液相色谱-串联质谱法测定秋水仙碱片在人尿中的含量

Determination of colchicine in human urine by LC-MS/MS

目的建立LC/MS/MS法测定人尿中的秋水仙碱浓度,初步研究人体口服秋水仙碱片剂后的排泄规律。方法色谱柱:Agilent Eclipse XDB C18柱,流动相:甲醇-10 mmol.L-1乙酸铵(60∶40),以ESI源正离子MRM模式测定。结果线性范围为3～3000 ng.mL-1(γ=0.9978),相对回收率为91.6%～93.7%,日内、日间变异(RSD)均<15%,基质效应为80.9%～90.9%。服药24,96 h后的原药平均累积尿排率分别为15.2%和20.9%。结论本方法适于秋水仙碱的尿药浓度测定,其在人体内仅经尿液排泄少部分原药。

Objective To develop a LC/MS/MS method for the determination of colchicine in human urine and study on its excretion.Methods Human urine samples,collected from 2 healthy volunteers were selected to fasting oral 1 mg colchicine tablet,added with scopolamine hydrobromide as internal standard,diluted by mobile phase solution,then measured by LC/MS/MS.Used the Agilent Eclipse XDB C18 as analytical column,and the mobile phase consisted of methanol-10 mmol·L-1 NH4AC buffer（60∶40）.The urine concentrations were detected in ESI positive MRM mode.Results The good linear range of colchicine was 3-3000 ng·mL-1（γ=0.9978）.The recovery was 91.6%-93.7%,and matrix effects was 80.9%-90.9%.The within-day and between-day deviations were less than 15%.The result showed that the mean urinary excretion percentage of colchicine after 24 h and 96 h were 15.2% and 20.9%,respectively.Conclusion The method suitable for determination of colchicine in human urine and clinical pharmacokinetic study.The drug only excreted small part through kidney in human in form of colchicine.