李存金 謝婷 周云峰 鄧杰華 吳喆 黃招光

中圖分類號 R917 文獻(xiàn)標(biāo)志碼 A 文章編號 1001-0408（2021）19-2377-06

DOI 10.6039/j.issn.1001-0408.2021.19.12

摘 要 目的：考察市售右歸丸中銅（Cu）、砷（As）、鎘（Cd）、汞（Hg）、鉛（Pb）等5種重金屬元素的含量，并評價其安全風(fēng)險。方法：以釔（89Y）、銦（115In）、鉍（209Bi）為內(nèi)標(biāo)，采用電感耦合等離子體質(zhì)譜（ICP-MS）法測定各元素的含量。設(shè)置ICP-MS的條件為霧化氣流量0.95 L/min，輔助氣流量1.2 L/min，等離子體氣（氬氣）流量18 L/min，泵速30 r/min;設(shè)置電感耦合等離子體射頻功率為1 200 W，模擬階段電壓為-1 750 V，脈沖階段電壓為1 300 V，偏轉(zhuǎn)裝置電壓為-12 V，檢測器為模擬和脈沖雙模式。對各元素含量測定方法進(jìn)行方法學(xué)考察，并對45批市售右歸丸樣品進(jìn)行測定。運用危害指數(shù)（HI）對各元素非致癌性風(fēng)險進(jìn)行分析，并擬定各元素的最大殘留閾值（MRL）。結(jié)果：Cu、As、Cd、Hg、Pb檢測質(zhì)量濃度線性范圍分別為10～200、1～50、0.4～30、0.2～6、2～100 μg/L， ?r均大于0.999 0;定量限分別為0.67、0.23、0.20、0.07、0.27 μg/L，檢測限分別為0.20、0.07、0.06、0.02、0.08 μg/L;精密度、穩(wěn)定性、重復(fù)性試驗的RSD均小于3.5%（n=6或n=5）;平均加樣回收率為92.96%～100.89%，RSD為2.23%～3.62%（n=3）。45批右歸丸樣品中Cu、As、Cd、Hg、Pb的平均含量分別為2.72、0.28、0.07、0.05、0.62 mg/kg，各元素的疊加HI小于1。右歸丸中5種重金屬元素的含量均低于擬定的MRL（Cu、As、Cd、Hg、Pb的MRL分別為20、2、1、0.2、5 mg/kg或者111.11、4.44、2.22、1.48、8.89 mg/kg）。結(jié)論：所建方法可用于測定右歸丸中5種重金屬的含量;市售右歸丸的常見重金屬污染率低，安全風(fēng)險小。

關(guān)鍵詞 右歸丸;重金屬;電感耦合等離子體質(zhì)譜法;限度;最大殘留閾值;危害指數(shù)

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.