右归丸中5种重金属元素的含量分析

李存金 谢婷 周云峰 邓杰华 吴喆 黄招光

中图分类号 R917 文献标志码 A 文章编号 1001-0408（2021）19-2377-06

DOI 10.6039/j.issn.1001-0408.2021.19.12

摘 要 目的：考察市售右归丸中铜（Cu）、砷（As）、镉（Cd）、汞（Hg）、铅（Pb）等5种重金属元素的含量，并评价其安全风险。方法：以钇（89Y）、铟（115In）、铋（209Bi）为内标，采用电感耦合等离子体质谱（ICP-MS）法测定各元素的含量。设置ICP-MS的条件为雾化气流量0.95 L/min，辅助气流量1.2 L/min，等离子体气（氩气）流量18 L/min，泵速30 r/min;设置电感耦合等离子体射频功率為1 200 W，模拟阶段电压为-1 750 V，脉冲阶段电压为1 300 V，偏转装置电压为-12 V，检测器为模拟和脉冲双模式。对各元素含量测定方法进行方法学考察，并对45批市售右归丸样品进行测定。运用危害指数（HI）对各元素非致癌性风险进行分析，并拟定各元素的最大残留阈值（MRL）。结果：Cu、As、Cd、Hg、Pb检测质量浓度线性范围分别为10～200、1～50、0.4～30、0.2～6、2～100 μg/L，  r均大于0.999 0;定量限分别为0.67、0.23、0.20、0.07、0.27 μg/L，检测限分别为0.20、0.07、0.06、0.02、0.08 μg/L;精密度、稳定性、重复性试验的RSD均小于3.5%（n=6或n=5）;平均加样回收率为92.96%～100.89%，RSD为2.23%～3.62%（n=3）。45批右归丸样品中Cu、As、Cd、Hg、Pb的平均含量分别为2.72、0.28、0.07、0.05、0.62 mg/kg，各元素的叠加HI小于1。右归丸中5种重金属元素的含量均低于拟定的MRL（Cu、As、Cd、Hg、Pb的MRL分别为20、2、1、0.2、5 mg/kg或者111.11、4.44、2.22、1.48、8.89 mg/kg）。结论：所建方法可用于测定右归丸中5种重金属的含量;市售右归丸的常见重金属污染率低，安全风险小。

关键词 右归丸;重金属;电感耦合等离子体质谱法;限度;最大残留阈值;危害指数

Content Analysis of 5 Kinds of Heavy Metal in Yougui Pills

LI Cunjin1，XIE Ting2，ZHOU Yunfeng3，DENG Jiehua3，WU Zhe3，HUANG Zhaoguang3（1. The Fourth Inspection Institute of Jiangxi Drug Inspector Center， Jiangxi Yichun 336000， China; 2. Science and Education Department， Yichun Municipal Peoples Hospital， Jiangxi Yichun 336000， China; 3. Drug Department， Yichun Institute for Food and Drug Inspection， Jiangxi Yichun 336000， China）

ABSTRACT   OBJECTIVE： To investigate the contents of 5 kinds of heavy metal as copper （Cu）， arsenic （As）， cadmium （Cd）， mercury （Hg） and lead （Pb） in Yougui pills， and to evaluate its safety risk. METHODS： Using yttrium （89Y）， indium （115In） and bismuth （209bi） as internal standard， the contents of each element were determined by ICP-MS. ICP-MS condition included that atomization gas flow rate was 0.95 L/min，auxiliary gas flow rate was 1.2 L/min，plasma gas （argon） flow rate was 18 L/min， pump speed was 30 r/min. RF power of inductively coupled plasma was 1 200 W， the voltage in simulation stage was 1 750 V， the voltage in pulse stage was 1 300 V， the voltage of deflection device was -12 V， and the detector was in analog and pulse dual-mode. The determination methods of various elements were investigated， and 45 batches of marketed Yougui pills were determined. Hazard index （HI） was used to analyze the non-carcinogenic risk of each element and calculate the maximum residual limit （MRL） of each element. RESULTS： The linear range of Cu， As， Cd， Hg and Pb ranged from 10-200， 1-50， 0.4-30， 0.2-6 and 2-100 μg/L （all r>0.999 0）， respectively. The limits of quantitation were 0.67， 0.23， 0.20， 0.07， 0.27 μg/L. The limits of detection were 0.20， 0.07， 0.06， 0.02， 0.08 μg/L. RSDs of precision， stability and reproducibility tests were all lower than 3.5% （n=6 or n=5）. Average recoveries were 92.96%-100.89% （RSD=2.23%-3.62%， n=3）. Average contents of Cu， As， Cd， Hg and Pb in 45 batches of Yougui pills were 2.72， 0.28， 0.07， 0.05， 0.62 mg/kg， and superimposed HI of each element was less than 1. The contents of 5 kinds of heavy metals in Yougui pills were lower than the proposed MRL （MRL of Cu， As， Cd， Hg and Pb were 20， 2， 1， 0.2， 5 mg/kg or 111.11， 4.44， 2.22， 1.48， 8.89 mg/kg respectively）. CONCLUSIONS： Established method can be used for the determination of content of 5 kinds of heavy metal in Yougui pills; the heavy metal pollution rate of marketed Yougui pills is low and the safety risk is small.