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％HNO3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75As、111 Cd、202Hg、208 Pb、59Co、60Ni、51V、7Li、121Sb、63Cu 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.
Abstract
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 pharmaceuti-cal excipient sucrose was dissolved in 0.1％HN03 solution directly,and the contents of 75 As,111Cd,202Hg,208Pb,59 Co,60 Ni,51V,7 Li,121 Sb,and 63 Cu in sucrose were determined by the ICP-MS method with the optimized instru-mental 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=0.999 1).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.
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