液相色谱-串联质谱法测定片剂中卡马西平的含量

目的 建立液相色谱-串联质谱（LC/MS/MS）测定片剂中的卡马西平含量的方法.方法 色谱柱Zorbax Extend-C18柱（150 mm×4.6 mm,5 μm）;流动相：甲醇-0.01 mmol/l乙酸胺溶液（80：20,v/v）;流速：0.3 ml/min.结果 卡马西平浓度在0.05～40 μg/,ml范围内,峰面积与浓度线性关系良好,平均回收率为100.2%,RSD为1.02%.日内精密度、日间精密度的RSD分别为1.72%和1.91%.4批样品中卡马西平的含量分别为96.3%、98.6%、96.5%、99.0%.结论 本方法具有良好的灵敏度、准确度、精确度及专属性,结果准确,重现性好,易于操作,可用于制剂中卡马西平含量的测定.

Content determination of carbamazepine tablet by liquid chromatographic tandem mass spectrometry

Objective To develop liquid chromatography with tandem mass spectrometry （LC-MS/MS） detection for the con- tent determination of carbamazcpine tablet. Methods The method was used. The sample was analyzed on Zorbax Extend-C18 （ 150 mm × 4.6 mm ,5 μm ） ,with mobile phase consisting of methanol-0.01 rnmol/1 amine acetic acid （80 ： 20, v/v） at a flow rate of 0.3 ml/ rain. Results It was proved to be linear in the range of 0.05 ~ 40 μg/ml with a regression coefficient of 0. 999 4. The average recovery rate was 100.2% （n = 5） and RSD was 1.02%. The RSD of average contents of intra-day and inter-day was 1.72% and 1.91% respectively. The concentrations of four lot samples were 96.3% , 98.6% , 96.5% and 99.0% , respectively. Conclusion This method is accurate, precise, sensitive and specific to be used in the content determination of earbamazepine tablet.