ICP-MS 法测定药用辅料蔗糖中元素杂质的含量  

ICP-MS determination of elemental impurities in pharmaceutical excipient sucrose

作　　者：吴明珍 李樾[1,2] 朱健萍 刘庄蔚 杨锐 赵霞[1,2] WU Mingzhen;LI Yue;ZHU Jianping;LIU Zhuangwei;YANG Rui;ZHAO Xia(National Institutes for Food and Drug Control,Beijing 100050,China;NMPA Key Laboratory for Quality Research and Evaluation of Pharmaceutical Excipients,Beijing 100050,China;Guangxi Institute for Drug Control,Nanning 530022,China)

机构地区：[1]中国食品药品检定研究院,北京100050 [2]国家药品监督管理局药用辅料质量研究与评价重点实验室,北京100050 [3]广西壮族自治区药品检验研究院,南宁530022

出　　处：《中国药品标准》2024年第4期423-429,共7页Drug Standards of China

摘　　要：目的:建立ICP-MS法测定药用辅料蔗糖中砷(As)、镉(Cd)、汞(Hg)、铅(Pb)、钴(Co)、镍(Ni)、钒(V)、锂(Li)、锑(Sb)、铜(Cu)等10种元素的含量,评估其风险。方法:将药用辅料蔗糖溶解在0.1%HNO_(3)溶液中,采用ICP-MS法,设定测定模式为STD模式,通过优化仪器参数,测定蔗糖中^(75)As、^(111)Cd、^(202)Hg、^(208)Pb、^(59)Co、^(60)Ni、^(51)V、~7Li、^(121)Sb、^(63)Cu等10种元素的含量。结果:As、Cd、Pd、Co、Ni、V、Li、Sb、Cu等10种元素在0~100 ng·mL^(-1)范围内线性良好(r不低于0.99);Hg在0~2 ng·mL^(-1)范围内线性良好(r=0.999 1)。10种元素的平均回收率在99.8%~100.0%,RSD小于5%(n=6)。结论:方法易操作、准确度高,可用于药用辅料蔗糖中10种元素杂质的含量测定。通过结果可见,药用辅料蔗糖中含上述十种元素量远低于ICH Q3D中规定值,风险较小,修订标准时可不再单独考虑重金属项。Objective:An ICP-MS method was established for the determination of arsenic(As),cadmium(Cd),mercury(Hg),lead(Pb),cobalt(Co),nickel(Ni),vanadium(V),lithium(Li),antimony(Sb),copper(Cu)and other 10 elements in pharmaceutical excipients sucrose to assess their risks.Methods:The pharmaceutical excipient sucrose was dissolved in 0.1%HNO 3 solution directly,and the contents of ^(75)As,^(111)Cd,^(202)Hg,^(208)Pb,^(59)Co,^(60)Ni,^(51)V,~7Li,^(121)Sb and ^(63)Cu in sucrose were determined by the ICP-MS method with the optimized instrumental parameters in the STD mode.Results:The results showed that the linearity of the method was great in the range of 0-100 ng·mL^(-1) for As,Cd,Pd,Co,Ni,V,Li,Sb and Cu(the correlation coefficient r was not less than 0.99),and the linearity of the method was good in the range of 0-2 ng·mL^(-1) for Hg(r=0.9991).The average recoveries for the 10 elements were in the range of 99.8%-100.0%,and the RSDs were less than 5%(n=6).Conclusion:The method is easy to operate and has high accuracy.It can be used for the determination of 10 elemental impurities in pharmaceutical excipient sucrose.It can be seen that the content of the above ten elements in sucrose is much lower than the specified value in ICH Q3D,and the risk is small.The heavy metal item can no longer be considered separately when revising the standard.

关 键 词：蔗糖 药用辅料 电感耦合等离子体质谱法 元素杂质 ICH Q3D 

分 类 号：R921.2[医药卫生—药学]