ICP-MS法测定18种动物药中重金属及有害元素的残留量及初步风险分析

目的：建立动物药中重金属及有害元素残留量的测定方法，为相关品种重金属及有害元素的风险评估、标准完善和质量监督提供依据。方法：采用电感耦合等离子体质谱（ICP-MS）法测定动物药中铅、镉、砷、汞的含量。等离子气流量：15.0 L·min^-1；蠕动泵0.20 r·s^-1；雾化室温度：2℃；辅助气流量：0.8 L·min^-1；He气流量：5 mL·min^-1；载气流量：0.8 L·min^-1；射频功率：1 550 W；数据采样模式：跳峰采集模式；采样深度：10 mm；重复次数：3次；扫描次数：100次。结果：4种重金属及有害元素的线性关系良好（r>0.990），回收率为80%~120%，重复性良好。按照现行2015年版中国药典水蛭等动物药重金属及有害元素限量标准，18种58批动物药的总体合格率为74.1%，其中铅、镉、砷、汞元素均存在超标的情况，其中合格率分别为91.4%、89.7%、86.2%和96.6%。结论：本文所建立的ICP-MS法适用于动物药中重金属及有害元素残留量的分析和评定。个别动物药品种重金属及有害元素污染情况较为严重。建议重视动物药的质量，从风险评估的角度，完善动物药重金属及有害元素的限量标准。

Objective: To establish a method for the determination of heavy metals and harmful elements in animal medicines, so as to provide a reference for risk evaluation, standard improvement and quality supervision for the related medicines.Methods: The contents of lead, cadmium, arsenic and mercury in animal drugs were determined by inductively coupled plasma mass spectrometry(ICP-MS). The determination conditions were as follows:plasma gas flow:15.0 L·min^-1; peristaltic pump:0.20 r·s^-1; spray chamber temperature:2℃; auxiliary gas flow rate:0.8 L·min^-1; He gas flow rate:5 mL·min^-1; sample carrier gas flow rate:0.8 L·min^-1; radio frequency power:1 550 W; data sampling mode:peak-jump acquisition mode; sampling depth:10 mm; repeat times:3 times; and scanning times:100 times.Results: The linear relationship of the four heavy metal elements was good(r>0.990), the recovery rate ranged from 80% to 120%, and the repeatability was also good. The established method was applicable for determining the amount of heavy metals and harmful elements of animal medicines. According to limits of heavy metals and harmful elements for animal medicines such as leech in Chinese Pharmacopoeia of 2015 edition, the qualified rate of heavy metals and harmful elements of these animal medicines was 74.1%. The qualified rates of Pb, Cd, As and Hg were 91.4%, 89.7%, 86.2% and 96.6%, respectively.Conclusion: The ICP-MS method established in this paper is suitable for the analysis and evaluation of heavy metals and harmful elements in animal drugs. The problem of heavy metals and harmful elements in animal medicines cannot be ignored. It is suggested to pay more attention to the quality of animal medicines and improve the standards of heavy metals and harmful elements of animal medicines from the view of risk assessment.

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