Chinese Journal of Natural Medicines
·
2016
·
IF 1.382
Feng ZHANG,Liang SUN,Shou-Hong GAO,Wan-Sheng CHEN,Yi-Feng CHAI
Tanreqing injection (TRQ), a well-known traditional Chinese medicine formula, is commonly used to treat respiratory diseases. In the present study, a rapid, selective, and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated to simultaneously determinate the plasma contents of 5 major constituents of TRQ, including chlorogenic acid (CHA), caffeic acid (CFA), baicalin (BA), ursodeoxycholic acid (UDCA) and chenodeoxycholic acid (CDCA) in rats after intravenous administration of TRQ. Chromatographic separation was performed on an Agilent Zorbax SB-C 18 column (3.5 μm, 100 mm × 2.1 mm), with acetonitrile and 0.1% aqueous formic acid as mobile phase at a flow rate of 0.3 mL·min −1 . The calibration curves were linear over the ranges of 27.0–13 333.0 ng·mL −1 for CFA, 30.0–14 933.0 ng·mL −1 for CHA, 50.0–50 333.0 ng·mL −1 for BA, 550.0–55 000.0 ng·mL −1 for UDCA, and 480.0–48 000.0 ng·mL −1 for CDCA, respectively. Intra- and inter-day precisions (relative standard deviations, RSDs) were from 3.11% to 14.08%. The extraction recoveries were greater than 71% and accuracy (relative recovery) was from 89% to 137% for all analytes, except endogenous bile acids. This validated method was successfully applied to the first pharmacokinetic study of CFA, CHA, BA, UDCA and CDCA in rat plasma after intravenous administration of TRQ.
研究领域:
中药学
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分析化学
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药理学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2022
·
IF 3.318
Hao Wang,Xi Zhang,Yingfei Peng,Baishen Pan,Beili Wang,David Haixiang Peng,Wei Guo
Monosaccharides are important players in cell metabolism and potential biomarkers. An effective tool to quantify monosaccharides is required in basic research and healthcare. In this study, we developed a liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay that could simultaneously quantify 14 free monosaccharides and evaluated its performance according to clinical guidance. The LC-MS/MS step separated and quantified 14 monosaccharides with 6 min. The coefficient of variation at the lower limit of quantification was less than 20% for each analyte. The R square values from linear regression analyses were all greater than 0.995. The validated assay was employed to profile free monosaccharides in conditioned media from cell culture and patient sera from glucose tolerance test. Both LO2 cells and HEK293 cells consumed D-glucosamine, D-glucose and produced D-glucuronic acid, N-acetyl-D-glucosamine. Additionally, LO2 cells produced D-mannose and L-fucose, whereas HEK293 cells consumed D-mannose. In patient sera from glucose tolerance test, the level of D-glucose increased significantly after glucose intake, but the levels of other monosaccharides didn’t. In conclusion, the LC-MS/MS assay we developed for 14-monosaccharide profiling met clinical requirements. The monosaccharide profiling results showed the distinct monosaccharide metabolism between liver and kidney cells, and the ignorable diet effect on 6 serum monosaccharides.
研究领域:
分析化学
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代谢组学
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临床医学
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产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2024
·
IF 8.5
Fenglan Zhou,Chunjie Zhou,Wenhua Zhang,Zsolt Zalán,Hui Shi,Jianquan Kan,Kewei Chen,Tian Cai
The detection of mycotoxins in Sichuan peppers is crucial for ensuring food safety. Hence, an efficient detection approach based on the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method followed by LC–MS/MS (liquid chromatography–tandem mass spectrometry) was established for the analysis of various mycotoxins in dried red and green Sichuan peppers. Samples were extracted with a solution containing 99 % acetonitrile and 1 % formic acid. A new adsorbent, namely, ENVI-Carb, and primary secondary amines were used as purifying agents. The proposed method demonstrated good linearity (R 2 ≥ 0.999), satisfactory recovery (77.3 %–109.2 %), and good repeatability (intraday and interday relative standard deviations ≤9.7 %) in dried red and green Sichuan peppers. Its limits of detection in red and green Sichuan peppers were 0.2–0.6 and 0.1–0.7 μg/kg, respectively. The established method can effectively eliminate complex matrix interference and provides an effective approach for the high-throughput detection of mycotoxins in various complex food matrices.
研究领域:
食品科学
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分析化学
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产品关联
DOI
PubMed
高影响因子
Bioanalysis
·
2024
·
IF 1.9
Tianyi Wang,Yalian Zhang,Luan Jia,Ying Li,Lu Wang,Yanru Zhu,Yuxin Jiang,Furong Zhao,Shuang Wang,Dan Song
Aim: Branched-chain amino acids (BCAAs) and aromatic amino acids (AAAs) were suggested as potential biomarkers in liver disease. This study aimed to develop and validate a simple and rapid LC-MS/MS method to simultaneously measure serum BCAAs and AAAs levels in patients with liver injury, and further establish reference intervals of Chinese healthy adult populations.Patients & methods: Samples were prepared by a one-step protein precipitation and analysis time was 4 min per run.Results: The validation results showed good linearity (r2 >0.9969), satisfactory accuracy (94.44% – 107.75%) and precision (0.10% – 5.90%).Conclusion: This method proved to be suitable for high-throughput routine clinical use and could be a valuable adjunct diagnosis tool for liver injury and other clinical applications.
研究领域:
临床医学
·
生物分析
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2022
·
IF 3.318
Hua Li,Yang Wang,Ru Ding,Chen Chen,Zhixuan Tian,Hongnan Yin,Lieming Ding
A sensitive and reliable method was developed to determine befotertinib (D-0316) and its metabolite D-0865 from human plasma by LC-MS/MS. The samples were prepared by simple protein precipitation and 2 µL of the supernatant were chromatographed on a C18 analytical column (ACE Excel 2 Super C 18 , 50 × 2.1 mm). Elution was performed with mobile phase A (10 mM ammonium acetate in water containing 1 % formic acid) and mobile phase B (acetonitrile containing 1 % formic acid) under a gradient program in a total run time of 4 min. Triple Quadruple 5500 equipped with Turbo Ion Spray source and multiple reaction monitoring (MRM) were used for the analysis detection. The transitions were m / z 568.3 → 72.1 m / z (befotertinib), m / z 554.2 → 497.2 (D-0865), and m / z 455.2 → 164.9 (verapamil, internal standard). According to the Chinese Pharmacopeia Commission and ICH Harmonised Guideline for Bioanalytical Method Validation, this method was validated within the spectrum of its accuracy, precision, selectivity, linearity, recovery, matrix effect, and stability. This LC-MS/MS method was successfully applied for the quantitation of befotertinib and its metabolite D-0865 in human plasma during the pharmacokinetics study of befotertinib in non-small cell lung cancer (NSCLC) patients.
研究领域:
药物分析
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临床药理学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2017
·
IF 3.255
Yang Yang,Ying Lian,Ping Zhong,Dandan Wang,Bin Di,Bo Li
Ten related substances in coenzyme A (CoA) were detected using a newly developed gradient reverse phase high performance liquid chromatographic (HPLC) method. A highly specific and efficient LC–MS/MS method was developed to characterize process-related substances and the major degradation products, and three unknown related substances were further synthesized and characterized by H-NMR and C-NMR spectroscopy. Synthesized samples of the related substances were used for quantitative analysis by HPLC. The method was validated according to ICH guidelines with respect to specificity, precision, accuracy and linearity. The forced degradation studies included acidic, alkaline, oxidative, photolytic and thermal stress conditions. Furthermore, we depicted and speculated the probable mechanism of formation of related substances and the plausible fragmentation mechanism showed that all the related substances came from the manufacturing process. Characterization, synthesis and quantitative analysis of related substances were discussed in detail, and were critical for quality control, manufacturing process optimization and CoA monitoring, all of which were important to ensure the security of CoA.
研究领域:
药物分析
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生物化学
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制药工程
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2019
·
IF 2.983
Qingqing Yang,Jing Sun,Chuan Li,Haizhi Zhang,Weiren Xu,Changxiao Liu,Xuemin Zheng
Specific study about the effect of cytochrome P450 2D6 (CYP2D6) polymorphisms on the metabolism of clinic drugs is of great significance for drug safety investigation. Here, the interaction between CYP2D6 variants (*1, *2, *10, *39) and metoprolol (MET) was intensively researched in vitro from the aspect of drug-enzyme kinetic study. To obtain quantitative data, α -hydroxymetoprolol (main metabolite of MET) was selected as an ideal analyte and an LC–MS/MS method was adopted for sample determination. Firstly, by selecting suitable internal standard and optimizing separation condition, the LC–MS/MS method was established and validated. Then, the drug-enzyme incubation system was optimized by two parameters: incubation time and amount of enzyme. Lastly, the interaction between CYP2D6 allelic variants and MET was characterized by K m , V max and CL int . As a result, four CYP2D6 enzymes displayed diverse K m or V max towards MET and the values of CL int showed a wide range from 8.91 to 100%. Relative to CYP2D6*1 (CL int *1 = 100%), CYP2D6*2 demonstrated the second high catalytic activity (CL int *2/*1 = 74.87%) while CYP2D6*39 (CL int *39/*1 = 29.65%) and CYP2D6*10 (CL int *10/*1 = 8.91%) showed minimal catalytic activity. This comprehensive in vitro data suggested the prominent influence of CYP2D6 polymorphisms on the metabolism of MET, which could offer valuable information for personalized administration of MET in clinic.
研究领域:
药理学
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临床医学
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生物化学
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产品关联
DOI
PubMed
高影响因子
Bioanalysis
·
2025
·
IF 1.8
Yujie Li,Shu Zhang,Xiayi Wang,Xiaochuan Li,Lizhong Guo
Background Background: An oligonucleotide drug named nusinersen sodium is used to treat Spinal Muscular Atrophy (SMA), requires accurate detection for therapeutic research. There are no published reports on liquid chromatography-tandem mass spectrometry (LC-MS/MS) methods for detecting nusinersen in rat cerebrospinal fluid (CSF).Methods An LC-MS/MS method has been created and verified to detect nusinersen in Sprague-Dawley (SD) rat CSF. The method employed solid-phase extraction for post-extraction analysis and used dT20 as an internal standard. Negative ion multiple reaction monitoring (MRM) mode scanning and the electrospray ionization (ESI) source were used. The method was validated over a concentration range of 5–2000 ng/mL with a Lower Limit of Quantification (LLOQ) of for nusinersen at 5 ng/mL.Results and conclusions The method achieves extremely high accuracy and precision, good linearity, high extraction recovery, and provides a useful approach for evaluating the pharmacokinetics of nusinersen in rats.
研究领域:
分析化学
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药代动力学
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神经药理学
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质谱分析
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产品关联
DOI
PubMed
高影响因子
Scientific Reports
·
2016
·Vol. 6
·期 1
·1-12
·
IF 5.228
Chen Ang,Zhou Xiaojing,Tang Shuowen,Liu Mingyao,Wang Xin
Plumbagin (5-hydroxy-2-methyl-1,4-naphthoquinone), a natural naphthoquinone compound isolated from roots of Plumbago zeylanica L., has drawn a lot of attention for its plenty of pharmacological properties including antidiabetes and anti-cancer. The aim of this study was to investigate the effects of plumbagin on CYP1A2, CYP2B1/6, CYP2C9/11, CYP2D1/6, CYP2E1 and CYP3A2/4 activities in human and rat liver and evaluate the potential herb-drug interactions using the cocktail approach. All CYP substrates and their metabolites were analyzed using high-performance liquid chromatography–tandem mass spectrometry (LC-MS/MS). Plumbagin presented non-time-dependent inhibition of CYP activities in both human and rat liver. In humans, plumbagin was not only a mixed inhibitor of CYP2B6, CYP2C9, CYP2D6, CYP2E1 and CYP3A4, but also a non-competitive inhibitor of CYP1A2, with K i values no more than 2.16 μM. In rats, the mixed inhibition of CYP1A2 and CYP2D1, and competitive inhibition for CYP2B1, CYP2C11 and CYP2E1 with K i values less than 9.93 μM were observed. In general, the relatively low K i values of plumbagin in humans would have a high potential to cause the toxicity and drug interactions involving CYP enzymes.
研究领域:
药理学
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分析化学
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毒理学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2023
·
IF 3.4
Huanhuan Yang,Cong Liu,Chuanhong Zhu,Yan Zheng,Juan Li,Qianyun Zhu,Hao Wang,Xiangming Fang,Quan Liu,Man Liang,Zilong Liu
Determination of antipsychotics from biological samples is meaningful in the field of clinical and forensic medicine. Compared to blood, keratinized matrices such as hair and nails have attracted increasing attention in drug analysis for wider detection window. Nevertheless, the distribution and stability of antipsychotics in keratinized matrices are not clarified yet. Therefore, we developed a LC-MS/MS based method for simultaneous determination of 10 antipsychotics from blood, hair and nails, with high recovery (78.1–107.4%, 71.3–93.5% and 75.2–90.5%), low LOD (5–10 pg/mL, 5–10 pg/mg and 5 pg/mg) and high accuracy (96.0%−101.6%, 97.5%−102.5% and 97.6–101.7%). The method was applied to sets of blood, hair, and nail samples of 54 patients who received long-term therapy, and significant correlations between drug concentrations in blood and hair was found, while the correlation between nails and other matrices varied depending on the drug. Except for olanzapine , the concentrations of antipsychotics in segmental hair samples were consistent with drug exposure. Besides, the hair and nail samples of suspects in two forensic cases were analyzed and provided supporting evidence for the suspects’ psychiatric state. Our research offered a deeper understanding of keratinized matrix as stable and retrospective bio-samples for antipsychotics detection in forensic practice.
研究领域:
临床医学
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法医学
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产品关联
DOI
PubMed
高影响因子
ANALYTICAL BIOCHEMISTRY
·
2024
·
IF 2.6
Lingfang Dong,Kun Li,Shan Gao,Wenyi Wang,Yinghua Feng,Jingying Zhang,Jie Yang,Weifeng Dong,Wei Zhang
we developed an effective protein precipitation method for determination of levamlodipine in human plasma using LC–MS/MS. Sample extraction was carried out by using liquid–liquid extraction in 96-well plate format. (S)-Amlodipine-d4 was used as internal standard (IS). The chromatographic separation was achieved using Philomen Chiral MX (2) column (3 μm, 2.1 × 100 mm). Mobile phase A was comprised of Acetonitrile (ACN), Mono ethanol amine (MEA) and Iso-Propyl alcohol (IPA) (1000:1:10, v/v/v), Mobile phase B was IPA-ACN (2:1, v/v). The flow rate was 0.4 mL/min. The total run time of each sample was 4.0 min with gradient elution. LC-MS/MS spectra were generated in positive ion mode, and multiple reaction monitoring (MRM) was used to detect the following transitions: m/z 409.20 → 238.15 for levamlodipine and 415.25 → 240.20 for (S)-Amlodipine-d4 (the IS). The method was linear from 50 to 10000 pg/mL（R 2 ＝0.9988489）,and the lower limit of quantification (LLOQ) was 50 pg/mL. This method was applied to a bioequivalence study of levamlodipine.
研究领域:
药物分析
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临床药理学
✓ 已验证
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2025
·
IF 3.1
Minlu Cheng,Xianjing Li,Ya Li,Yiya Wang,Wenjia Li,Shuai Wang,Chang Shu,Qinxin Song,Li Ding
Recently, the approval of Trop-2 targeted antibody drug conjugate (ADC) has changed the dilemma of patients with advanced triple-negative breast cancer who rely on chemotherapeutics to improve their survival. FDA018, an ADC consisting of an anti-Trop-2 antibody conjugated with a topoisomerase inhibitor SN-38 via an acid-cleavable linker, is currently being investigated in clinical trials. Based on the urgent demand to evaluate the clinical pharmacokinetics of FDA018, ligand binding assays (LBAs) for the determination of SN-38-conjugated antibody and total antibody and LC-MS/MS methods for the determination of the free SN-38, its metabolite SN-38G and total SN-38 were developed. The comparability and DAR sensitivity evaluation of the ELISA strategies for SN-38-conjugated antibody and total antibody were emphasized. The sensitivity of the LC-MS/MS method for the simultaneous determination of SN-38 and SN-38G reached 0.500 ng/mL and 0.250 ng/mL, respectively. An effective solution has been proposed for the optical instability of the cleavable linker of FDA018 during the pretreatment process of biological samples. The established bioanalytical methods were comprehensively validated and the results satisfied the acceptable criteria of ICH M10. The validated bioanalytical methods have been applied to the single-dose pharmacokinetic study of FDA018 in patients with Trop-2-positive malignant tumors successfully, and the pharmacokinetic profiles of FDA018 and its constituent components were investigated.
研究领域:
肿瘤学
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药物分析
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临床药理学
✓ 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）