GC-MS法测定磷酸苯丙哌林中潜在基因毒性杂质  

Determination of the Potentially Genotoxic Impurities in Benproperine Phosphate by GC-MS

作　　者：董斌 徐桂连 郝爱鱼 姜博海 王戈 DONG Bin;XU Gui-lian;HAO Ai-yu;JIANG Bo-hai;WANG Ge(Dalian Institute For Drug Control,Liaoning Dalian 116021,China)

机构地区：[1]大连市药品检验检测院,辽宁大连116021

出　　处：《中国药物评价》2023年第4期313-315,共3页Chinese Journal of Drug Evaluation

基　　金：大连市高层次人才创新支持计划(青年科技之星项目)(项目编号:2021RQ032;项目名称:磷酸苯丙哌林生产工艺中风险管控关键评价技术研究)。

摘　　要：目的:建立GC-MS法测定磷酸苯丙哌林中潜在基因毒性杂质环氧丙烷和二氯亚砜。方法:采用TG-WAXMS毛细管柱,程序升温;离子源温度230℃,SIM模式;顶空进样,炉温为90℃,时间为30 min。结果:环氧丙烷在0.09~1.8μg·mL^(-1)浓度范围内线性关系良好;二氯亚砜在0.0454~1.818μg·mL^(-1)浓度范围内线性关系良好;环氧丙烷和二氯亚砜回收率分别为97.6%和99.2%(n=9);重复性RSD分别为4.9%和5.0%(n=6);10批原料药中均未检出环氧丙烷和二氯亚砜。结论:本方法灵敏度高,准确度好,可用于磷酸苯丙哌林中环氧丙烷和二氯亚砜的测定。Objective:To develop a GC-MS method for the determination of Propylene oxide and Thionyl chloride in Benproperine phosphate.Methods:A TG-WAXMS column was adopted with a gradient elution system.SIM was adopted for mass spectrometry,and Ion source temperature was 230℃.Headspace sampling was used,the equilibrium temperature was 90℃,and the equilibrium time was 30 minutes.Results:Propylene oxide showed good linearity at 0.09-1.8μg·mL^(-1),and thionyl chloride showed good linearity at 0.0454-1.818μg·mL^(-1).The recoveries of propylene oxide and thionyl chloride were 97.6%and 99.2%,respectively(n=9).The repeatability was 4.9%and 5.0%,respectively(n=6).No propylene oxide and thionyl chloride was detected in 10 batches of API.Conclusion:The method was sensitive and accurate,suitable for the quality control of propylene oxide and thionyl chloride in Benproperine phosphate.

关 键 词：磷酸苯丙哌林 环氧丙烷 二氯亚砜 基因毒性杂质 气相质谱联用法 

分 类 号：R927.11[医药卫生—药学]