摘要
目的 建立电感耦合等离子体质谱(ICP-MS)法测定硫酸氢伊伐布雷定缓释片中钴(Co)、铬(Cr)、镍(Ni)、钼(Mo)、钒(V)、砷(As)、镉(Cd)、铅(Pb)、钯(Pd)和汞(Hg)共10种元素杂质的含量。方法 采用微波消解法对样品进行前处理,以铋(Bi)、钪(Sc)和碲(Te)为内标,采用动能甄别(KED)碰撞模式进行检测。实验条件为: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0.8L/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 10种待测元素在25%~200%浓度范围内线性关系良好;定量限为0.015~1.08 ng/ml;平均加样回收率(n=9)为70.0%~105.0%;重复性试验的相对标准偏差(RSD,n=6)均≤6.5%。结论 该方法准确且灵敏度高,适用于硫酸氢伊伐布雷定缓释片中10种元素杂质的痕量控制。
Objective To establish an inductively coupled plasma mass spectrometry(ICP-MS)method for the determination of ten elemental impurities,including cobalt(Co),chromium(Cr),nickel(Ni),molybdenum(Mo),vanadium(V),arsenic(As),cadmium(Cd),lead(Pb),palladium(Pd),and mercury(Hg)in sustained-release tablets of ivabradine bisulfate.Methods The samples were pretreated using microwave digestion,with bismuth(Bi),scandium(Sc),and tellurium(Te)as internal standards.The kinetic energy discrimination(KED)collision mode was used,and the samples were introduced via a glass concentric nebulizer.The operating conditions were as follows:RF forward power,1300 W;nebulizer gas flow rate,0.8 L/min;plasma gas flow rate,15.0 L/min;and auxiliary gas flow rate,1.2 L/min.Results The ten target elements exhibited good linear relationships within the concentration range of 25%to 200%.The limits of quantification were between 0.015 and 1.08 ng/ml.The average recovery rates(n=9)were between 70.0%and 105.0%.The relative standard deviations(RSD,n=6)in the repeatability tests were all≤6.5%.Conclusion The established method is accurate and highly sensitive,which can be used for the trace analysis of elemental impurities in sustained-release tablets of ivabradine bisulfate.
作者
相晓伟
王晓莉
敦晓旭
赵春杰
XIANG Xiaowei;WANG Xiaoli;DUN Xiaoxu(School of Pharmacy,Shenyang Pharmaceutical University,Shenyang 110016,China;Jiangsu Hengrui Pharmaceuticals Co.,Ltd,Lianyungang 222047,China;不详)
出处
《中国处方药》
2025年第8期25-30,共6页
Journal of China Prescription Drug
