LC-MS/MS法测定人尿液中舒巴坦钠的浓度及其动力学研究

目的:建立测定尿液中舒巴坦钠浓度的方法,并考察其动力学。方法:采用高效液相色谱串联质谱电喷雾检测(LC-MS/MS)法,以Agilent Zorbax SB C18进行分离,通过串联质谱仪,以选择反应监测方式进行测定。用于定量分析的舒巴坦钠离子对为m/z231.8→140.0,按外标法定量。结果:舒巴坦钠尿药浓度在0.051～40.80μg.mL-1范围内线性关系良好(r=0.9999),该方法的最低检测限为0.051μg.mL-1;相对回收率为98.95%～102.6%,日内和日间RSD分别为1.54%～7.97%、1.99%～9.85%。3个剂量(1、2、4g)组舒巴坦钠24h内平均尿液累积排泄率分别为(79.48±17.22)%、(79.83±15.25)%、(77.72±10.94)%。结论:本方法快速、简便、准确、灵敏,适用于舒巴坦钠的人体药动学研究。

Determination of Sulbactam Sodium Concentration in Human Urine by LC-MS/MS and Its Kinetics Study

OBJECTIVE:To establish a method for the determination of sulbactam sodium concentration in urine and to study excretion kinetics of it.METHODS:LC-MS/MS was adopted.The human urine was separated on Agilent Zorbax SB C18 column.A tandem mass spectrometer equipped with ESI was used as detector and operated in the negative ion mode.Sulbactam sodium in human urine was calculated by computing the peak area of sulbactam(m/z 231.8→140.0).RESULTS:The linear range of sulbactam sodium in human urine were 0.051～40.80 μg·mL-1(r=0.999 9).The lowest detection limit was 0.051 μg·mL-1.Relative recovery was from 98.95% to 102.6%.The RSDs of intra-day and inter-day were 1.54%～7.97% and 1.99%～9.85% respectively.Average accumulative urine excretion percentage of 3 doses of sulbactam sodium(1,2,4 g) in 24 h were(79.48±17.22)%,(79.83±15.25)% and(77.72±10.94)%.CONCLUSION:The developed method in the study has been proved to be rapid,simple,accurate and sensitive,and it is suitable for the excretion kinetics study of sulbactam sodium.