液相色谱-质谱联用法测定人血浆中氯吡格雷的浓度

发布时间：2018-05-19 14:09

  本文选题：氯吡格雷 + 液相色谱-质谱法　； 参考：《中国临床药理学杂志》2016年18期

【摘要】：目的建立液相色谱-质谱联用法(HPLC-MS/MS)测定人血浆中氯吡格雷的血药浓度。方法以硫酸氢氯吡格雷-d4作为内标,色谱柱为Xterra~汶RP_(18)(4.6 mm×100 mm,3.5μm),流动相为乙腈∶水相(0.1%甲酸水溶液)=66∶34,流速为1.0 m L·min~(-1)。三重四极杆质谱仪进行多反应监测模式,电喷雾离子源正离子检测。生物样品预处理用乙腈直接沉淀蛋白。考察该方法的专属性、标准曲线和定量下限、精密度与回收率、稳定性、溶血实验及试验样品再分析实验。结果线性范围为5.00~5000.00 ng·L~(-1),最低定量下限为5.00ng·L~(-1);批内、批间精密度均在1.28%~9.86%,相对偏差(RE)在-6.19%~14.27%;低、中、高3种浓度氯吡格雷质控样本内标归一化的基质效应分别为(113.69±10.62)%,(104.96±5.23)%,(105.12±4.01)%;提取回收率分别为(103.07±5.75)%,(102.87±14.34)%,(97.76±2.04)%。采血时溶血不影响测定准确度;试验样品再分析实验准确度符合要求。结论本方法是一种特异、快速、灵敏、稳定的HPLC-MS/MS,适用于人血浆中氯吡格雷的检测和药代动力学研究。
[Abstract]:Objective to establish a liquid chromatography-mass spectrometry (LC-MS) method for the determination of clopidogrel in human plasma. Methods Clopidogrel d4 sulfate was used as the internal standard. The chromatographic column was Xterra-1 RP_(18)(4.6 脳 100mm ~ (3. 5 渭 m), the mobile phase was acetonitrile (acetonitrile): water phase (0.1% formic acid solution) was 66: 34, the flow rate was 1.0 mL 路min ~ (-1). The triple quadrupole mass spectrometer is used to monitor the multi-reaction and the electrospray ion source is used to detect the positive ion. The protein was precipitated directly by acetonitrile in biological sample pretreatment. The specificity, standard curve and quantitative limit, precision and recovery, stability, hemolysis and sample reanalysis of the method were investigated. 缁撴灉绾挎，

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