Department of Pharmacy, Tongji Hospital of Tongji Medical College, Huazhong University of Science and Technology, Wuhan 430030, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Oct 15;878(28):2911-5. doi: 10.1016/j.jchromb.2010.08.008. Epub 2010 Aug 17.
A rapid, sensitive and simple high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for determination of cefazedone in human plasma using metronidazole as internal standard (IS). The chromatographic separation was achieved on an Ultimate XB-CN column (2.1mm×150mm, 5μm) with an isocratic mobile phase of acetonitrile and 20mM ammonium acetate in 0.1% formic acid in water (15:85, v/v). Detection was performed using electrospray ionization in positive ion multiple reaction-monitoring mode (SRM), monitoring the transitions m/z 548.2→344.1 for cefazedone and m/z 172.2→128.1 for IS. Calibration curves were linear over a wide range of 0.20-401.12μg/mL for cefazedone in plasma. The lower limit of quantification (LLOQ) was 0.20μg/mL. The intra- and inter-day precisions were less than 7.2%. The average recovery of cefazedone was 90.8-91.0%. The validated method was successfully applied to the pharmacokinetic study of cefazedone in Chinese healthy volunteers following intravenous (IV) administration of 500, 1000 and 2000mg cefazedone injection.
建立了一种灵敏、快速和简单的高效液相色谱-串联质谱(HPLC-MS/MS)法,用于以甲硝唑为内标(IS)测定人血浆中的头孢唑肟。采用 Ultimate XB-CN 柱(2.1mm×150mm,5μm),以乙腈和 20mM 乙酸铵在 0.1%甲酸水溶液(15:85,v/v)中的等度洗脱为流动相,在正离子多反应监测模式(SRM)下进行检测,监测头孢唑肟的 m/z 548.2→344.1 和 IS 的 m/z 172.2→128.1。头孢唑肟在血浆中的浓度范围为 0.20-401.12μg/mL 时,校准曲线呈线性。定量下限(LLOQ)为 0.20μg/mL。日内和日间精密度均小于 7.2%。头孢唑肟的平均回收率为 90.8-91.0%。该方法已成功应用于中国健康志愿者静脉注射 500、1000 和 2000mg 头孢唑肟注射液后头孢唑肟的药代动力学研究。