LC-MS法检测大鼠血中甲苯磺丁脲含量

目的建立用LC-MS法检测大鼠血中的甲苯磺丁脲的方法。方法 Agilent Zoxbax SB-C18色谱柱,30℃柱温;流动相:0.1%甲酸溶液和乙腈梯度洗脱,流速为0.4 mL·min-1。使用SIM测定甲苯磺丁脲,卡马西平(内标)m/z 237,采用峰面积法定量。结果甲苯磺丁脲在10～1000ng·mL-1浓度范围内线性关系良好(r=0.9988)。日内精密度RSD和日间精密度RSD均小于8%,回收率均大于80%。结论本方法灵敏度高、专属性强,且操作简单,达到生物样本分析的要求。

Determination concentration of tolbutamide in rat plasma by LC-MS

OBJECTIVE To develop a LC-MS method for determination of tolbutamide in rats plasma.METOHDS Tolbutamide were extracted from rats plasma samples,and separation were carried out on Zorbax SB-C18 column（2.1mm×50mm,3.5 μm）at 35 ℃,acetonitrile-0.1% formic acid was used as mobile phase with the flow rate of 0.4 mL·min-1.ESI source was applied and operated in positive ion mode,and SIM mode were used to quantify tolbutamide（m/z 271）and carbamazepine（m/z 237,internal standard）.RESULTS The calibration curve in the concentration range of 10～1000 ng·mL-1 showed a good linear（r=0.9988）of the tolbutamide.The average extraction recoveries were better than 80%.Intra-day RSD and inter-day RSD were less than 8%.CONCLUSION This method is simple,rapid,accurate,and can be used to detect the tolbutamide in rat plasma for studying its pharmacokinetics.