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
·
分析化学
·
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
Analytical Methods
·
2025
·
IF 2.6
Aiwen Shi,Bin Qi,Xiaolei Tang,Li Liu,Chang Wang,Ziyi Jia
Frankincense is a resin drug widely used in the medical field. Comprehensive qualitative and quantitative analysis of the differences in the chemical composition of frankincense, stir fried frankincense and vinegar frankincense by combined GC-MS and LC-MS chromatographic methods. In GC-MS analysis, six chemical compositions with high content in frankincense were selected, including β-ocimene、1-octanol、acetic acid, octyl ester、nerolidol、lauric acid and incensole acetate. In the LC-MS analysis, eight more widely studied chemical compositions were selected, including 11-keto-β-boswellic acid、β-elemolic acid、acetyl-11-keto-β-boswellic acid、β-elemonic acid、α-boswellic acid、β-boswellic acid、3-0-acetyl-α-boswellic acid、3-0-acetyl-β-boswellic acid. In addition, some chemical composition of frankincense were identified by LC-MS fragmentation information.
研究领域:
中药学
·
分析化学
✓ 已验证
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
✓ 已验证
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
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生物分析
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICAL BIOCHEMISTRY
·
2024
·
IF 2.6
Cheng Li,Qinghui Chen,Jinqiao Rong,Houde He,Yu Lu,Yuxia Liu,Zhongfu Wang
As the main active glycoprotein of egg white, the biological functions of chicken ovomucin α- and β-subunit are closely related to the structure of glycans. However, the exact composition and structure of the subunit glycans are still unknown. We obtained highly pure chicken ovomucin α-subunit and β-subunit protein bands by the strategy combined with two-step isoelectric precipitation and SDS-PAGE gel electrophoresis. The ammonia-catalyzed one-pot procedure was then used to release and capture α-and β-subunit protein glycans with 1-phenyl- 3-Methyl-5-pyrazolone (PMP). The N / O -glycans of bis-PMP derivatives were purified and analyzed by LC-MS. More importantly, an effective dual modification was performed to accurately quantify neutral and sialylated O -glycans through methylamidation of sialic acid residues and simultaneously through carbonyl condensation reactions of reducing ends with PMP. We first showed that the α-subunit protein has only N -glycosylation modification, and the β-subunit only O -glycosylation, a total of 22 N -glycans and 20 O -glycans were identified in the α- and β-subunit, respectively. In addition, the complex N -glycan (47 %) and the sialylated O -glycan (77 %) are each major types of the above subunits. Such findings in this study provide a basis for studying the functional and biological activities of chicken ovomucin glycans.
研究领域:
生物化学
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糖生物学
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蛋白质组学
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产品关联
DOI
PubMed
高影响因子
Chinese Medicine
·
2020
·Vol. 15
·期 1
·1-13
·
IF 2.96
Yang Yi-Yao,Wu Zhao-Yu,Zhang Hao,Yin Shi-Jun,Xia Fang-Bo,Zhang Qian,Wan Jian-Bo,Gao Jian-Li,Yang Feng-Qing
Background The dry root and rhizome of Salvia miltiorrhiza Bunge, or Danshen, is a well-known traditional Chinese medicine with anticoagulant activity. Taking into account that thrombin (THR) and factor Xa (FXa) play crucial roles in the coagulation cascade, it is reasonable and meaningful to screening THR and/or FXa inhibitors from Danshen. Methods Four extracts [butanol (BA), ethyl acetate (EA) and remained extract (RE) from 75% ethanol extract, and water extract (WE)] of Danshen were prepared, and their THR/FXa inhibitory activities were assessed in vitro. Then, the active EA extract was further separated by silica-gel column chromatography (SC), and its fractions (SC1–SC5) were analyzed by LC–MS. The principal component analysis (PCA) and orthogonal partial least squares discriminate analysis (OPLS-DA) were employed for predicting the specific marker compounds. The chemical structures of targeted compounds were identified by LC–MS/MS and their interactions with THR/FXa were analyzed by the molecular docking analysis. Results Danshen EA extract showed strong activity against THR and FXa, and its fractions (SC1–SC5) exhibited obvious difference in inhibitory activity against these two enzymes. Furthermore, four marker compounds with potential THR/FXa inhibitory activity were screened by PCA and OPLS-DA, and were identified as cryptotanshinone, tanshinone I, dihydrotanshinone I and tanshinone IIA. The molecular docking study showed that all these four tanshinones can interact with some key amino acid residues of the THR/FXa active cavities, such as HIS57 and SER195, which were considered to be promising candidates targeting THR and/or FXa with low binding energy (< − 7 kcal mol −1 ). Conclusions LC–MS combined with multivariate statistical analysis can effectively screen potential THR/FXa inhibitory components in Danshen.
研究领域:
中药学
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生物化学
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分子生物学
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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
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
·
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
✓ 已验证
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
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MOLECULES
·
2024
·Vol. 29
·期 11
·2513
·
IF 4.2
Luyi Xie,Lihong Zhou,Rongrong Zhang,Hang Zhou,Yi Yang
Aspergillus cristatusis a crucial edible fungus used in tea fermentation. In the industrial fermentation process, the fungus experiences a low to high osmotic pressure environment. To explore the law of material metabolism changes during osmotic pressure changes, NaCl was used here to construct different osmotic pressure environments. Liquid chromatography–mass spectrometry (LC–MS) combined with multivariate analysis was performed to analyze the distribution and composition ofA. cristatusunder different salt concentrations. At the same time, the in vitro antioxidant activity was evaluated. The LC–MS metabolomics analysis revealed significant differences between threeA. cristatusmycelium samples grown on media with and without NaCl concentrations of 8% and 18%. The contents of gibberellin A3, A124, and prostaglandin A2 related to mycelial growth and those of arabitol and fructose-1,6-diphosphate related to osmotic pressure regulation were significantly reduced at high NaCl concentrations. The biosynthesis of energy-related pantothenol and pantothenic acid and antagonism-related fluvastatin, aflatoxin, and alternariol significantly increased at high NaCl concentrations. Several antioxidant capacities ofA. cristatusmycelia were directly related to osmotic pressure and exhibited a significant downward trend with an increase in environmental osmotic pressure. The aforementioned results indicate thatA. cristatusadapts to changes in salt concentration by adjusting their metabolite synthesis. At the same time, a unique set of strategies was developed to cope with high salt stress, including growth restriction, osmotic pressure balance, oxidative stress response, antioxidant defense, and survival competition.
研究领域:
真菌生物学
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代谢组学
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食品科学
·
生物技术
✓ 已验证
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）