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 C_(18)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。
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 precipitation with methanol, the supernatant was evaporated to dryness and reconstituted with 200 IxL of mobile phase, then 40 μL was injected for analysis. A Diamonsil Cl8 column （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^-1 were 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. Resttits：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 pharrnaeokineties study of adefovir dipivoxil.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2008年第2期202-206,共5页
Chinese Journal of Pharmaceutical Analysis
