LC-MS/MS测定人血浆中格列本脲的浓度

 目的建立LC-MS/MS测定人血浆中格列本脲浓度的方法。方法以格列齐特为内标,采用0.1%甲酸-乙腈(35∶65)为流动相,以ZORBAX Eclipse XDB-C₁₈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 494.2→368.9(格列本脲)和m/z 324.0→126.9(格列齐特)。结果格列本脲线性范围6.67～500μg·L^-1,定量下限为(6.67±0.3)μg·L^-1(n=5)。日内、日间精密度(RSD)小于8%,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,适用于格列本脲临床药动学研究。

LC-MS/MS Determination of Glibenclamide in Human Plasma

OBJECTIVE To establish a LC/MS/MS method for the determination of glibenclamide in human plasma.METHODS Gliclazide was used as the internal standard. Glibenclamide was separated using a ZORBAX Eclipse XDB-C₁₈ column.The mobile phase consisted of 0.1% formic acid-acetonitrile (35∶65).Electrospray ionization(ESI) source was applied and operated in the positive ion mode.Selected reaction monitoring(SRM) mode with the transitions of m/z 494.2→368.9 and m/z 324.0→126.9 were used to quantify glibenclamide and the internal standard,respectively. RESULTS The linear calibration curve was obtained in the concentration range of 6.67～500 μg·L^-1. The limit of quantitation was(6.67±0.3) μg·L^-1(n=5). The inter-and intra-day precision(RSD) was less than 8% .The average recoveries were above 90%. CONCLUSION The method was proved to be robust,convenient,sensitivity and suitable for the clinical investigation of glibenclamide pharmacokinetics.