顶空毛细管气相色谱法测定阿伐斯汀原料药中的残留溶剂

Determination of Residual Solvents in Acrivastine by Headspace Gas Chromatography

目的建立顶空气相色谱法测定阿伐斯汀中乙醚、乙醇、甲苯共3种有机溶剂的残留量。方法采用顶空气相色谱法,氢火焰离子化检测器;载气为氮气,流速为2.0m L·min-1;色谱柱为DB-WAXETR毛细管柱(30m×0.32mm,0.50μm);采用柱温40℃保持5min,以30℃/min的速率升温至220℃,保持3min;进样口温度为220℃,检测器温度为250℃;分流进样,分流比为5∶1;顶空平衡温度为100℃,顶空平衡时间为30 min;顶空定量环体积为1 m L。以外标法用峰面积计算残留溶剂的含量。结果乙醚、乙醇、甲苯的线性关系良好(r=0.9992~1.0),平均回收率为96.4%~100.5%,检测限分别0.22μg·g-1、0.74μg·g-1和0.47μg·g-1。结论本方法可用于阿伐斯汀中残留溶剂的检查。

OBJECTIVE To establish a method for determination of three kinds of residual solvents in Acrivas- tine by headspace gas chromatography. METHODS The residual solvents were separated on DB-WAXETR （30m ×0. 32mm, 0. 50μm） capillary chromatography column equipped with FID detector. The carries gas was nitrogen with the flow rate of 2. 0mL· min-1. The initial temperature of column was set at 40℃ and maintained for 5min,and then followed by raising the temperature to 220℃ with a rate of 30℃/min and maintaining for 3rain. The inlet temperature was 220℃ and the FID detector temperature was 250℃. Split ratio was 5： 1. The temperature of the headspace oven was heated to 100℃ and lasted for 30min. The injection volume was 1.0mL. The content of residual solvents was calculated by using external standard method. RESULTS There was a good linear relationship in the experimental concentrations of three residual solvents（ r = 0. 9992 - 1.0）. The average recovery ranged from 96. 4% to 100. 5 %. The limit of detection was 0. 22μg· g-1 ,0. 74μg , g-1 and 0. 47 μg ·g-1, respectively. CONCLUSION The method can be used for detection of residual solvents in Acrivastine.