顶空气相色谱法测定丙氨酰谷氨酰胺原料药中苯的残留

Determination of Benzene Residue in Alanyl Glutamine API by Headspace Gas Chromatography

建立一种可以检测丙氨酰谷氨酰胺原料药中苯残留的顶空气相色谱分析方法。方法:以6%氰丙基苯、94%二甲基硅氧烷为固定相(安捷伦DB-62430.0 m×0.250 mm,1.40μm或极性相似)的毛细管柱为色谱柱;起始柱温为70℃,维持2分钟,以每分钟10℃的速率升至120℃,再以每分钟20℃的速率升至220℃,维持3分钟;顶空瓶平衡温度为80℃,平衡时间20 min,检测器为氢火焰离子化检测器(FID),检测器温度为250℃;进样口温度为200℃。结果:使用该方法,各溶剂无干扰,灵敏度高,线性回归方程y=396903.576x+559.762(n=6),相关系数r=0.9998,回收率在90.90%~99.93%之间、9个测定结果的RSD为3.3%,专属性、精密度、耐用性均良好,溶液在24小时内稳定性,符合分析方法验证要求。该方法操作简单,重复性好,适用于丙氨酰谷氨酰胺原料药中苯残留的测定。

Establish a headspace gas chromatography method for detecting petroleum ether residue in Alanyl Glutamine API.Method:A capillary column with 6%cyanopropyl benzene and 94%dimethyl siloxane as the stationary phase(Agilent DB-62430.0 m*0.250 mm,1.40μm,or similar polarity)was used as the chromatographic column.The initial column temperature is 70℃,maintained for 2 minutes,increased to 120℃at a rate of 10℃per minute,and then increased to 220℃at a rate of 20℃per minute,maintained for 3 minutes.The equilibrium temperature of the headspace bottle is 80℃,the equilibrium time is 20 minutes,and the detector is FID,with a detector temperature of 250℃;The temperature of the injection port is 200℃.Result:Using this method,the blank solvent has no interference,high sensitivity,linear regression equation is y=396903.576x+559.762(n=6),correlation coefficient(r)0.9998,recovery rate between 90.90%and 99.93%,RSD of 9 determination results is 3.3%,specificity,precision,and durability are all good,and the solution is stable within 24 hours,both meets the requirements of analytical method validation.This method was proved to be simple,repeatable,and suitable for the determination of benzene residue in Alanyl Glutamine API.