基于ICP-MS法的加味左金丸中无机元素分析

Analysis of inorganic elements in Jiawei Zuojin Pills by ICP-MS

目的通过电感耦合等离子体质谱(inductively coupled plasma mass spectrometry,ICP-MS)法建立加味左金丸中Cd、Pb、As、Hg、Co、V、Ni、Cu、Li、Sb、Ba、Mo、Sn、Cr、Na、Mg、Al、Ca、Ti、Mn、Fe、Zn、Ga、Se、Sr、Tl共计26种无机元素的测定方法。方法加味左金丸通过微波消解法处理后,根据相对分子质量的大小选择内标物,其中^(7)Li、^(23)Na、^(24)Mg、^(27)Al、^(40)Ca、^(48)Ti、^(51)V、^(52)Cr、^(55)Mn、^(56)Fe、^(58)Ni、^(59)Co、^(63)Cu、^(66)Zn、^(70)Ga、^(75)As、^(77)Se、^(86)Sr以^(72)Ge作为内标;^(95)Mo、^(114)Cd、^(118)Sn、^(121)Sb、^(137)Ba以^(115)In作为内标;^(202)Hg、^(205)Tl、^(208)Pb以^(209)Bi作为内标。对标准品溶液、空白溶液与供试品溶液进行分析,采用标准曲线法进行定量分析。通过ICP-MS法进行测定。结果26种无机元素线性的相关系数r≥0.9996,检出限为0.001~1.500μg/L,定量限为0.01~5.00μg/L,精密度与重复性试验的RSD均小于5%,平均回收率在82.64%~106.44%,RSD均小于5%。对3个厂家的12批样品进行了测定,26种元素的含量差异较大,其中Na、Mg、Ca、Fe 4种元素的含量比较高,均大于500μg/g,Cd、Pb、As、Hg、Co、Li、Sb、Mo、Sn、Cr、Se、Tl的含量比较低,均小于1μg/g。由结果可知,人体的常量元素,如Na、Mg、Ca的含量比较高,Cd、Pb、As、Hg等有害元素含量比较低。根据《中国药典》2020年版一部的要求,本品中Cd、Pb、As、Hg与Cu均符合规定。结论该方法快速、准确,可以用于加味左金丸中无机元素的测定。

Objective To establish a method for the simultaneous analysis of 26 inorganic elements in Jiawei Zuojin Pills(加味左金丸,JZP),including Cd,Pb,As,Hg,Co,V,Ni,Cu,Li,Sb,Ba,Mo,Sn,Cr,Na,Mg,Al,Ca,Ti,Mn,Fe,Zn,Ga,Se,Sr,Tl.Methods After JZP was treated by microwave digestion,the internal standard was selected according to the molecular weight,^(72)Ge was used as the internal standard for^(7)Li,^(23)Na,^(24)Mg,^(27)Al,^(40)Ca,^(48)Ti,^(51)V,^(52)Cr,^(55)Mn,^(56)Fe,^(58)Ni,^(59)Co,^(63)Cu,^(66)Zn,^(70)Ga,^(75)As,^(77)Se,and^(86)Sr;^(115)In was used as the internal standard for^(95)Mo,^(114)Cd,^(118)Sn,^(121)and^(137)Ba;^(209)Bi was used as the internal standard for ^(202)Hg,^(205)Tl and ^(208)Pb.The standard solution,blank solution and test solution were analyzed,and the quantitative analysis was conducted by standard curve method.It was determined by ICP-MS.Results The detection limits and quantification limits of 26 elements were in the range of 0.001-1.500μg/L and 0.01-5.00μg/L.The 26 trace elements showed the good linearity in the selected concentration ranges(r≥0.9996),with the average recovery from 82.64%to 106.44%,while their RSD was below 5%.Twelve batches of samples from three manufacturers were determined.The content difference of 26 elements was relatively large,among which the content of Na,Mg,Ca and Fe was relatively high,all of which were greater than 500μg/g,the contents of Cd,Pb,As,Hg,Co,Li,Sb,Mo,Sn,Cr,Se and Tl were relatively low,all less than 1μg/g.The results showed that the contents of major elements such as Na,Mg and Ca in human body were relatively high,and the contents of harmful elements such as Cd,Pb,As and Hg were relatively low.According to the requirements of Chinese Pharmacopoeia,Volume I,2020 edition,Cd,Pb,As,Hg and Cu in this product met the requirements.Conclusion The method is rapid and accurate,and can be used forthe quality control of inorganic elements in JZP.