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目的:建立人血清中亮丙瑞林浓度的LC-MS/MS测定方法。方法:采用乙腈沉淀蛋白提取血清中目标成分。选用Agela Venusil ASB C18色谱柱(150 mm×4.6 mm,5μm),以乙腈-5 mmol.L-1醋酸铵-甲酸(30∶70∶0.1)为流动相,采用多反应离子监测(MRM)模式进行正离子检测,选择监测离子反应为m/z605.6→248.9[M+2H]2+(亮丙瑞林)和151.8→110.1[M+H]+(对乙酰氨基酚)。结果:血清中内源性物质不干扰亮丙瑞林的测定;亮丙瑞林的线性范围为0.1~10.0 ng.mL-1,最低定量限为0.1 ng.mL-1。方法准确度为88.5%~111.5%,日内和日间精密度均<15%。结论:本文建立的LC-MS/MS法,简单快速,专属性强,灵敏度高,可用于亮丙瑞林缓释制剂在人体内的药代动力学研究。
Objective: To establish a method for the determination of leuprolide in human serum by LC-MS / MS. Methods: The target components in serum were extracted by acetonitrile precipitation protein. Agela Venusil ASB C18 column (150 mm × 4.6 mm, 5 μm) and acetonitrile-5 mmol·L -1 ammonium acetate-formic acid (30:70:0.1) were used as the mobile phase and multi-reactive ion monitoring (MRM) Positive ion detection was performed with the choice of monitoring ion responses m / z 605.6 → 248.9 [M + 2H] 2+ (leuprorelin) and 151.8 → 110.1 [M + H] + (paracetamol). Results: The serum endogenous substances did not interfere with the determination of leuprorelin; the linear range of leuprolide was 0.1 ~ 10.0 ng.mL-1, the lowest limit of quantification was 0.1 ng.mL-1. The accuracy of the method was 88.5% -111.5%, with intra-day and inter-day precision <15%. Conclusion: The LC-MS / MS method established in this paper is simple, rapid, specific and sensitive and can be used to study the pharmacokinetics of leuprolide sustained-release preparation in human.