, and was 0.0625–2.00 and 0.00625–0.200 μg/mL for polymyxin B1 and B2, respectively in bronchoalveolar lavage fluid. The accuracy of the intra- and inter-assay studies ranged from 80.6% to 114.9%, and the coefficients of variation for intra- and inter-day assays were less than 14.8%. Among a considerable number of patients, the average steady-state plasma concentration of PB was suboptimal. Moreover, the exposure to PB in patients with acute kidney injury (AKI) was considerably higher than that in patients without AKI. Meanwhile, a higher concentration of PB in ELF could be achieved than that in plasma after PB nebulization treatment. The established method was proven to be rapid, simple, and suitable for TDM of PB and PK/PD studies in human plasma and ELF.
研究领域:
药理学
·
临床医学
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DOI
PubMed
高影响因子
Current Pharmaceutical Analysis
·
2022
·Vol. 18
·期 10
·919-929
·
IF 0.743
Gao Pan,Zou Qiao-gen
Background: Perampanel (PER) is a third-generation antiepileptic drug (AED). Several methods have been developed for the quantification of perampanel in plasma. The pharmacokinetic characteristics of perampanel in healthy Chinese ubjects have not been comprehensively reported.
Objective: A simple, fast and sensitive LC-MS/MS method was established and validated for the quantification of perampanel in human plasma and its application to a bioequivalence study. Methods: Chromatographic separation was accomplished on a ZORBAX Eclipse XDB-Phenyl column (4.6 mm
× 75 mm, 3.5 μm) using a binary gradient with mobile phase (A) (water containing 5 mmol/L ammonium acetate and 0.1% formic acid and (B) acetonitrile-water (95:5, v/v) at a flow rate of 0.9 mL/min and sample preparation was by one-step protein precipitation via acetonitrile. Results:
The total run time in this study was 4.5 min and the retention time of perampanel and perampanel-d5 (internal standard) were 2.30 min and 2.32 min, respectively. The method was developed and validated over the concentration range of 2.00-500 ng/mL for perampanel, with a correlation coefficient
greater than 0.9992. The inter-day precision was 3.1%-3.8% and accuracy was 98.9%-103.5%. The intra-day precision was 2.4%-6.8% and the accuracy was 97.6%- 104.9%. The extraction recovery ranged from 99.23%-103.84% and the matrix effect was not significant. Perampanel was proved to be stable
in solution and human plasma under different tested conditions. The validated method was successfully applied to a randomized, open-label, 2- period, crossover bioequivalence study in healthy Chinese subjects, and the results indicated that bioequivalence was achieved for 2 formulations of
the 4-mg perampanel tablet under both fasting and fed conditions, and both treatments were safe and well-tolerated by all study subjects. Conclusion: The validated method was successfully applied to a bioequivalence study of perampanel in human plasma and has achieved satisfactory results.
研究领域:
药理学
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分析化学
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临床医学
✓ 已验证
DOI
高影响因子
JOURNAL OF PHARMACOLOGICAL AND TOXICOLOGICAL METHODS
·
2025
·
IF 1.8
Jinxingyi Wang,Ruyu Tao,Hanshuai Hu,Xue Lan,Jiejie Gao,Yanping Guan,Qian Liu
Background Busulfan and cyclophosphamide (Bu-Cy) is a widely used conditioning regimen for hematopoietic stem cell transplantation (HSCT) in the treatment of hematologic malignancies. To explore the exposure-efficiency relationships of Bu-Cy regimen and evaluate the necessity of relative therapeutic drug monitoring (TDM), we developed a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to simultaneously quantify the busulfan and cyclophosphamide in human plasma. Methods A simple LC-MS/MS bioassay for simultaneous determination of busulfan and cyclophosphamide using isotope dilution internal standardization has been established. Plasma samples were subjected to protein precipitation prior to their injection into a column for subsequent separation (Thermo Accucore aQ C 18 , 50 × 2.1 mm, 2.6 μm). Positive electrospray ionization (ESI) mode with selected reaction monitoring (SRM) was used for analytes determination. Results Busulfan and cyclophosphamide could be measured within 3 min, with the calibration ranges of 80–4000 ng/mL for busulfan and 25–2000 ng/mL for cyclophosphamide. The validated method showed good sensitivity and linearity. Accuracies and precisions were less than 15 %. The results of stability showed that busulfan and cyclophosphamide were stable in the plasma under room temperature for 16 h, 4 °C for 24 h, −80 °C for 2 weeks, and after three freeze-thaw processes. Conclusion The bioassay was simple, sensitive and successfully implemented in the realm of TDM for Bu-Cy, ultimately leading to improved dosing precision.
研究领域:
药理学
·
临床化学
·
肿瘤学
·
分析化学
·
血液学
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产品关联
DOI
PubMed
高影响因子
MOLECULES
·
2023
·Vol. 28
·期 5
·2377
·
IF 4.6
Zili Guo,Bianbian Gao,Miaoliang Fan,Lisha Chen,Changjun Zhang,Xianrui Liang,Weike Su,Yuanyuan Xie
XYY-CP1106, a candidate compound synthesized from a hybrid of hydroxypyridinone and coumarin, has been shown to be remarkably effective in treating Alzheimer’s disease. A simple, rapid and accurate high-performance liquid chromatography coupled with the triple quadrupole mass spectrometer (LC-MS/MS) method was established in this study to elucidate the pharmacokinetics of XYY-CP1106 after oral and intravenous administration in rats. XYY-CP1106 was shown to be rapidly absorbed into the blood (Tmax, 0.57–0.93 h) and then eliminated slowly (T1/2, 8.26–10.06 h). Oral bioavailability of XYY-CP1106 was (10.70 ± 1.72)%. XYY-CP1106 could pass through the blood–brain barrier with a high content of (500.52 ± 260.12) ng/g at 2 h in brain tissue. The excretion results showed that XYY-CP1106 was mainly excreted through feces, with an average total excretion rate of (31.14 ± 0.05)% in 72 h. In conclusion, the absorption, distribution and excretion of XYY-CP1106 in rats provided a theoretical basis for subsequent preclinical studies.Keywords:XYY-CP1106;Alzheimer’s disease;LC-MS/MS;pharmacokinetics;tissue distribution;excretion study
研究领域:
药理学
·
神经科学
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产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2023
·
IF 4.8
Jiayi Sun,Jinna Dai,Xingqi Wang,Hong Shang
The objective of this study is to develop a quick and precise chiral liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) technology that operates in reversed phase mode. Following oral administration of 5.0 mg/kg rac -pranoprofen, the suggested approach was completely validated and successfully used to the stereoselective detection of pranoprofen enantiomers in rat plasma for the first time. Both the polysaccharide derivatized chiral stationary phase and a homemade β-cyclodextrin (β-CD) derivatized based chiral column were assessed. The latter one, a per-4-chlorophenylcarbamate-β-cyclodextrin bonded chiral stationary phase (CPCDP) made in our laboratory, allowed for the highly sensitive detection, relatively short retention time and complete separation (resolution 2.0) of the pranoprofen enantiomers. A solid phase extraction (SPE) procedure on C 18 cartridge was optimized for the extraction of S -(+)-, R -(−)-pranoprofen and internal standard ( S -(+)-ketoprofen, IS) from rat plasma in detail. Acetonitrile with 0.1 % formic acid in aqueous phase (60:40, v:v ) at a flow rate of 0.6 mL/min was the ideal mobile phase condition. The outcome of pharmacokinetic study showed that the values of maximum plasma concentration (C max ) and the area under plasma drug concentration–time curve to infinity (AUC 0-∞ ) for S -(+)-pranoprofen were 1.79 and 1.90 times greater than R -(−)-isomer, respectively. Altogether, this work is the first to examine the stereospecific pharmacokinetics of pranoprofen enantiomers in vivo , whose data provided potential possibility for the development of pure isomer with superior pharmacological activity and safety to replace racemic application in the clinic.
研究领域:
药物分析
·
药理学
·
分析化学
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产品关联
DOI
高影响因子
XENOBIOTICA
·
2020
·
IF 1.902
Luyu Bai,Qingsong Fei,Fang Lei,Rui Luo,Qun Ma,Manman Dai,Huimin Zhang,Ning He
The objective of this study was to compare the pharmacokinetics of vancomycin hydrochloride administered into rabbits through different routes and explore the feasibility of peptide drugs entering the systemic circulation through ocular administration.A convenient, accurate, and rapid liquid chromatography-trandem mass spectrometric (LC-MS/MS) method was established and used for the determination of vancomycin hydrochloride in rabbit plasma after intravenous administration (1.5 mg/kg), intragastric, and ocular administration (15 mg/kg). The pharmacokinetic parameters were analyzed using the DAS 2.0 software.We obtained a linear calibration curves vancomycin hydrochloride in plasma of rabbits over a concentration range of 0.05–10.0 μg/mL (R2 > 0.9995), the interassay accuracy was within 5%, precision of 1.66–3.38%, and recovery of >85%. No matrix effects were observed. The absolute bioavailability of vancomycin hydrochloride after intragastric and ocular administration was 1.0 and 7.3%, with the half-life values of 63.1 and 138.5 min, respectively.Therefore, the LC-MS/MS method established in this experiment was suitable for the determination of vancomycin hydrochloride. Vancomycin hydrochloride was rapidly absorbed into the blood circulation after ocular administration. Ocular administration was linked to higher bioavailability compared with intragastric administration, suggesting that the former will become a route for the delivery of peptide drugs.
研究领域:
药理学
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分析化学
·
药物代谢
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DOI
PubMed
高影响因子
Forensic Toxicology
·
2018
·Vol. 37
·期 1
·121-131
·
IF 3.924
Chen Lizhu,Yu Yingjia,Wang Yang,Xiang Ping,Duan Gengli
Purpose It is crucial for forensic analysis to differentiate clinical use from illegal abuse. Selegiline (SG) is mainly metabolized to desmethylselegiline (DM-SG), R -(−)-methamphetamine (R-MA) and R-(−)amphetamine (R-AM); while abused methamphetamine and amphetamine mainly contain the S -(+)-form. The aim of this study was to simultaneously determine SG, DM-SG, R / S -MA, and R / S -AM in human oral fluid (OF) and to differentiate clinical use from illegal use. We also aim to apply the present method to the OF samples from authentic cases in forensic toxicology. Methods Liquid–liquid extraction and liquid chromatography-tandem mass spectrometry operating in positive ion multiple-reaction monitoring mode were utilized. The chromatographic system consisted of a Chirobiotic TM V2 column (2.1 mm × 250 mm, 5 μm) and a mobile phase of methanol containing 0.1% (v/v) glacial acetic acid and 0.02% (v/v) ammonium hydroxide. Results and conclusions The calibration curves were linear from 1 to 100 ng/mL, and r > 0.995 for all analytes with imprecisions ≤ 15% and accuracy between 85 and 115%. Extraction recoveries ranged from 46.3 to 104.7% with coefficient of variation (CV) ≤ 10.3% and matrix effects (MEs) ranged from 47.4 to 114.8% with CV ≤ 12.9%. The lower limit of quantification was 0.2 ng/mL for SG and DM-SG and 1.0 ng/mL for S-MA, R-MA, S-AM and R-AM. The present method is simple, rapid (accomplished in 12 min), sensitive, and validated by authentic samples.
研究领域:
法医学
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分析化学
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产品关联
DOI
高影响因子
MOLECULES
·
2025
·Vol. 30
·期 18
·3797
·
IF 4.6
Bin Lin,Fen Wang,Hongliang Wang,Xinsheng Huang,Xueqin Liu,Xuechun Wang,Chihua Wang,Yan Xing,Chunqing Dai,Yi Zheng
Theophylline represents a significant public health challenge due to its dual acute and chronic toxicity resulting from therapeutic, environmental, and dietary exposures. Effective monitoring across the bio-environmental–food triad requires analytical methods that are highly sensitive, universally applicable, and capable of overcoming complex matrix interferences. This study introduces a flat membrane-based liquid-phase microextraction (LPME) technique combined with LC–MS/MS for the determination of theophylline in diverse matrices. The method eliminates the need for specialized adsorbents or equipment, offering a simple and cost-effective solution for high-throughput sample clean-up. Under optimized conditions, the method demonstrated exceptional sensitivity (LOD: 0.2 ng mL−1) and a wide linear range (0.01–10 μg mL−1). It was successfully applied to plasma, urine, hospital sewage, and green tea, providing accurate (recoveries of 86.7–111.3%) and reproducible (RSD < 10%) results across all matrices. This unified and robust approach effectively addresses matrix interferences and provides a reliable tool for the monitoring and risk assessment of theophylline across multiple domains.
研究领域:
药物代谢
·
分析化学
·
环境毒理学
·
临床药理学
·
食品安全
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生物监测
·
色谱质谱技术
✓ 已验证
产品关联
DOI
PubMed
高影响因子
LWT-FOOD SCIENCE AND TECHNOLOGY
·
2025
·
IF 6.6
Mingzheng Duan,Ting Jiang,Xi Wang,Kangjian Song,Xu Xiao,Xiaoting Fu,Sijiu He,Jieming Feng,Muhammad Junaid Rao,Hengcui Guo
Strawberries ( Fragaria × ananassa ) are prized for bioactive flavonoids and anthocyanins, contributing to antioxidant capacity and health benefits. However, decades of breeding for yield and shelf-life have eroded their phytochemical diversity. To explore this trade-off, we compared wild strawberries ( Fragaria nilgerrensis , HM) with three cultivated varieties (pink-FY, red-RF, white-DX) using integrated LC-MS/MS metabolomics and transcriptomics. Wild HM strawberries contained twice the vitamin C (134.2 mg/100g), 2.5× more total flavonoids (138.7 mg/100g), and higher antioxidant activity (367 μg Trolox/g) than commercial varieties. In contrast, red-fruited RF showed abundant anthocyanins (pelargonidin-3-glucoside 6.6% abundance), while the wild HM genotype accumulated higher levels of flavonoids, with neohesperidin, lonicerin, hyperin and ternatumoside II collectively representing 20.9% of total flavonoids - concentrations 3-169 times greater than those observed in the three commercial varieties (FY, RF, DX). Transcriptomic analysis (RNA-seq, Illumina HiSeq 2500) revealed distinct MYB transcription factor associations: FxaYL_611g0111200 (MYB66) showed strong positive correlation with anthocyanin biosynthesis in RF (r=0.92, **p<0.005 ), while FxaYL_242g0472670 (MYB44-like) was significantly associated with HM's unique antioxidant flavonoid profile (r=0.96, ***p<0.0001 ). These regulatory relationships were corroborated by hierarchical clustering demonstrating varietal-specific expression patterns and principal component analysis (82.6% variance explained), collectively providing molecular targets for enhancing nutritional quality in strawberry breeding programs.
研究领域:
植物科学
·
食品化学
·
分子生物学
·
营养学
·
代谢组学
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产品关联
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2019
·
IF 2.983
Jing Nie,Peter Yaro,Kaifeng He,Su Zeng
Triticonazole with an asymmetrical carbon atom has two enantiomers and is a broad-spectrum systemic fungicide, but its disposition in animals is unclear. In this study, a chiral analytical method of LC–MS/MS was developed and validated for the assay of triticonazole enantiomers in rat plasma and tissues. There were no endogenous interferences in the blank plasma and tissues of rats. R -(−)- and S -(+)-triticonazole peaks were separated entirely. The calibration curves were linear from 25 to 2500 ng/mL of each enantiomer. The accuracy, precision, and stability met the requirements of bioanalysis. Therefore, this method is enantioselective, accurate, precise, sensitive and reliable, and has been successfully applied to analyze R -(−)- and S -(+)-triticonazole in rat plasma and to study the toxicokinetics of triticonazole enantiomers in rats. After single oral administration of 50 mg/kg racemate triticonazole to rats, the AUC (0-∞) and C max of R -(−)-triticonazole were 3.5 and 3.6 times higher than that of S -(+)-triticonazole, respectively. The content of S- (+)-triticonazole was higher in the kidney whilst R- (−)-triticonazole was higher in the brain and small intestine. The results showed that the toxicokinetics and tissues distribution of triticonazole enantiomers in rats have stereoselective differences.
研究领域:
分析化学
·
毒理学
·
药代动力学
✓ 已验证
DOI
高影响因子
CHEMISTRY & BIODIVERSITY
·
2022
·Vol. 20
·期 1
·e202200574
·
IF 2.745
Haixia Han,Rui Ma,Aidi Xie,Juanjuan Gao,Zhen Wang,Yi Zhao,Huanming Pang,Wei Zhang
Eleven polyphenols, classified as flavonoid glycosides, flavonoid aglycones, and phenolic acids, are important bioactive components in the capitula of Coreopsis tinctoria (CCT). Nevertheless, their full pharmacokinetic profiles have not been demonstrated simultaneously. Therefore, a liquid chromatography – tandem mass spectrometry (LC/MS/MS) method was developed in the present work and used it to study the pharmacokinetics of these 11 compounds. We performed LC/MS/MS with a gradient mobile phase composed of water containing 0.1 % formic acid and acetonitrile containing 0.1 % formic acid on a Proshell 120 SB C18 column (2.1 mm×100 mm, 2.7 μm). We achieved a good chromatographic peak shape, resolution, and mass signal response, and multiple reaction monitoring facilitated the simultaneous detection of 11 analytes. In addition, we validated the selectivity, correlation coefficient, precision, extraction recovery, matrix effects, and stability of the LC/MS/MS method to be acceptable for 11 analytes in rat plasma. Subsequently, rats were orally administered with 50 % ethanol eluent of CCT (ECCT). Nine of 11 polyphenols were absorbed quickly (except for QCD and TCA), and their plasma levels peaked within 40 min. The exposure and C max values of flavonoid glycosides and phenolic acids were lower than those of flavonoid aglycones. This is the first report to demonstrate the pharmacokinetics of 11 polyphenols in ECCT, which may play an important role in future studies of the bioactive components of ECCT and their bioactive mechanisms. Graphical
研究领域:
药理学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）