微波消解ICP-MS法测定清血八味片中32种无机元素

Determination of 32 kinds of inorganic elements in Qingxue Bawei Tablets by inductively coupled plasma mass spectrometry with microwave digestion

目的采用微波消解-电感耦合等离子体质谱(ICP-MS)法建立清血八味片中Be、B、Na、Mg、Al、P、K、Ca、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Ga、As、Se、Rb、Sr、Mo、Ag、Cd、Sn、Sb、Cs、Ba、Hg、Tl、Pb共32种无机元素的测定方法,建立清血八味片无机元素指纹谱并分析其特征元素。方法以硝酸加过氧化氢体系为消解试剂,样品经微波消解后,以~6Li、Sc、Y、Rh、In、Ho、Bi、Th元素为内标元素,采用ICP-MS法测定清血八味片中无机元素的量,绘制无机元素量分布曲线图,并用SPSS 19.0软件对数据进行主成分分析(PCA)。结果测定的各元素线性关系良好,r≥0.999 5,各元素的检测限在0.001～6.390μg/L,精密度、稳定性和重复性试验的RSD均符合定量分析要求;加样回收率为94.36%～105.47%,RSD 1.53%～4.56%。通过无机元素量分布曲线分析建立了清血八味片的无机元素指纹谱,不同批次的样品均有相似的峰形,且不同无机元素量的多寡顺序趋于一致。经PCA筛选出清血八味片主要特征无机元素为Co、As、Ba、Ca、Sb、Ti、Ni、Fe、Cs、Se、P、Al、K。测定的样品中检测出Pb、Cd、As、Hg、Cu,5种重金属元素的量均低于《中国药典》2015年版的限度要求。结论该方法简便、快速、准确,适用于同时测定清血八味片中32种无机元素。通过对清血八味片无机元素的分析,可以为清血八味片的质量控制、安全性评价及临床使用提供一定参考。

Objective To establish an inductively coupled plasma mass spectrometry （ICP-MS） with microwave digestion method for the determination of 32 kinds of inorganic elements in Qingxue Bawei Tablets （QBT）, including Be, B, Na, Mg, Al, P, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, St, Mo, Ag, Cd, Sn, Sb, Cs, Ba, Hg, TI, and Pb, in order to establish the fingerprint chromatogram of inorganic elements and analyze characteristic elements. Methods The samples with nitric acid and hydrogen peroxide system as digestion reagents were digested via microwave, calibrated by internal standard elements, such as 6Li, Sc, Y, Rh, In, Ho, Bi, and Th. The contents of 32 inorganic elements were analyzed by ICP-MS. The content distribution curve of inorganic elements was plotted. And the principal components were analyzed with the SPSS 19.0 software. Results The 32 inorganic elements showed good linearity in the selected concentration ranges, with the correlation coefficients over 0.999 5. The detection limits of the 32 elements were in the range of 0.001--6.390 p^g/L. The RSD values of precision, stability, and repeatability all met the demands of quantitative analysis. The recovery was 94.36%--105.47%, while their RSD was 1.53%--4.56%. The fingerprint ehromatogram was established by the content distribution curve of inorganic elements. Different batches of samples were similar peak shape, and the amount of inorganic elements content in different order tend to be consistent. The results of principal component analysis showed that Co, As, Ba, Ca, Sb, Ti, Ni, Fe, Cs, Se, P, A1, and K might be the characteristic elements in QBT. The content of five heavy metals （Pb, Cd, As, Hg, and Cu） was under the limit requirements of Chinese Pharmacopoeia （2015）. Conclusion The method is simple, rapid, and accurate, and it can be used for the content determination of inorganic elements in QBT. The analysis of inorganic elements can provide certain reference for the quality control, safety evaluation, and clinical application of QBT.