ICP-MS法测定艾拉戈克钠中14种元素杂质的含量  

Determination of 14 Elemental Impurities in Elagolix Sodium by ICP-MS

作　　者：田帅华 田凤艳 刘红伟 宗在伟[1] TIAN Shuaihua;TIAN Fengyan;LIU Hongwei;ZONG Zaiwei*(Jiangsu Aosaikang Pharmaceutical Co.,Ltd.,Nanjing 211112,China)

机构地区：[1]江苏奥赛康药业有限公司,南京211112

出　　处：《药学与临床研究》2024年第6期505-508,共4页Pharmaceutical and Clinical Research

摘　　要：目的:建立电感耦合等离子体质谱(ICP-MS)法测定艾拉戈克钠中铅(Pb)、镉(Cd)、汞(Hg)、砷(As)、钴(Co)、钒(V)、镍(Ni)、铬(Cr)、锰(Mn)、铁(Fe)、硅(Si)、硼(B)、铝(Al)、钯(Pd)的残留量。方法:采用微波消解法对样品进行前处理,以铋(Bi)、锗(Ge)、铟(In)和钪(Sc)为内标,采用动能歧视的碰撞模式(KED),石英同心雾化器进样,射频正向功率为1300 W,雾化气流速为0.9 L·min^(-1),等离子体气流速为17.0 L·min^(-1),辅助气流速为1.2 L·min^(-1)。结果:14种待测元素线性关系良好(r≥0.999);定量限在9.509×10^(-4)~9.029μg·g^(-1);平均加样回收率(n=9)在83.21%~126.5%;重复性试验RSD(n=6)均≤4.0%。建立的方法准确且灵敏度高,可用于艾拉戈克钠中14种元素杂质的痕量控制。结论:所建立的方法操作简便,方法专属性好,定量准确,满足艾拉戈克钠中14种元素杂质的质量控制要求。Objective:To establish an inductively coupled plasma mass spectrometry(ICP-MS)method for the quantification of lead(Pb),cadmium(Cd),mercury(Hg),arsenic(As),cobalt(Co),vanadium(V),nickel(Ni),chromium(Cr),manganese(Mn),iron(Fe),silicon(Si),boron(B),aluminum(Al)and palladium(Pd)in elagolix.Methods:Samples were pretreated using microwave digestion,with bismuth(Bi),germanium(Ge),indium(In)and scandium(Sc)as internal standards.Energy discrimination(KED)collision mode was employed,along with a glass concentric nebulizer for sampling,RF forward power at 1300 W,nebulizer gas flow rate at 0.9 L·min^(-1),plasma gas flow rate at 17.0 L·min^(-1) and auxiliary gas flow rate at 1.2 L·min^(-1).Results:Good linear relationships were achieved for the 14 elements to be tested(r≥0.999).The limits of quantification were 9.509×10^(-4)-9.029μg·g^(-1).The average recoveries(n=9)ranged from 91.19% to 126.5%,and the relative standard deviations(RSD,n=6)were all≤4.0%.Conclusion:The established method is simple,specific,accurate,and meets the quality control requirements for the determination of the 14 elemental impurities in elagolix.

关 键 词：艾拉戈克钠 电感耦合等离子体质谱 微波消解 元素杂质 

分 类 号：R92[医药卫生—药学]