卡波姆系列药用辅料中苯残留的气相色谱测定方法的优化  

Optimization of gas chromatographic method for the determination of residual benzene content in carbomers

作　　者：陈沁颖 熊晔蓉[1] 冯作勋 何东升 孙春萌[1] 涂家生[1] CHEN Qinying;XIONG Yerong;FENG Zuoxun;HE Dongsheng;SUN Chunmeng;TU Jiasheng(NMPA Key Laboratory for Research and Evaluation of Pharmaceutical Preparations and Excipients,China Pharmaceutical University,Nanjing 210009,China)

机构地区：[1]国家药品监督管理局药物制剂及辅料研究与评价重点实验室,中国药科大学,南京210009

出　　处：《中国药品标准》2024年第4期398-404,共7页Drug Standards of China

基　　金：国家药典委员会-药品标准制修订研究课题资助项目(2018Y017,2018Y018,2018Y019)。

摘　　要：目的:采用气相色谱法对卡波姆共聚物、卡波姆均聚物和卡波姆间聚物中残留溶剂苯的检测进行方法的优化,解决《中国药典》现行方法在实际检测过程中存在的混合对照品溶液中苯检测灵敏度低、检测重复性差等问题。方法:选用DB-624色谱柱(30 m×0.530 mm, 3.00μm),程序升温,进样口温度140℃,检测器温度250℃,分流比5∶1,采用外标法定量检测残留溶剂苯。结果:苯在0.04~1.00μg·mL^(-1)浓度范围内线性关系良好(r=0.996 8);进样精密度RSD为6.8%(n=6);平均回收率为96.89%(RSD=8.1%,n=9)。结论:本试验建立的气相测定方法较《中国药典》现行方法系统适用性更好,准确度、精密度更高。优化后的方法更适用于卡波姆共聚物、卡波姆均聚物和卡波姆间聚物中残留溶剂苯的测定,为其质量管理和控制提供了参考与指导。Objective:To develop and validate gas chromatographic methods for the determination of residual benzene in carbomer copolymer,carbomer homopolymer and carbomer interpolymer,to address the issues of the current method in the Chinese Pharmacopoeia in the actual detection process,such as low sensitivity and poor repeatability of benzene detection in the mixed reference solution,and to optimize and improve the current standards for series of carbomer pharmaceutical excipients.Methods:Samples were separated on a column DB-624(30 m×0.530 mm,3.00μm)with temperature programming,the inlet temperature of 140℃,the detector temperature of 250℃,and the split ratio of 5∶1.The external standard method was adopted for the quantitative determination of residual benzene.Results:The linearity was great across the range of 0.04-1.00μg·mL^(-1)(r=0.9968),the injection precision of benzene was 6.8%(n=6),and the average recovery rate was 96.89%(RSD=8.1%,n=9).Conclusion:The gas chromatographic method established in this research is more specific,with higher accuracy and precision compared to the current method in the Chinese Pharmacopoeia.This optimized method is more suitable for the determination of residual benzene content in carbomer copolymer,carbomer homopolymer and carbomer interpolymer,providing reference and guidance for the quality management and the control of carbomer.

关 键 词：卡波姆 苯 气相色谱法 质量标准 残留溶剂 药用辅料 

分 类 号：R921.2[医药卫生—药学]