基于ICP-MS法的桂枝茯苓胶囊中无机元素分析

Analysis of inorganic elements in Guizhi Fuling Capsules by ICP-MS

目的采用电感耦合等离子体质谱(ICP-MS)法建立桂枝茯苓胶囊(GFC)中29种无机元素(Li、Be、B、Na、Mg、Al、Ca、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Ga、As、Se、Sr、Mo、Cd、Sn、Sb、Ba、Hg、Tl、Pb、Bi)的测定方法。方法 GFC样品以浓硝酸为消解试剂经微波消解后,以Ge、In元素为内标,以灌木枝叶标准物质作为质控标准物质,采用ICP-MS法测定其中29种无机元素含量。结果待检测的29种无机元素在各的自线性范围内线性关系良好,r≥0.999 4;各元素的检出限在0.012~4.105μg/L,定量限在0.045~14.500μg/L,平均加样回收率在79.88%~105.76%,RSD≤4.55%。测定的12批样品中Ca、Na、Mg含量较高,均超过300μg/g;Fe、Mn、Sr含量也相对较高,而有害元素Be、As、Cd、Sb、Hg、Tl、Bi含量相对较低,均在0.030μg/g以下。结论该方法操作简便,分析速度快,灵敏度高,适用于GFC中无机元素的测定。

Objective To establish a method for the simultaneous analysis of 29 inorganic elements in Guizhi Fuling Capsules（GFC）, including Li, Be, B, Na, Mg, Al, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Sr, Mo, Cd, Sn, Sb, Ba, Hg, Tl, Pb, and Bi. Methods The sample of GFC was digested by microwave with concentrated nitric acid, calibrated by internal standard elements, such as Ge and In, with bush branches and leaves as the controlled reference standard, and inlet into ICP-MS to analyze the contents of 29 inorganic elements. Results The detection limits and quantification limits of the 29 elements were in the range of 0.012—4.105 μg/L and 0.045—14.500 μg/L. The 29 trace elements showed the good linearity in the selected concentration ranges（r ≥ 0.999 4）, with the average recovery from 79.88% to 105.76%, while their RSD was below 4.55%. In the 12 batches of samples, the quantities of Ca, Na, and Mg were higher than 300 μg/g. The quantities of Fe, Mn, and Sr were also relatively high, while the amount of Be, As, Cd, Sb, Hg, Tl, and Bi was relatively low, which was below 0.030 μg/g. Conclusion The method is simple, rapid, and accurate, and can be used for the quality control of trace elements and heavy metals in GFC.