摘要
目的:建立前列欣胶囊中铅、镉、铜、汞、砷5种元素残留量的测定方法。方法:样品经微波消解后采用电感耦合等离子体质谱法(ICP-MS法)测定,射频功率为1. 70 k W,载气流速为1. 05 L·min^-1。通过在线加入内标锗、铟、铋元素的方法来校正基体效应和干扰。结果:5种元素在检测质量浓度范围内线性关系均良好(r> 0. 996 6),进样精密度RSD在0. 93%~1. 68%,重复性RSD在1. 45%~3. 03%,各元素的回收率为93. 60%~95. 90%(RSD <1. 69%),样品在消解后24 h内各元素稳定性良好(RSD <1. 41%)。结论:该方法简便、灵敏、准确,可用于前列欣胶囊中铅、镉、铜、汞、砷的检测,为其风险监控提供技术参数。
Objective: To develop a method for the determination of residues of lead( Pb),cadmium( Cd),copper( Cu),mercury( Hg) and arsenic( As) in the Qianliexin capsules. Methods: Samples were digested by microwave and determined by inductively coupled plasma mass spectrometry( ICP-MS). The RF power was 1. 75 k W and the carrier gas flow rate was 1. 05 L·min^-1. Matrix effect and interference was corrected by on-line addition of internal standard elements Ge,in and Bi. Results: The linearities for the elements were good with the correlation coefficients( r) being all above 0. 996 6. The RSDs of the injection precision test were in the range of0. 93%-1. 68% and the RSDs of the repeatability test were in the range of 1. 45%-3. 03%. The recoveries of the 5 elements were in the range of 93. 60%-95. 90% with the RSDs being all bellow 1. 69%. The digested solution was stable in 24 h. Conclusion: The method was simple,sensitive and accurate,and it can be used for the content determination of Pb,Cd,Cu,Hg,As in Qianliexin capsules,providing helpful information for the risk monitoring.
作者
张玉伟
田方园
姚元成
刁瑞丽
范圣此
李秀凤
孟兆青
ZHANG Yu-wei;TIAN Fang-yuan;YAO Yuan-cheng;DIAO Rui-li;FAN Sheng-ci;LI Xiu-feng;MENG Zhao-qing(Shandong Hongjitang Pharmaceutical Group Co.,Ltd.,Shandong Ji'nan 250103,China)
出处
《中国药物评价》
2019年第6期430-434,共5页
Chinese Journal of Drug Evaluation
基金
国家十三五重点研发计划(项目编号:SQ2017YFC170600)
山东省济南市泉城“5150”引才倍增计划(项目编号:2017017)
关键词
前列欣胶囊
重金属
含量测定
电感耦合等离子体质谱法
Qialiexin capsules
Heavy metal
Content determination
Inductively coupled plasma mass spectrometer(ICP-MS)
