摘要
目的:建立测定人尿液中依非巴特浓度的方法。方法:尿液样品经蛋白沉淀后,采用液-质联用法进样测定,以甲醇-0.008mol·L-1甲酸铵水溶液(含0.1%甲酸)(35∶65)为流动相,AgilentZorbaxEclipseXDB-C18为色谱柱进行分离;采用电喷雾电离源,以多反应监测(MRM)方式进行正离子检测,用于定量分析的离子对依非巴特为m/z832.6→m/z646.4,内标为m/z931.6→m/z745.6。结果:依非巴特尿药浓度在5.0～5000.0ng·mL-1范围内线性关系良好(r=0.9996),最低定量限(LLOQ)为5.0ng·mL-1;日内和日间RSD均<7%,方法回收率为99.4%～103.1%,绝对回收率≥93%。结论:本方法选择性强、灵敏度高、重现性好,能快速、准确测定人尿液中依非巴特的浓度,并且成功用于依非巴特尿药排泄的研究。
OBJECTIVE： To establish the method for the determination of eptifibatide in human urine. METHODS： Following protein precipitation, LC-MS method was adopted. The determination was performed on a Agilent Zorbax Eclipse XDB-C18 （150 mm×4.6 mm,5 μm） column with mobile phase consisted of methanol-0.008 mol·L-1 ammonium formate （containing 0.1% formic acid）（35∶65）. Electrospray ionization source was used as detector and operated in the positive ion mode. Quantification was performed using multiple reaction monitoring （MRM） of the transitions m/z of 832.6→646.4 and 931.6→745.6 for eptifibatide and internal standard, respectively. RESULTS： The linear range was 5.0～5 000.0 ng·mL-1 for eptifibatide （r=0.999 6） with the LLOQ of 5.0 ng·mL-1. The intra-day and inter-day RSDs were less than 7%. Method recoveries were 99.4%～103.1% and absolute recovery was no less than 93%. CONCLUSION： The method is selective, sensitive, reproducible, rapid and accurate for the determination of eptifibatide in human urine and study of eptifibatide excretion.
出处
《中国药房》
CAS
CSCD
2012年第46期4350-4352,共3页
China Pharmacy
基金
广东省自然科学基金(9151064101000063)
广东省医学科研基金立项课题(A2011004)
