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目的:建立使用液相色谱-串联质谱(LC-MS/MS)同时测定尿样中三种普坦类药物(托伐普坦、考尼伐坦和利希普坦)的方法。方法:样品用5%乙酸铅水溶液沉淀蛋白质并离心后,在电喷雾正离子模式下,以多反应监测(MRM)方式采集数据进行定性和定量分析。结果:托伐普坦、考尼伐坦、利希普坦的最低检测限(LOD)分别为15 ng/m L、1 ng/m L和2 ng/m L,线性范围(r2>0.99)分别为45~3000、3~2000和6~400ng/m L。3种药物在低、中、高3个浓度水平下,日内变异系数均小于8.2%,日间变异系数均小于13.6%,检测的准确度大于90%。结论:该方法具有样品前处理简单、检测快捷、灵敏度高、重现性好、定性定量准确等特点,已用于我们实验室的兴奋剂控制样品常规检测中。
OBJECTIVE: To establish a method for the simultaneous determination of three types of opium in urine samples (tolvaptan, memantine and lilipustine) by liquid chromatography-tandem mass spectrometry (LC-MS / MS). Methods: Samples were precipitated with 5% aqueous lead acetate and centrifuged. The samples were collected by MRM in positive electrospray ionization (ESI) mode for qualitative and quantitative analysis. Results: The limits of detection (LOD) of tolvaptan, memantine and lilipustine were 15 ng / m L, 1 ng / m L and 2 ng / m L, respectively. The linear range (r2> 0.99) Respectively 45 ~ 3000, 3 ~ 2000 and 6 ~ 400ng / m L. The three kinds of drugs at low, medium and high levels of three concentrations, the intra-day coefficient of variation were less than 8.2%, the coefficient of variation were less than 13.6% day, the detection accuracy is greater than 90%. Conclusion: This method has the characteristics of simple sample pretreatment, rapid detection, high sensitivity, good reproducibility and qualitative and quantitative accuracy. It has been used in the routine testing of stimulant control samples in our laboratory.