ICP-OES/ICP-MS技术研究枯矾及其伪品的差异特征元素及无机元素含量分布

目的:分析临床用枯矾及其伪品铵明矾炮制品的差异无机元素,并建立其特征图谱,为枯矾提供新的质量控制手段。方法:应用ICP-OES及ICP-MS测定枯矾和铵明矾炮制品中22种无机元素的含量,采用SPSS 16. 0软件对原始数据进行分层聚类分析,以SIMCA-P 13. 0软件配合t检验及秩和检验对差异性无机元素进行识别,建立枯矾与伪品的无机元素特征谱。结果:枯矾中主含K,Al等元素,伪品主含Al,Fe等元素;枯矾Cr,Sr,Mn含量相对较高,铵明矾炮制品Mn,Ti,Ga含量相对较高。其中枯矾中K元素含量约为伪品的205倍;相反,Fe,Ti,Mn,Ga等元素,伪品的平均含量远高于枯矾,分别约为枯矾平均含量的33,46,38,27倍。聚类分析将18个样品聚类为枯矾和铵明矾炮制品两大类。共筛选出18种含量具有显著性差异(P 0. 05)的元素,分别为Be,Mg,Al,K,Ti,V,Mn,Fe,Co,Ni,Cu,Ga,As,Sn,Sb,Hg,Tl,Pb。建立了枯矾、伪品枯矾含21种无机元素特征谱。结论:该分析方法可用于枯矾的质量控制。

Research on Differential Feature Elements and Characteristic Spectrum of Inorganic Elements Between Calcined Alumen and Its Counterfeit Processed Products Based on ICP-OES/ICP-MS

Objective: To provide the new quality control means for Alumen by investigating the elemental differences between calcined Alumen and its counterfeit processed products of ammonium alum, and establishing their characteristic chromatogram. Method: The contents of 22 inorganic elements both in calcined Alumen and processed products of ammonium alum were determined by means of inductively coupled plasma (ICP)-optical emission spectrometer-mass spectrometry (ICP-OES/ICP-MS),SPSS 16.0 was used for cluster analysis (CA) while SIMCA-P 13.0 with t-test and Rank-Sum test was used to identify the differential inorganic elements. In addition, the characteristic spectrum of the inorganic elements for calcined Alumen and counterfeit calcined alumen were established. Result: Calcined Alumen had highest contents of K and Al while counterfeit calcined Alumen has highest contents of Al and Fe;Cr,Sr,and Mn contents in calcined Alumen were relatively higher,while Mn,Ti,and Ga contents in processed products of ammonium alum were relatively higher. The content of K in calcined Alumen was about 205 times of that of counterfeit products. On the contrary,the average contents of Fe,Ti,Mn and Ga in counterfeit products of ammonium alum were much higher than those in calcined Alumen,33,46,38, 27 times, respectively. A total of 18 samples were clustered into two categories in CA:calcined Alumen and processed products of ammonium alum. 18 inorganic elements showed significant difference in contents(P<0.05),Be, Mg,Al,K,Ti,V,Mn,Fe,Co,Ni,Cu,Ga,As,Sn,Sb,Hg,Tl,and Pb respectively. Characteristic spectrum of 21 inorganic elements in calcined Alumen and counterfeit calcined Alumen were established. Conclusion: This method can be used for quality control of calcined Alumen.