| 引用本文: | 王猛猛,俞蕴莉,屈昱晨,华雯妍,王吉,张全英.LC-MS/MS测定大鼠血清中15种胆汁酸成分[J].中国现代应用药学,2020,37(9):1030-1034. |
| WANG Mengmeng,YU Yunli,QU Yuchen,HUA Wenyan,WANG Ji,ZHANG Quanying.Determination of Fifteen Bile Acids Concentration in Rats' Serum by LC-MS/MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2020,37(9):1030-1034. |
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| LC-MS/MS测定大鼠血清中15种胆汁酸成分 |
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王猛猛1, 俞蕴莉1, 屈昱晨2, 华雯妍1, 王吉3, 张全英1
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1.苏州大学附属第二医院, 药物临床试验机构, 江苏 苏州 215004;2.苏州大学药学院, 江苏 苏州 215123;3.苏州大学附属第二医院, 肿瘤科, 江苏 苏州 215004
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| 摘要: |
| 目的 建立同时测定大鼠血清中15种胆汁酸浓度的液相色谱-串联质谱法（LC-MS/MS）。方法 血清样本用乙腈蛋白沉淀后，采用Xterra RP18（4.6 mm×100 mm，3.5 μm）色谱柱分离操作，以乙腈-10 mmol·L-1醋酸铵水溶液为流动相，梯度洗脱，流速为1 mL·min-1，用电喷雾离子源，负离子多反应监测。结果 15种胆汁酸成分在定量范围内线性关系良好，日内和日间精密度均<10%，低、中、高浓度提取回收率在69.93%~88.83%。结论 本研究建立的LC-MS/MS法简便、快速、专属性强，能够适用于大鼠血清中15种胆汁酸组分的检测。 |
| 关键词: 胆汁酸 液质联用 方法学 分型检测 |
| DOI：10.13748/j.cnki.issn1007-7693.2020.09.002 |
| 分类号:R917 |
| 基金项目:国家自然科学基金青年基金项目（81603181）；苏州市科技发展计划（SYSD2018234）；苏州市“科教兴卫”青年科技项目（KJXW2017015） |
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| Determination of Fifteen Bile Acids Concentration in Rats' Serum by LC-MS/MS |
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WANG Mengmeng1, YU Yunli1, QU Yuchen2, HUA Wenyan1, WANG Ji3, ZHANG Quanying1
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1.The Second Affiliated Hospital of Soochow University, Department of Clinical Pharmacology, Suzhou 215004, China;2.College of Pharmaceutical Sciences, Soochow University, Suzhou 215123, China;3.The Second Affiliated Hospital of Soochow University, Department of Oncology, Suzhou 215004, China
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| Abstract: |
| OBJECTIVE To establish an LC-MS/MS method for simultaneous determination of 15 bile acids in rats' serum. METHODS Serum samples were protein precipitated with acetonitrile and the separation was performed on a Xterra RP18 column(4.6 mm×100 mm, 3.5 μm). All analytes were gradient eluted with acetonitrile and 10 mmol·L-1 ammonium acetate in aqueous solution, of which flow rate was 1 mL·min-1. Quantitative analysis of 15 bile acids was conducted by a triple-quadrupole mass spectrometer with negative-electrospray ionization(ESI) source, monitored under a multiple reaction monitoring(MRM) mode. RESULTS The calibration curves of 15 biles acids were linear in the quantitative range. The RSDs of the intra-day and inter-day precision results were all <10%. The average extraction recoveries of the control samples at low, middle and high concentrations were between 69.93%-88.83%. CONCLUSION Established LC-MS/MS method is simple, rapid and specific, and can be used for the determination of 15 bile acids in rat serum. |
| Key words: bile acids LC-MS/MS method validation typing detection |
