HPLC-MS/MS法测定大鼠肺透析液中头孢哌酮/舒巴坦的浓度

Determination the concentration of cefoperazone/sulbactam in rat pulmonary dialysate by HPLC-MS/MS

目的建立液质联用(HPLC-MS/MS)法测定大鼠肺部透析液中头孢哌酮/舒巴坦的浓度。方法微透析样品通过HPLC-MS/MS检测,用Agilent Elipse XDB-C18柱(150 mm×4.6 mm,5μm),流动相为乙腈-0.125%甲酸水,等度洗脱,以负离子扫描多反应监测扫描方式进行检测。检测的离子对头孢哌酮m/z 644.2→m/z 115.2,舒巴坦m/z 232.0→m/z 140.0,内标奥美拉唑m/z344.3→m/z 194.1。结果头孢哌酮/舒巴坦的线性范围分别为0.2~20μg·mL^(-1),0.05~10μg·mL^(-1);日间和日内精密度相对偏差均小于15%;准确度和稳定性均符合生物样品的测定要求。结论本方法灵敏度高,操作简便快捷,适用于微透析样品中头孢哌酮/舒巴坦的浓度测定。

Objective To develop an high performance liquid chromatography- tandem mass spectrometry（ HPLC- MS / MS） method for measuring the concentration of cefoperazone / sulbactam in rat pulmonary dialysate. Methods Microdialysis samples were detected by HPLC-MS / MS. An Agilent Elipse XDB- C18column（ 4. 6 mm × 150 mm,5μm） was used with a mobile phase consisting acetonitrile and water with0. 125% formic acid,isocratic elution. The analysis was performed in multiple reaction monitoring mode via negative electrospray ionization source. Ion pairs were cefoperazone m / z 644. 2 →m / z 115. 2,sulbactam m / z 232. 0 →m / z 140. 0,omeprazole m / z 344. 3 →m / z 194. 1. Results The method had a lower limit of quantification of 0. 2 μg · mL^（-1）cefoperazone and 0. 05 μg·mL^（-1）sulbactam,linear up to 20 μg·mL^（-1）cefoperazone and 10 μg·mL^（-1）sulbactam. The intra- and inter- day precision were all less than 15%. The accuracy and stability were in line with the requirements for the detection of biological samples. Conclusion The method was proved to be rapid,easy and sensitive for determination of cefoperazone / sulbactam in microdialysis samples.