LC-MS/MS法同时测定人血浆中西地那非及其活性代谢物的浓度

Simultaneous Determination of Sildenafil and its Active Metabolite in Human Plasma Using LC-MS/MS Method

目的 建立人血浆中西地那非及其活性代谢物同时测定的方法 .方法采用LC-MS/MS分析,色谱柱为00B-4454-B0(Gemini?5μm NX-C18110?,50×2mm),流动相A为0.1% 甲酸的水溶液,流动相B为0.1% 甲酸的乙腈溶液.结果 在2.00~1000ng·mL-1范围内,西地那非及N-去甲基西地那非两者峰面积与内标峰面积的比值和浓度的线性关系均良好,批内、批间RSD均小于10.结论 本试验所建立的LC-MS/MS分析方法准确、灵敏、方便,可用于西地那非及其代谢物的人体药动学研究.

OBJECTIVE To establish a liquid chromatography-tandem mass spe ctrometry (LC-MS/MS) method for the determination of sildenafil and its activem etabolite in human plasma was developedand validated. METHODS L C-MS/MS method was used with a C 18 column (00B-4454-B0,Gemini 5μm NX-C 18 110 ,50×2mm) by the mobile phase A of water (containing 0.1% formic acid) and the mobile phase B of acetonitrile (containing 0.1% formic aci d) with the gradient elution. RESULTS The calibration curves of si ldenafil and its activemetabolite were established over the range of 2.00~1000 ng·mL -1 .The intra-day and inter-day relative standard deviations were less than 10%. CONCLUSION The present LC-MS/MS method was accu racy,sensitive and simple,and can be applied to a pharmacokinetic study in hum an.