超级微波消解-电感耦合等离子体质谱法同时检测羟苯甲酯与羟苯丙酯中16种元素杂质  

Simultaneous Determination of 16 Elemental Impurities in Methylparaben and Propylparaben Using Ultra Microwave-Assisted Digestion and Inductively Coupled Plasma Mass Spectrometry(ICP-MS)

作　　者：蔡立荣 舒海平 梁晟 周斌 谭跃 李昌亮 刘雁鸣 Cai Lirong;Shu Haiping;Liang Sheng;Zhou Bin;Tang Yue;Li Changliang;Liu Yanming(Hunan Institute for Drug Control,NMPA Key Laboratory for Pharmaceutical Excipients Engineering Technology Research,Changsha 410001,China;Hunan Warrant Pharmaceutical Co.,Ltd.,Changsha 410006,China)

机构地区：[1]湖南省药品检验检测研究院,国家药监局药用辅料工程技术研究重点实验室,湖南长沙410001 [2]湖南华纳大药厂股份有限公司,湖南长沙410006

出　　处：《广东化工》2024年第15期160-162,共3页Guangdong Chemical Industry

基　　金：湖南省自然科学基金科药联合基金资助项目(2023JJ60105,2023JJ60106)。

摘　　要：目的:建立符合法规要求的元素杂质检测方法并考察两种防腐剂羟苯甲酯和羟苯丙酯中元素杂质的残留水平。方法:采用超级微波消解样品,ICP-MS进行元素检测,用所建方法对多个厂家的多批次羟苯甲酯和羟苯丙酯中的16种元素杂质水平进行检测评估。结果:所建方法线性、检测限、定量限、准确度、精密度均符合法规要求,大多数批次所有元素均未超过吸入给药时的控制阈值,少数批次Ni、Cr、V含量超过了控制阈值。结论:所建方法适用于羟苯甲酯和羟苯丙酯中多种元素杂质的定量筛查,羟苯甲酯与丙酯,用于高风险吸入制剂时,元素杂质的残留风险总体较小,个别厂家需关注Ni、Cr、V的残留风险。Objective:To establish a method for detecting elemental impurities that complies with regulatory requirements and to investigate the residual levels of elemental impurities in the preservatives methylparaben and propylparaben.Methods:Samples were prepared by advanced microwave digestion and analyzed by Inductively Coupled Plasma Mass Spectrometry(ICP-MS)for the detection of elemental impurities.The developed method was applied to assess the levels of 16 elemental impurities across multiple batches of methylparaben and propylparaben from various manufacturers.Results:The method demonstrated compliance with regulatory standards in terms of linearity,detection limits,quantitation limits,accuracy,and precision.Most batches had elemental impurity levels below the control thresholds for inhalation administration.However,certain batches exhibited nickel(Ni),chromium(Cr),and vanadium(V)levels exceeding these thresholds.Conclusion:The developed method is suitable for the quantitative screening of multiple elemental impurities in methylparaben and propylparaben.Overall,the risk of elemental impurities is relatively low when these preservatives are used in high-risk inhalation formulations,though specific manufacturers should address potential residual risks associated with Ni,Cr,and V.

关 键 词：药用辅料 羟苯甲酯 羟苯丙酯 元素杂质 ICHQ3D 风险评估 

分 类 号：TQ[化学工程]