基于ICP-MS对肝爽颗粒中26种无机元素的分析及质量评价

Quality evaluation of 26 inorganic elements in Ganshuang granules based on ICP-MS

目的采用微波消解-电感耦合等离子体质谱(ICP-MS)法对肝爽颗粒中无机元素组成进行分析并建立相关指纹图谱,为产品的质量均一性和安全性评价提供参考。方法以硝酸为消解试剂,Ge、In元素为内标,采用ICP-MS法定量测定肝爽颗粒中无机元素的含量,通过Heatmaps图谱,Pearson相关系数对结果进行分析;通过无机元素指纹图谱、聚类分析结合主成分分析(PCA)对质量均一性进行评价。结果肝爽颗粒中无机元素以K、Mg、Na、Ca、Al、Fe、Mn为主,且不同元素含量之间存在一定相关。Cu、As、Cd、Hg、Pb这五种重金属元素的限量符合相关限度规定。不同批次的样品均有相似的峰形,且不同无机元素的多寡顺序趋于一致。从指纹图谱相似度、聚类分析、PCA结果来看,肝爽颗粒中无机元素的质量均一性较好,主要特征元素为Mg、K、Ca、Mo、Tl、Cd、Se、Zn。结论该方法操作简便、灵敏度高、准确可靠,适用于肝爽颗粒中无机元素的测定。通过对肝爽颗粒中无机元素的分析,可以为肝爽颗粒的质量均一性和安全性评价提供参考。

Objective To analyze the inorganic elements composition in Ganshuang granules(GSG)by microwave digestion-inductively coupled plasma spectrometer(ICP-MS)method,establish the fingerprint of inorganic elements,and provide the research basis for the quality uniformity and safety evaluation.Methods Nitric acid was used as the digestion reagent,the GSG samples calibrated by internal standard elements,such as Ge,and In.The content of inorganic elements was determined by ICP-MS.The results were analyzed by Heatmaps and Pearson correlations.The quality uniformity was evaluated by inorganic elemental fingerprint,cluster analysis and principal components analysis(PCA)for different batches of GSG.Results The main inorganic elements in GSG included K,Mg,Na,Ca,Al,Fe and Mn,and there was a certain correlation among different elements.The content of 5 heavy metal elements,including Cu,As,Cd,Hg,and Pb,were below the limit of heavy metals and harmful elements.The reference fingerprint of inorganic elements in GSG was generated with the average and median methods.Different batches of samples had similar peak shape,and the content of inorganic elements content in different orders tended to be consistent.The results of fingerprint similarity,cluster analysis,and PCA showed that the inorganic elements showed good quality uniformity,and Mg,K,Ca,Mo,Tl,Cd,Se,and Zn might be the characteristic elements in GSG.Conclusion The method is simple,rapid,accurate,and reliable,and can be used in the content determination of inorganic elements in GSG,which provide a certain reference for uniformity,safety evaluation of GSG.