ICP-MS检测十一味参芪胶囊中常见金属元素

Determination of Common Metal Elements in Eleven-ingredients Shenqi Capsules by Inductively Coupled Plasma Mass Spectrometry

目的建立电感耦合等离子体质谱(ICP-MS)检测十一味参芪胶囊常见金属元素的方法,了解十一味参芪胶囊中铁(Fe)、铬(Cr)、锰(Mn)、镍(Ni)、铜(Cu)、锌(Zn)、砷(As)、银(Ag)、镉(Cd)、锡(Sn)、锑(Sb)、钡(Ba)、铅(Pb)等常见金属元素含量。方法取十一味参芪胶囊3批,准确称取0.4 g,湿法消解至溶液清澈透明呈微黄色,定容至10 mL。采用在线内标,建立ICP-MS检测样品中常见金属元素的方法;通过有证参考物质榉木叶与茶叶验证方法的准确度和精密度;并对3批药品金属元素进行检测。ICP-MS射频功率:1350 W;Barbington雾化器;载气流速:1.4 mL·min-1;采样深度:8.5 mm;采集模式:Spectrum;样品提升速度:0.4 L·min-1。结果ICP-MS测定十一味参芪胶囊中常见13种金属元素线性相关系数均>0.9990;稳定性试验日内误差RSD在0.50%～4.56%之间,日间误差RSD在1.17%～5.03%之间。有证参考物质榉木叶与茶叶回收率高,精密度好:所测金属元素含量大于100 mg·kg-1时,回收率在95.8%～100.5%之间,RSD为1.82%～2.68%;含量在1～100 mg·kg-1间,元素回收率在86.0%～104.9%之间,RSD为1.70%～6.33%;含量在0.1～1 mg·kg-1间,元素回收率在97.1%～103.9%之间,RSD为2.51%～5.19%;含量小于0.1 mg·kg-1的元素,回收率在92.1%～110.0%之间,RSD在2.75%～14.48%之间,符合分析技术要求。依据本法检测3批药品,Pb、Cd、Sn、Sb、Ag、As含量均在1 mg·kg-1以下,Cr、Ni、Cu含量在1.3～4.6 mg·kg-1之间,Ba、Zn、Mn含量在17.2～25.7 mg·kg-1之间,Fe含量最高,在577～616 mg·kg-1之间。结论 3批十一味参芪胶囊中Cu、As、Cd、Pb符合国家中药材质量标准,Zn、Sn符合国家相关食品标准,其余元素未见中药材标准限值。除Ag、Ba未见《美国药典》规定的口服限量外,其余元素均符合《美国药典》规定的口服限量规定。

Objective To set up analysis method for common metal elements, ganese（Mn）, nickel（Ni）, euprum（Cu）, zinc（Zn）, arsenicum（As）, argentums（ stibine（Sb）, barium（Ba）, and plumbum（Pb）, in Eleven-ingredient Shengqi Caps ferrum（Fe）, chromium Ag）, ules, chromium（Cd）, stannum（Sn and to detect those elements the capsules. Methods Three batches of Eleven-ingredient Shengqi Capsules were randomly sampled and weighed indi- vidually into 0.4 g. The three weighed samples were digested by wet method with concentrated nitric acid（HNO3） into colorless or yellowish solution, the metered volume being 10 mL. Based on online internal standards, the analysis method for common metal elements in the samples was set up. The accuracy and precision of the analysis method was verified with certified reference materials lyophilised beech leave powder and tea leaves. Common metal elements in the three batches of samples were analysed by inductively coupled plasma mass spectrometry（ICP-MS）. The instrument parameters were below： radio frequency（RF） power at 1350 W, Barbington atomizer, carrier gas flow rate at 1.4 mL· min^-1, sampling depth at 8.5 mm, Spectrum collection mode, and sample lifting speed at 0.4 L·min^-1 Results Thelinear correlative coefficients for the common thirteen elements in the capsules were higher than 0.9990. The accuracy, precision and stability of the method were detected, and they all conformed to the analysis standard. RSD of within-day error was in the range of 0.50 %-4.56 %, and that of inter-day error was in the range of 1.17 %-5.03 %. Recoveries were 95.8 %-100.5 %（RSD being 1.82 %-2.68 %）, 86.0 %-104.9 %（RSD being 1.70 %-6.33 %）, 97.1%-103.9 % （RSD being 2.51%-5.19 %） and 92.1%-110.0 %（RSD being 2.75 %-14.48 %） when the contents of metals were higher than 100 mg·kg^-11, in the range of 1-100 mg·kg^-1, 0.1-1 mg·kg^-1 and lower than 0.1mg·kg^-1, respectively. Con- tents of Pb, Cd, Sn, Sb and Ag in the three batches of samples were lower than 1 mg·kg^-1, Cr, Ni and Cu in the range of 1.3-4.6 mg·kg^-1, Ba, Zn and Mn in the range of 17.2-25.7 mg·kg^-1, and Fe were the highest, in the range of 577-616 mg·kg^-1. Conclusion Contents of Cu, As, Cd, Pb in the three bathces of Eleven-ingredient Shengqi Cap sules meet the national quality standards of traditional chinese medical material（TCM）. Contents of Zn, Sn reach the national food quality standards. The standard contents limited of Cr, Mn, Ni, Ag, Sb and Ba in Chinese medicinal material have not been found in relative references. Except Ag and Ba, other detected elements fit the oral dose limited of United States Pharmacopoeia.