LC-MS/MS法测定人血浆中米格列醇

LC-MS/MS determination of miglitol in human plasma

目的:建立测定人血浆中米格列醇的 LC-MS/MS 法。方法:以盐酸格拉司琼为内标,以 Kromasil CN 柱(2.1 mm×150mm,3.0μm)为分析柱;采用0.05%三氟乙酸乙腈溶液-0.05%三氟乙酸水溶液(80:20)为流动相;流速0.2 mL·min^(-1);柱温45℃。质谱条件为电喷雾电离源(ESI^+),以选择反应离子监测(SRM)方式进行检测,用于定量分析的反应离子分别为 m/z208.1→146.1(米格列醇),m/z 313.1→138.0(盐酸格拉司琼)。结果:米格列醇在0.01～4.0μg·mL^(-1)浓度范围内线性良好;最低检测限为2.0 ng·mL^(-1)(S/N=4);日内、日间精密度(RSD)均小于7%;低、中、高3个浓度的方法回收率均大于90%。结论:本法专属性强,灵敏度高,样品处理简单,可用于米格列醇临床药物动力学研究。

Objective： To establish an LC - MS/MS method for the determination of miglitol in the human plasma. Methods：Granisetron hydrochloride was used as the internal standard. The separation and analysis was performed on a Kromasil CN column（2.1mm×150mm,3.0μm）. The mobile phase consisted of 0. 05% trifluoroacetic acid acetonitrile solution-0.05% trifluoroacetic acid aqueous solution（80： 20）. The flow rate was 0. 2 mL · min^-1 and column temperature was 45℃. Electrospray ionization （ESI） source was applied and operated in the positive mode. Selected reaction monitoring（SRM） mode with the transitions of m/z 208. 1→146. 1 and m/z 313. 1→138.0 were adopted to quantify miglitol and granisetron hydrochloride （ internal standard）, respectively. Results： The assay linearities of miglitol was confirmed over the range of 0.01 -4. 0 μg·mL^-1, and the detection limit was 2. 0 ng·mL^-1. The intra and inter - day precision （RSD） were less than 7 %. The average recoveries were above 90%. Conclusion ：The method is proved to be specific, sensitive and covenient for the clinical pharmacokinetic studies of miglitol.