摘要
目的 对桂利嗪片中镉(Cd)、铅(Pb)、砷(As)、汞(Hg)、钴(Co)、钒(V)、镍(Ni)7种元素杂质进行快速定量和风险评估.方法 样品无须预处理,采用能量色散型X射线荧光光谱法测定 11 家生产企业的 17 批桂利嗪片中 7 种元素杂质的含量.电压为 50 kV,电流为100 μA,氛围为空气,测试时间为 3 100 s.结果 Cd,Pb,As,Hg,Co,V,Ni元素的质量浓度分别在 0～16.6 mg/kg、0～16.6 mg/kg、0～50 mg/kg、0～100 mg/kg、0～166.6 mg/kg、0～333.5 mg/kg、0～667 mg/kg范围内与待测元素和校正元素的荧光强度比值线性关系良好(r≥0.999 0);平均回收率分别为 93.75%,80.00%,90.17%,82.28%,112.79%,115.60%,104.71%;定量限分别为 0.578,1.090,0.281,0.625,0.364,1.747,1.534 mg/kg.17 批桂利嗪片中上述 7 种元素的含量均低于控制阈值,未发现风险.结论 该方法操作简便,可直接快速定量桂利嗪片中 7 种元素杂质,适用于口服固体制剂桂利嗪片中元素杂质的风险评估.
Abstract
Objective To establish a rapid quantitation method for cadmium(Cd),lead(Pb),arsenic(As),mercury(Hg),cobalt(Co),vanadium(V)and nickel(Ni)in Cinnarizine Tablets,and to assess their risk.Methods The contents of seven elemental impurities in 17 batches of Cinnarizine Tablets from 11 manufacturers were determined by energy dispersive X-ray luorescence spectrometry without sample pretreatment.The voltage was 50 kV,the current was 100 μA,the atmosphere was air,and the test time was 3 100 s.Results The linear ranges of Cd,Pb,As,Hg,Co,V and Ni were 0-16.6 mg/kg,0-16.6 mg/kg,0-50 mg/kg,0-100 mg/kg,0-166.6 mg/kg,0-333.5 mg/kg,and 0-667 mg/kg(r≥0.999 0),respectively.The average recovery rates of seven elemental impurities were 93.75%,80.00%,90.17%,82.28%,112.79%,115.60%,and 104.71%,respectively.The limits of quantification of seven elemental impurities were 0.578,1.090,0.281,0.625,0.364,1.747,and 1.534 mg/kg,respectively.The contents of the seven elements mentioned above in 17 batches of Cinnarizine Tablets were all below the control threshold,and no risk was found.Conclusion The method is simple,it can directly and quickly quantify the seven elemental impurities in Cinnarizine Tablets,which is suitable for the risk assessment of elemental impurities in oral solid preparations of Cinnarizine Tablets.
维普
万方数据