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目的:使用液相色谱-串联质谱联用(LC-MS/MS)技术,为氯拉扎尼(chlorazanil,I)、氯索隆(cicletanine,II)、西氯他宁(chlorxolone,III)、苄氢氯噻嗪(benzylhydrochlorothiazide,IV)、芬喹唑(fenquizone,V)和美替克仑(meticrane,VI)等6种利尿剂建立在人尿中的检测方法并进行方法验证。方法:将尿样用同等体积的5%乙酸铅水溶液沉淀蛋白质并离心后,使用电喷雾电离源的正、负离子切换模式,以多反应监测(MRM)模式进行定性和定量分析。结果:上述利尿剂I-VI的最低检测限(LOD)分别为1、0.1、0.01、1、2和10 ng/m L;线性范围(R2>0.99)分别为3~300 ng/m L、0.3~500 ng/m L、0.03~4000 ng/m L、3~1500 ng/m L、6~600 ng/m L和30~1600 ng/m L;6种药物在低、中和高三个浓度水平的日内变异系数均小于8%,日间变异系数均小于12%,检测的准确度在80%至120%之间;基质效应均在83%~115%范围内。结论:新建方法具有前处理简单、分析速度快、灵敏度高和重现性好等特点,已应用于我们实验室的兴奋剂常规检测中。
OBJECTIVE: To investigate the effect of chlorazanil (I), cicletanine (II), chloroxolone (III) 6 kinds of diuretics such as benzylhydrochlorothiazide (IV), fenquizone (V) and meticrane (VI) were established in human urine and verified by methods. Methods: Urine samples were precipitated by the same volume of 5% aqueous solution of lead acetate and centrifuged. Positive and negative ion exchange modes of the electrospray ionization source were used for qualitative and quantitative analysis by MRM. Results: The minimum detectable limit (LOD) of diuretic I-VI was 1, 0.1, 0.01, 1, 2 and 10 ng / m L, respectively. The linear range (R2> 0.99) 0.3 ~ 500 ng / m L, 0.03 ~ 4000 ng / m L, 3 ~ 1500 ng / m L, 6 ~ 600 ng / m L and 30 ~ 1600 ng / m L; The intra-day coefficients of variation (CVs) were all less than 8%, the day-to-day CVs were less than 12%, and the accuracy of detection was between 80% and 120%. The matrix effects ranged from 83% to 115%. Conclusion: The new method has the advantages of simple pre-treatment, fast analysis, high sensitivity and good reproducibility. It has been applied to the routine testing of stimulants in our laboratory.