ICP-MS测定普瑞巴林口服溶液中7种元素杂质
ICP-MS Determination of Seven Element Impurities in Pregabalin Oral Solution
黎龙香 1肖邦意 1钟祥1
作者信息
- 1. 江西科睿药业有限公司,江西 赣州 341000
- 折叠
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 0.007～0.3 μg·L-1,定量限在 0.02～1.0 μg·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.
Abstract
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 0.3 μg·L-1 and the quantitation limits were from 0.02 to 1.0 μg·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.
关键词
普瑞巴林口服溶液/电感耦合等离子体质谱法(ICP-MS)/元素杂质/内标物Key words
pregabalin oral solution/inductively coupled plasma mass spectrometry(ICP-MS)/element impurities/internal standards引用本文复制引用
基金项目
赣鄱俊才支持计划-主要学科学术和技术带头人培养项目(20232BCJ22042)
出版年
2024
NETL
NSTL
万方数据