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目的:建立同时测定人血浆中阿莫西林和克拉维酸钾的浓度的高效液相色谱-质谱联用(HPLC-MS-MS)方法。方法:以头孢羟氨苄为内标,血浆样品经乙腈沉淀蛋白后用0.5 ml二氯甲烷萃取,采用Hypersil ODS2色谱柱(2.1 mm×150mm,5μm),以乙腈-5 mmol·L-1醋酸铵含0.3%甲酸水溶液(9.5∶90.5)为流动相,流速为0.3 ml·min-1,以液相色谱分离、电喷雾离子化串联质谱进行检测,采用多反应检测模式(MRM)同时测定阿莫西林(m/z,363.9/222.7)和克拉维酸(m/z,197.8/135.8)的浓度。结果:阿莫西林和克拉维酸钾标准曲线的线性范围分别是20~22 000 ng·ml-1(r=0.998 4)和15~6 000 ng·ml-1(r=0.999 1);日内精密度与日间精密度RSD均小于15%。结论:本方法能简便、快速、准确地测定人血浆中阿莫西林和克拉维酸钾浓度,适用于阿莫西林克拉维酸钾缓释片的临床药动学研究。
Objective: To establish a high performance liquid chromatography-mass spectrometry (HPLC-MS-MS) method for simultaneous determination of amoxicillin and clavulanate potassium in human plasma. METHODS: Cefadroxil was used as an internal standard. The plasma samples were extracted with acetonitrile and then extracted with 0.5 ml dichloromethane. The samples were separated on a Hypersil ODS2 column (2.1 mm × 150 mm, 5 μm) with acetonitrile-5 mmol·L -1 ammonium acetate The mobile phase consisted of 0.3% formic acid aqueous solution (9.5: 90.5) with a flow rate of 0.3 ml · min-1 and separated by liquid chromatography and electrospray ionization tandem mass spectrometry. Simultaneous determination of amo The concentrations of xilin (m / z, 363.9 / 222.7) and clavulanic acid (m / z, 197.8 / 135.8). Results: The linear range of amoxicillin and clavulanate potassium standard curve was 20 ~ 22 000 ng · ml-1 (r = 0.998 4) and 15 ~ 6 000 ng · ml-1 (r = 0.999 1) RSD precision and daytime precision are less than 15%. Conclusion: The method is simple, rapid and accurate for the determination of amoxicillin and clavulanate in human plasma, and is suitable for clinical pharmacokinetics of amoxicillin-clavulanate sustained-release tablets.