關(guān)鍵詞：電感耦合等離子體質(zhì)譜法;中藥注射液;重金屬及有害元素;直接稀釋法

建立電感耦合等離子體質(zhì)譜法（ICP-MS）測定復(fù)方蒲公英注射液、野菊花注射液、腫節(jié)風(fēng)注射液、白花蛇舌草注射液和夏天無注射液中銅（Cu）、砷（As）、鎘（Cd）、鉛（Pb）和汞（Hg）5種重金屬及有害元素含量的方法。樣品用2%硝酸（V/V）直接稀釋，以⁷²Ge、¹¹⁵In、¹⁸⁵Re為內(nèi)標(biāo)，采用ICP-MS測定溶液中元素含量。方法學(xué)驗(yàn)證表明：Cu、As、Cd、Pb在0.5~50 μg/L和Hg在0.5~10 μg/L的質(zhì)量濃度范圍內(nèi)線性關(guān)系良好（r²>0.999）；低、中、高3種濃度水平，復(fù)方蒲公英注射液、夏天無注射液、腫節(jié)風(fēng)注射液、野菊花注射液、白花蛇舌草注射液中5種元素的平均回收率（n=3）分別為90.7%~121.2%、83.4 %~119.9%、90.8%~116.3%、86.4%~109.0%、85.0%~118.0%，重復(fù)性RSD（n=3）分別為1.4%~9.8%、0.2%~6.7%、0.4%~7.4%、0.6%~10.0%、0.1%~11.1%；5種注射液中Cu、As、Cd、Pb、Hg的LOQ分別為0.002 1 mg/L、0.001 6 mg/L、0.000 56 mg/L、0.001 8 mg/L、0.001 7 mg/L，滿足方法學(xué)驗(yàn)證的要求。各3批次實(shí)際中藥注射液樣品的測試結(jié)果表明，5種元素含量均小于限量值，說明其安全風(fēng)險(xiǎn)較小。方法操作簡便、快速、靈敏度高、準(zhǔn)確度好，適合5種注射液中的Cu、As、Cd、Pb、Hg等有害元素含量的測定，為其他中藥注射液中元素雜質(zhì)分析方法的建立提供參考。

Determination of heavy metals and harmful elements in five traditional Chinese medicine injections using inductively coupled plasma mass spectrometry (ICP-MS)
ZHANG Chunhua, CHEN Chuntao, HAN Bikai, LI Ziyi, CHEN Liang, ZHU Zhixin, WU Huiqin, HUANG Xiaolan
Guangdong Provincial Public Laboratory of Analysis and Testing Technology, Guangdong Engineering and Technology Research Center for Quality and Safety of Traditional Chinese Medicine, China National Analytical Center, Guangzhou, Guangzhou 510070, China
Abstract: A method for the determination of heavy metals and harmful elements(Cu, As, Cd, Pb, Hg) in five traditional Chinese medicine injections using inductively coupled plasma mass spectrometry (ICP-MS) was developed and validated. The traditional Chinese medicine injections was pretreated by diluting with 2% nitric acid (V/V), then the five target elements and internal standard elements (⁷²Ge, ¹¹⁵In, ¹⁸⁵Re) were detected by ICP-MS. The established method was fully validated. The calibration curves were linear over a range of 0.5-50 μg/L for Cu, As, Cd, Pb, and 0.5-10 μg/L for Hg, and the correlation coefficients (r²) were higher than 0.999. At three spiked levels (low, medium and high concentration), the average recoveries (n=3) for the five elements in Fufang Pugongying injection, Xiatianwu injection, Zhongjiefeng injection, Yejuhua injection, Baihuasheshecao injection were 90.7%-121.2%, 83.4%-119.9%, 90.8%-116.3%, 86.4%-109.0%, 85.0%-118.0%, respectively, with the RSDs (n=3) were 1.4%-9.8%, 0.2%-6.7%, 0.4%-7.4%, 0.6%-10.0%. 0.1%-11.1%. The limits of quantitation (LOQ) for Cu, As, Cd, Pb, Hg in five traditional Chinese medicine injections were 0.002 1, 0.001 6, 0.000 56, 0.001 8, 0.001 7 mg/L. Three batches of five actual traditional Chinese medicine injections were analyzed using the developed method, and the results showed that the contents of Cu, As, Cd, Pb and Hg were all less than the limits. The method, proved to be easy to handle, rapid and sensitive, meets the method validation requirements, and was suitable for the determination of the heavy metals and harmful elements in five traditional Chinese medicine injections. It also can supply a reference for the determination of the elemental impurities in the other traditional Chinese medicine injections
Keywords: inductively coupled plasma mass spectrometry (ICP-MS);traditional Chinese medicine injections;heavy metals and harmful elements;direct dilution

關(guān)鍵詞：電感耦合等離子體質(zhì)譜法;中藥注射液;重金屬及有害元素;直接稀釋法