高效液相-质谱联用法测定盐酸二甲双胍血药质量浓度

Determination of metformin hydrochloride in plasma by liquid chromatography-mass spectrometry

目的：建立测定盐酸二甲双胍血药质量浓度的高效液相-质谱联用方法（LC／MS／MS）。方法：色谱柱：CAPCELL C18柱（150mm×2．0mm，5μm）；流动相：10mmol·L^-1醋酸铵缓冲液-乙腈（50：50）；流速：0．2mL·min^-1；血浆样品用乙腈沉淀蛋白法处理，在三级四极杆串联质谱中经ESI源离子化，以多反应离子监测方式测定盐酸二甲双胍（m／z 130．0→71．0）的质量浓度。结果：盐酸二甲双胍血药质量浓度在10～2000μg·L^-1范围线性良好（r=0．9981），回收率为86．01％～98．28％，绝对回收率为92．72%～96．08％，日内、日间精密度均不大于10％。结论：方法灵敏、准确、快速、特异性强，可用于该药临床药动学特征的研究。

OBJECTIVE To establish an HPLC/MS/MS method in order to determine metformin hydrochloride in human plasma. METHODS The CAPCELL C18 column（ 150 mm ×2. 0 mm, 5μm）was used as analytical column with a mobile phase consisted of 10 mmol·L^-1 NH4 AC buffer-acetonitrile（50：50）, the flow rate was 0. 2 mL·min^-1. The plasma sample was wiped off protein with acetonirile, then ionized by electrospray ionization （ESI） source in the triple quadruple tandem mass spectrometer,and was quantitated with multiple reaction monitoring mode of m/z 130. 0→71.0. RESULTS The linear range was 10～ 2 000 μg· L^-1 , （ r = 0. 998 1 ） for metformin hydrochloride in human plasma, the recovery and the absolute recovery was 86. 01 % - 98. 28% and 92. 72% - 96. 08% ,respectively. The within- day and between- day deviations were less than 10%. CONCLUSION The method is proved to be sensitive, accurate, rapid, specific, and suitable for the clinical pharmacokinetics study.