LC/MS/MS测定人血浆中茚地那韦的浓度

 目的建立LC/MS/MS测定人血浆中茚地那韦的浓度。方法以利托那韦为内标,采用10 mmol·L^-1乙酸胺缓冲液(pH 4.10)-含0.1%甲酸的乙腈溶液(20:80)为流动相,以ZORBAX Eclipse XDB-C₈色谱柱为分析柱,通过电喷雾电离源(ESI),以选择离子反应监测(SRM)方式进行检测。用于定量分析的离子反应分别为m/z 614.4→421.2(茚地那韦)和m/z 721.3→296.0 (利托那韦)。结果茚地那韦线性范围0.009～30.0 mg·L^-1,定量下限为(0.010±0.001)mg·L^-1(n=5)。日内、日间精密度(RSD)小于4%,平均回收率大于90%。结论本法专属性强,样品处理方便,灵敏度高,适用于茚地那韦临床药动学研究。

LC/MS/MS determination of indinavir in human plasma

OBJECTIVE To establish a LC/MS/MS method for the determination of indinavir in human plasma.METHODS Ritonavir was used as the internal standard. Indinavir was separated on a ZORBAX Eclipse XDB-C₈ column.The mobile phase consisted of 10 mmol·L^-1 ammonium acetate buffer(pH 4.10)-acetonitrile contained 0.1% formic acid (20:80) .Electrospray ionization(ESI) source was applied and operated in the positive ion mode. Selected reaction monitoring(SRM) mode with the transitions of m/z 614.4→421.2 and m/z 721.3→ 296.0 was used to quantify indinavir and the internal standard, respectively. RESULTS The linear calibration curve was obtained over the concentration range of 0.009～30.0 mg·L^-1. The detection limit was(0.010±0.001) mg·L^-1(n=5). The inter-and intra-day precision (RSD) was less than 4% .The average recoveries were above 90% .CONCLUSION The method is proved to be robust,covenient, sensitivity and suitable for the clinical investigation of indinavir pharmacokinetics.