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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 establish a method for the determination of colchicine in human urine by LC / MS / MS and to study the excretion of oral colchicine after oral administration. Method Column: Agilent Eclipse XDB C18 column, mobile phase: methanol-10 mmol.L-1 ammonium acetate (60:40) as ESI source positive ion MRM mode. The linear range was 3 ~ 3000 ng.mL-1 (γ = 0.9978). The relative recoveries ranged from 91.6% to 93.7%. The intra-day and inter-day variability was less than 15% and the matrix effect was 80.9% -90.9%. After 24,96 h medication, the average accumulated urine discharge rate was 15.2% and 20.9% respectively. Conclusion This method is suitable for the determination of urinary concentration of colchicine, which is excreted in the human body only by a small amount of the original drug.