摘要
建立电感耦合等离子体色谱法(ICP-MS)测定普瑞巴林口服溶液中镉(Cd)、铅(Pb)、汞(Hg)、砷(As)、钴(Co)、钒(V)、镍(Ni)共7种元素杂质含量。以^(115)In、^(209)Bi、^(69)Ge、^(45)Sc作为内标物,采用标准曲线法定量测定各元素杂质含量。结果表明,7种元素的专属性良好;检测限在0.007~0.3μg·L^(-1),定量限在0.02~1.0μg·L^(-1);相关系数(r)均大于0.999;加标回收率在93.5%~103.8%,RSD在2.4%~4.5%;重复性RSD在3.2%~6.2%(n=6);耐用性RSD在1.2%~8.8%。3批普瑞巴林口服溶液中元素杂质的含量均符合ICH Q3D的限度要求。该法操作简便,样品无需消解处理,稀释后直接检测,可快速、灵敏、准确测定普瑞巴林口服溶液中7种元素杂质的残留量。
To establish an inductively coupled plasma mass spectrometry(ICP-MS)method for the determination of seven elemental impurities(Cd,Pb,Hg,As,Co,V and Ni)in pregabalin oral solution.^(115)In,^(209)Bi,^(69)Ge and^(45)Sc were used as internal standards.The content of each element impurities was calculated by standard curve.The results show that the specificity of seven elemental impurities was good.The detection limits of the elemental impurities were from 0.007 to 0.3μg·L^(-1)and the quantitation limits were from 0.02 to 1.0μg·L^(-1).The correlation coefficients(r)were all above 0.999.The recoveries were between 93.5%to 103.8%and RSD was between 2.4%to 4.5%.The repeatability RSD was between 3.2%to 6.2%.The robustness RSD was between 1.2%to 8.8%.Test results of seven elements in three batches of samples met the requirements of ICH Q3D.This method is simple,rapid,sensitive,and accurate for the determination of seven elemental impurities in pregabalin oral solution.
作者
黎龙香
肖邦意
钟祥
Li Longxiang;Xiao Bangyi;Zhong Xiang(Jiangxi Kerui Pharmaceutical Co.,Ltd.,Ganzhou 341000,China)
出处
《山东化工》
CAS
2024年第3期134-137,共4页
Shandong Chemical Industry
基金
赣鄱俊才支持计划-主要学科学术和技术带头人培养项目(项目编号:20232BCJ22042)。
