六种钙类矿物药元素谱的X射线荧光光谱法无标样分析

Standard-less Analysis of Six Kinds of Calcium Mineral Drug Elements by X-Ray Fluorescence Spectrometry

目的：检测6种钙类矿物药的元素谱,尝试建立一种粉末状矿物药快速分析和同质性评价的方法。方法：将石膏、钟乳石、花蕊石、紫石英、龙骨、石燕药材粉碎至200目粉末后压片制样,应用X-射线荧光光谱仪的无标样分析方法,从氧到铀元素范围内进行元素谱扫描;以K,L,M谱线强度的平方根为纵坐标,2θ角为横坐标,将匹配后的元素标在图谱上,直观表征矿物药元素谱信息。结果：从6种钙类矿物药中共检出Al,Ca,Er,F,Fe,Ga,K,Mg,Mn,Mo,Na,Nb,O,P,Rb,S,Si,Sr,Ti,W,Y,Zr,Zn,Re,Ba共25种元素;同种矿物药的元素谱较稳定,不同品种间差异明显,其中Ca,F,O,P,S,Si等元素的含量变化较大,Al,Er,Fe,Ga,K,Mo等变化较小;性状特征不符合的3份石膏和1份紫石英,其含量也不符合2015年版《中国药典》要求。结论：X射线荧光光谱法具有操作简单,多元素同时分析、绿色环保等优势,能快速、简便获得矿物药的元素谱信息,可用于粉末状矿物药同质性分析和鉴别。

Objective：To study the element spectra of six kinds of calcium mineral drugs,in order to establish a rapid and environmental friendly analytical method to identify the authenticity and quality of mineral drugs powder,including the similar composition samples.Method：In this experiment,samples of Gypsum Fibrosum,Stalactitum,Ophicalcitum,Fluoritum,Os Draconis and Spirifer were crushed to 200-mesh powder.Afterwards the samples were pressed into directly pellets,and determined by X-ray fluorescence standard-less quantitative analysis method.All of the samples were measured within the scope of elements from oxygen to uranium.A method for characterizing the spectral characteristics of mineral elements were established,with the square root of K,L,M line intensity as the vertical coordinate and 2θ angle as the horizontal coordinate.The matched element spectral line coordinates were drawn on the spectra,so as to visually identify the elemental characteristics of medicinal materials.Result：From the six kinds of calcium mineral drug,25 elements,namely Al,Ca,Er,F,Fe,Ga,K,Mg,Mn,Mo,Na,Nb,O,P,Rb,S,Ba,Si,Sr,Zr,Ti,W,Y,Zn and Re,were detected.The element spectra of the same kind calcium mineral drugs were relatively stable,the element spectra of different medicinal materials were obviously different.Among them,the content of Ca,F,O,P,S,Si varied widely,with small changes in Al,Er,Fe,Ga,K,Mo.The content of three Gypsum Fibrosum samples and one Fluoritum sample did not meet the requirement of 2015 edition Chinese Pharmacopoeia.Conclusion：Compared with other methods,X-ray fluorescence spectrometry has the advantages of simple operation,simultaneous analysis of multi-elements and environmental friendliness.It can quickly and easily obtain the elements spectra information of mineral drugs and identify the homogeneity of mineral drug powder.