[关键词]
[摘要]
目的 采用电感耦合等离子体质谱(ICP-MS)法建立九味熄风颗粒中25种重金属及微量元素(Li、Mg、Cd、Sn、Al、Mn、Fe、Ti、V、Co、Zn、Ga、Cr、Ni、Tl、Pb、Cu、As、Be、B、Sb、Ba、Sr、Hg、Bi)的测定方法.方法 九味熄风颗粒样品经微波消解后,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法进行测定.结果 检测的25种元素线性关系良好,相关系数R2≥0.999 2,各元素的检出限在0.009~16.051 μg/L,回收率在70.75%~107.66%,RSD≤6.44%.测定的6批样品中Cr、Sn、Hg、Pb均未检出,Tl、Cd、As、Cu的量均较低或未检出,Cd≤0.011 μg/g,Cu≤0.373 μg/g,Tl≤0.021 μg/g,As≤0.571 μg/g.结论 该方法操作简便,分析速度快,灵敏度高,适用于九味熄风颗粒中重金属及微量元素的测定.
[Key word]
[Abstract]
Objective To establish a method for the simultaneous analysis of 25 trace elements and heavy metals in Jiuwei Xifeng Granules, including Li, Mg, Cd, Sn, Al, Mn, Fe, Ti, V, Co, Zn, Ga, Cr, Ni, Tl, Pb, Cu, As, Be, B, Sb, Ba, Sr, Hg, and Bi. Methods The samples, digested via microwave, calibrated by internal standard elements, such as Ge and In, with bush branches and leaves as the controlled reference standard, were inlet into ICP-MS to analyze the contents of the 25 trace elements and heavy metals. Results The detection limits of the 25 elements were in the range of 0.009-16.051 μg/L. The 25 trace elements and heavy metals showed the good linearity in the selected concentration ranges (R2 ≥ 0.999 2), with the average recovery from 70.75% to 107.66%, while their RSD was below ≤ 6.44%. Cr, Sn, Hg, and Pb were not detected in the six batches of samples, and the contents of Tl, Cd, As, and Cu were lower or not detected. Cd ≤ 0.011 μg/g, Cu ≤ 0.373 μg/g, Tl ≤ 0.021 μg/g, As ≤ 0.571 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 Jiuwei-xifeng Granules.
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[基金项目]
现代中药创新集群与数字制药技术平台(2013ZX09402203)