摘要
目的:建立电感耦合等离子体质谱(ICP-MS)法测定碳酸镧原料药中Cd、Pb、As、Hg、Co、V、Ni、Se共8种元素杂质的含量。方法:样品经3%硝酸溶解后直接进样,采用标准加入法和氧化镧基体匹配法2种方法进行测定,结合在线内标校正消除基质效应,同时对比分析2种方法的测定结果。结果:2种方法在质量浓度0~30 ng·mL^(-1)范围内,8种元素线性均良好(r均>0.998),检测限分别为0.0039~0.22 ng·mL^(-1)和0.0091~0.72 ng·mL^(-1),重复性RSD分别为1.5%~4.9%和5.1%~6.9%,加标回收率分别为87.0%~98.3%和83.4%~114.4%,3批碳酸镧原料药中8种元素杂质含量测定结果无显著差异。结论:ICP-MS标准加入法和基体匹配法简单快速,灵敏度高,准确性好,可有效消除基质效应,适用于碳酸镧原料药中元素杂质的质量控制。
Objective:To develop an inductively coupled plasma mass spectrometry(ICP-MS)method for the determination of Cd,Pb,As,Hg,Co,V,Ni and Se in the crude drug of lanthanum carbonate.Methods:Samples were diluted with 3%nitric acid and directly injected.The matrix effect was eliminated by standard addition method and matrix matching method.Lanthanum oxide was added into the standard solution as the matrix.Compare the linearity,repeatability,accuracy,quantification limit,detection limit and sample determination results of the two methods by methodological validation and sample determination.Results:The linear ranges of ICP-MS standard addition method and matrix matching method were O-30 ng·mL^(-1),the correlation coefficients for all elemental impurities were good(r>0.998).Limits of detection were between 0.0039-0.22 ng·mL^(-1) and 0.0091-0.72 ng·mL^(-1).The RSD of repeatability(n=6)were between 1.5%-4.9%and 5.1%-6.9%.The recoveries were between 87.0%-98.3%and 83.4%-114.4%.The contents of 8 elemental impurities in the crude drug of lanthanum carbonate were basically same.Conclusion:The established two methods can effectively eliminate the matrix effect.They were both simple,rapid,sensitive,accurate and applicable for the elemental impurity control of lanthanum carbonate.
作者
丁芳芳
索喆丹
郑金琪
艾婕
顾霄
DING Fang-fang;SUO Zhe-dan;ZHENG Jin-qi;AI Jie;GU Xiao(Zhejiang Institute for Food and Drug Control,Zhejiang Key Laboratory of Biopharmaceutical Contact Materials,Zhejiang Research Center for API Security,National Medical Products Administration Key Laboratory for Core Technology of Generic Drug Evaluation,Hangzhou 310052,China;Zhejiang Guobang Pharmaceutical Co.,Ltd.,Shaoxing 312300,China)
出处
《药物分析杂志》
北大核心
2025年第5期901-906,共6页
Chinese Journal of Pharmaceutical Analysis
作者简介
通信作者:顾霄,Tel:(0571)87180355,E-mail:guxiao@zjyj.org.cn;第一作者:丁芳芳,Tel:(0571)87180340,E-mail:dingffxm@163.com。
