【摘要】 建立电感耦合等离子体质谱法(ICP-MS)测定复方蒲公英注射液、野菊花注射液、肿节风注射液、白花蛇舌草注射液和夏天无注射液中铜(Cu)、砷(As)、镉(Cd)、铅(Pb)和汞(Hg)5种重金属及有害元素含量的方法。样品用2%硝酸(V/V)直接稀释,以72Ge、115In、185Re为内标,采用ICP-MS测定溶液中元素含量。方法学验证表明:Cu、As、Cd、Pb在0.5～50μg/L和Hg在0.5～10μg/L的质量浓度范围内线性关系良好(r2>0.999);低、中、高3种浓度水平,复方蒲公英注射液、夏天无注射液、肿节风注射液、野菊花注射液、白花蛇舌草注射液中5种元素的平均回收率(n=3)分别为90.7%～121.2%、83.4%～119.9%、90.8%～116.3%、86.4%～109.0%、85.0%～118.0%,重复性RSD(n=3)分别为1.4%～9.8%、0.2%～6.7%、0.4%～7.4%、0.6%～10.0%、0.1%～11.1%;5种注射液中Cu、As、Cd、Pb、Hg的LOQ分别为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,满足方法学验证的要求。各3批次实际中药注射液样品的测试结果表明,5种元素含量均小于限量值,说明其安全风险较小。方法操作简便、快速、灵敏度高、准确度好,适合5种注射液中的Cu、As、Cd、Pb、Hg等有害元素含量的测定,为其他中药注射液中元素杂质分析方法的建立提供参考。更多还原

【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(72 Ge, 115 In, 185 Re) 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 than0.999. 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更多还原