气相色谱法测定注射用艾司奥美拉唑钠包装用覆膜丁基胶塞中相关成分的迁移量

Migration Determination of Related Components in Film-Coated Butyl Rubber Stopper for Packaging of Esomeprazole Sodium for Injection by GC

目的建立检测注射用艾司奥美拉唑钠包装用覆膜丁基胶塞中棕榈酸和硬脂酸迁移量的气相色谱法。方法色谱柱为HP-5毛细管柱(30 m×0.32 mm,0.25μm),载气为氮气,流速为2.0 mL/min,进样口温度为300℃,采用氢火焰离子化检测器,检测器温度为300℃,程序升温,不分流进样,进样量为1μL。结果棕榈酸、硬脂酸质量浓度分别在0.38~18.81μg/mL(r=0.9998)、0.49~24.34μg/mL(r=1.0000)范围内与各待测成分峰面积/内标峰面积×内标质量浓度的平均值线性关系良好;精密度、重复性、稳定性试验结果的RSD均不大于2.10%;平均加样回收率分别为105.64%和102.40%,RSD分别为6.59%和3.21%(n=9)。迁移试验中各样品均未检出棕榈酸和硬脂酸。结论该方法灵敏度高,可用于注射用艾司奥美拉唑钠包装用覆膜丁基胶塞中棕榈酸和硬脂酸迁移量的监测。

Objective To establish a gas chromatography(GC)method for the migration dertermination of palmitic acid and stearic acid in the film-coated butyl rubber stopper for the packaging of Esomeprazole Sodium for Injection.Methods The chromatographic column was HP-5 capillary column(30 m×0.32 mm,0.25μm),the carrier gas was nitrogen,and the flow rate was 2.0 mL/min,the temperature of inlet was 300℃,the hydrogen flame-ionization detector(FID)was adopted with temperature of 300℃,the temperature was programmed,the sample was injected without partial flow,and the injection volume was 1μL.Results The linear ranges of palmitic acid and stearic acid were 0.38-18.81μg/mL(r=0.9998)and 0.49-24.34μg/mL(r=1.0000),respectively.The RSDs of precision,repeatability and stability tests were not more than 2.10%.The average recoveries of palmitic acid and stearic acid were 105.64%and 102.40%with RSDs of 6.59%and 3.21%,respectively.Palmitic acid and stearic acid were not detected in all samples in the migration test.Conclusion The method has high sensitivity and can be used to monitor the migration of palmitic acid and stearic acid in film-coated butyl rubber stopper for packaging of Esomeprazole Sodium for Injection.