电感耦合等离子体-质谱法测定药用辅料山梨酸钾中元素杂质残留量  

Determination of element impurities in medicinal excipient potassium sorbate by ICP-MS

作　　者：庞赛 江坤 王平 PANG Sai;JIANG Kun;WANG Ping(Shenzhen Institute for Drug Control,Shenzhen 518057,Guangdong Province,China;Shenzhen Key Laboratory of Drug Quality Standard Research,Shenzhen 518057,Guangdong Province,China)

机构地区：[1]深圳市药品检验研究院,广东深圳518057 [2]深圳市药品质量标准研究重点实验室,广东深圳518057

出　　处：《中国药师》2024年第8期1303-1308,共6页China Pharmacist

基　　金：国家药典委员会标准提高项目(2022Y015)。

摘　　要：目的根据人用药品技术要求国际协调理事会(ICH)Q3D最新指导原则,建立电感耦合等离子体质谱(ICP-MS)法同时测定药用辅料山梨酸钾中镉(Cd)、铅(Pb)、砷(As)、汞(Hg)、钴(Co)、钒(V)、镍(Ni)7种元素杂质残留量的分析方法。方法采用2%硝酸溶液溶解样品后,用密闭超高压微波消解技术对山梨酸钾样品进行消解,并选用铼(Re)、铑(Rh)、锗(Ge)、钪(Sc)、铋(Bi)元素作为内标,校正基体干扰和漂移。结果建立的元素杂质测定方法在各自的检测浓度范围内线性关系良好(r>0.9980)。检测限在0.002~0.042 ng/g之间,回收率在85%~106%之间,各元素精密度的RSD均≤5%。依法测定13批来自不同生产企业的国产及进口药用辅料山梨酸钾样品中的元素杂质含量,均未超过限度,符合ICH的规定。结论所建立的方法操作简便,准确灵敏,专属性强,重复性好;本试验对药用辅料山梨酸钾元素杂质残留量情况开展筛查,不仅能掌握山梨酸钾的质量整体水平,也保障了山梨酸钾做为药用辅料的安全性,为《中国药典》标准的修订提供方法依据。Objective To establish a inductively coupled plasma-mass spectrometry(ICP-MS)method for 7 elemental impurities,cadmium(Cd),lead(Pb),arsenic(As),mercury(Hg),cobalt(Co),vanadium(V)and nickel(Ni)in medicinal excipient potassium sorbate according to the latest requirement of The International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use(ICH)Q3D.Methods After dissolving the sample with 2%nitric acid solution,the potassium sorbate sample was digested by closed ultra-high pressure microwave digestion technology,and the elements rhenium(Re),rhodium(Rh),germanium(Ge),scandium(Sc)and bismuth(Bi)were used as internal standards to correct the matrix interference and drift.Results The 7 elements showed good linearity in the specified concentration range(r>0.9980).The detection limits were between 0.002-0.042 ng/g,the recovery rates were between 85%-106%,and the RSDs of each element precision were≤5%.The content of elemental impurities in 13 batches of domestic and imported potassium sorbate samples from different manufacturers was determined legally,and none exceeded the limit,which was in line with the provisions of ICH.Conclusion The established method is simple,accurate,sensitive,specific and reproducible.In this test,the elemental impurity residues in potassium sorbate are screened,which can not only grasp the overall quality level of potassium sorbate,but also ensure the safety of potassium sorbate as medicinal excipients,and provides a methodological basis for the revision of the Chinese Pharmacopoeia.

关 键 词：山梨酸钾 药用辅料 电感耦合等离子体质谱 元素杂质 人用药品技术要求国际协调理事会Q3D 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]