【摘要】 目的:建立测定人血清中阿德福韦的液相色谱-质谱/质谱联用（LC～MS/MS）方法。方法:血清样品经甲醇沉淀蛋白,上清液吹干,200μL流动相复溶,离心,取40μL进样。色谱柱为 Diamonsil C₁₈柱（250 mm×4.6 mm,5μm）,流动相为甲醇-水-甲酸（20:80:0.1,v/v/v）,流速0.6 mL·min^-1,采用电喷雾离子化四极杆串联质谱,多反应监测方式测定样品浓度。监测离子对分别为 m/z274→m/z162（阿德福韦）和 m/z226→m/z135（内标阿昔洛韦）。结果:阿德福韦在1.25～160μg·L^-1浓度范围内线性关系良好（r=0.9992,n=5）,最低定量限为1.25μg·L^-1。低、中、高3种浓度质控样品的日内、日间精密度小于8.64%,方法回收率99.20%～101.98%,阿德福韦提取回收率56.50%～59.26%。结论:该方法灵敏度高,定量准确,适用于阿德福韦酯人体药代动力学研究。更多还原

【Abstract】 Objective:To develop a liquid chromatography-tandem mass spectrometry（LC-MS/MS）method for the determination of adefovir in human serum.Methods:The analyte was isolated from serum by protein precipitati- on with methanol,the supernatant was evaporated to dryness and reconstituted with 200 μL of mobile phase,then 40 μL was injected for analysis.A Diamonsil C₁₈column（250 mm×4.6 mm,5 μm）and mobile phase consisted of methanol-water-formic acid（20:80:0.1 ,v/v/v）at a flow rate of 0.6 mL·min^-1were used to separate adefovir and IS.Electrospray ionization（ESI）source was applied and operated in the positive ion mode.Multiple reaction monitoring（MRM）mode with the transition of m/z 274→m/z 162 and m/z 226→m/z 135 were used to quantify adefovir and aciclovir（IS）,respectively.Results:A good linearity was obtained in the concentration range of 1.25 -160 μg·L^-1（r=0.9992,n=5 ）.The lower quantitative limit was 1.25 μg·L^-1.The inter-and intra-day RSDs were less than 8.64%,the method recoveries were within 99.20%-101.98% and the extraction recoveries were within 56.50%-59.26%.Conclusion:The method is sensitive and acuurate,and proves to be suitable for human pharmacokinetics study of adefovir dipivoxil.更多还原