摘要
建立顶空气相色谱法同时测定乙醇、丙酮、二氯甲烷、乙酸乙酯、正己烷和甲苯6种有机溶剂,检查国内部分已上市的注射用盐酸溴己新中溶剂残留情况。采用HP-5毛细管柱分离,考察了顶空平衡温度、平衡时间等条件对分离的影响并进行了方法学验证。结果显示,6种残留溶剂能够完全分离,在各自浓度范围内线性关系良好,r均大于0.999 0,检测限为0.024~0.400μg/m L,定量限为0.039~1.210μg/m L,回收率为85.0%~119.2%。由此可见,该方法操作简便、灵敏度高、准确可靠,可用于注射用盐酸溴己新中6种残留溶剂的测定。
A headspace gas chromatography method was established for the determination of six residual solvents including ethanol,acetone,methylene chloride,ethyl acetate,n-hexane and toluene in bromhexine hydrochloride for injection,checking the solvent residue of some marketed bromhexine hydrochloride in China.The study was achieved on a HP-5 capillary column and the effects of equilibrium temperature and equilibrium time on separation were investigated and verified by methods.The results showed that the six solvents could be completely separated with good linear relationships(r>0.9990)in their respective concentration ranges.The limits of detection and quantitation of the 6 residual solvents were 0.024-0.400μg/mL and 0.039-1.210μg/mL,respectively.And the spiked recoveries were in the range of 85.0%-119.2%.It can be seen that this method is simple,sensitive and accurate,which could be used for the determination of 6 residual solvents in bromhexine hydrochloride for injection.
作者
徐树娟
张磊
白青山
王亮
王洪凤
XU Shujuan;ZHANG Lei;BAI Qingshan;WANG Liang;WANG Hongfeng(Linyi Inspection and Testing Center,Linyi Shandong,276000,China)
出处
《质量安全与检验检测》
2024年第3期13-17,共5页
QUALITY SAFETY INSPECTION AND TESTING
基金
2022年山东省药品质量风险监测工作专项课题(鲁食药检业〔2022〕37号)。
关键词
顶空气相色谱法
注射用盐酸溴己新
残留溶剂
Headspace gas chromatography
Bromhexine hydrochloride for injection
Residual solvent
