首页|ICP-MS法测定帕立骨化醇中11种元素杂质的含量

ICP-MS法测定帕立骨化醇中11种元素杂质的含量

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建立了电感耦合等离子体质谱(ICP-MS)法测定帕立骨化醇(1)中铅(Pb)、镉(Cd)、汞(Hg)、砷(As)、钴(Co)、钒(V)、镍(Ni)、锂(Li)、锑(Sb)、铜(Cu)、铬(Cr)l1种元素杂质的含量.采用微波消解法对样品进行前处理,以铋(Bi)、锗(Ge)和钪(Sc)为内标,采用动能甄别(KED)碰撞模式,玻璃同心雾化器进样,射频正向功率为1 300 W,雾化气流速为0.8 L/min,等离子体气流速为15.0 L/min,辅助气流速为1.2 L/min.结果显示,11种待测元素在25%~200%浓度范围内线性关系良好;定量限在0.007~2.023 ng/mL;平均加样回收率(n=9)在86.0%~104.9%;重复性试验RSD(n=6)均≤2.3%.建立的方法准确且灵敏度高,可用于1中11种元素杂质的痕量控制.
Determination of Eleven Elemental Impurities in Paricalcitol by ICP-MS
An ICP-MS method was established to determine the contents of eleven elemental impurities,including lead(Pb),cadmium(Cd),mercury(Hg),arsenic(As),cobalt(Co),vanadium(V),nickel(Ni),lithium(Li),antimony(Sb),copper(Cu),and chromium(Cr),in paricalcitol(1).The sample was pretreated by microwave digestion method,with bismuth(Bi),germanium(Ge),and scandium(Sc)as internal standards.The kinetic energy discrimination(KED)collision mode was used,and the sample was injected into a glass concentric atomizer.The radio frequency forward power was 1 300 W,the atomization gas flow rate was 0.8 L/min,the plasma gas flow rate was 15.0 L/min,and the auxiliary gas flow rate was 1.2 L/min.The results showed that it was linear for above eleven elemental impurities in the concentration range of 25%-200%.The quantification limits were 0.007-2.023 ng/mL,the average sample recoveries(n=9)were 86.0%-104.9%,and RSDs(n=6)in the repeatability test were less than 2.3%.The established method is accurate and highly sensitive,which can be used for the trace control of eleven elemental impurities in 1.

paricalcitolICP-MSmicrowave digestionelemental impurity

李一芒、姚莉蓓、李思阅、于新颖、韩飞

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沈阳药科大学药学院,辽宁沈阳 110016

帕立骨化醇 电感耦合等离子体质谱 微波消解 元素杂质

2024

中国医药工业杂志
上海医药工业研究院,中国化学制药工业协会

中国医药工业杂志

CSTPCD
影响因子:0.487
ISSN:1001-8255
年,卷(期):2024.55(4)
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