基于粉末X射线衍射和电子自旋共振技术对全蝎的检测  

Detection of Scorpion based on Powder X-ray Diffraction and Electron Spin Resonance

作　　者：项太平 张进 路大勇[1] 刘巧丽[1] XIANG Taiping;ZHANG Jin;LU Dayong;LIU Qiaoli(Research Center for Materials Science and Engineering,Jilin Institute of Chemical Technology,Jilin 132022,China)

机构地区：[1]吉林化工学院材料科学与工程研究中心,吉林吉林132022

出　　处：《吉林化工学院学报》2022年第5期13-19,共7页Journal of Jilin Institute of Chemical Technology

基　　金：吉林省自然科学基金自由探索重点项目(YDZJ202101ZYTS125);吉林省中医药科技委托重点项目(2020037)。

摘　　要：目的:建立了一种粉末X射线衍射(PXRD)和电子自旋共振(ESR)技术联用的无损检测方法,对随机采购的10种市售全蝎进行质量控制和微量元素来源鉴定.方法:运用PXRD谱模拟方法获得全蝎的特征标记峰,以鉴定NaCl的含量及来源;通过ESR谱分析其中的一些微量元素.结果:(1)随机采购的10种市售全蝎体内的NaCl含量为4.35~13.33 g/100 g,含矾量为3.73~11.27 g/100 g,含硅量为2.38~4.40 g/100 g;(2)全蝎中的晶态PXRD峰起源于NaCl晶体和Na_(2)SO_(4)晶体,且无机盐Na_(2)SO_(4)是全蝎自身含有的,而NaCl是炮制过程中带入的;(3)ESR技术检测出g=2.003的信号和具有六线特征的Mn^(2+)信号;(4)溶解实验后烘干的全蝎存在g=4.3弱的宽信号Fe^(3+)和g=2.17对称信号Cu^(2+),说明Fe^(3+)和Cu^(2+)是全蝎自身含有的金属离子;(5)电感耦合等离子发射光谱(ICP)实验和溶解实验证实了全蝎中的Mn^(2+)起源于食盐,而非全蝎自身.结论:PXRD和ESR技术联合应用,可建立一种无损检测技术,该技术可对全蝎进行质量控制,并对过渡金属元素的来源进行检测.Objective:A non-destructive testing technology combining powder X-ray diffraction(PXRD)and electron spin resonance(ESR)was established to make the quality control and identify the sources of trace elements of 10 commercially available scorpions.Methods:The characteristic marker peaks of Scorpion were obtained by PXRD spectrum simulation method to identify the content and source of NaCl.Some of the trace elements were analyzed by ESR technique.Results:(1)The NaCl content of 10 randomly purchased commercial scorpions was 4.35~13.33 g/100 g,the alum content was 3.73~11.27 g/100 g,the silicon content was 2.38~4.40 g/100 g.(2)The PXRD peaks in the scorpion originate from sodium chloride(NaCl)crystal and sodium sulfate(Na_(2)SO_(4))crystal.The inorganic salt Na_(2)SO_(4) originates from the scorpion itself,while NaCl is added through the concocting process.(3)There is a signal with g=2.003 and a Mn^(2+)signal with six-line characteristics in the ESR spectrum.(4)In the ESR test,the dried scorpion after the dissolution experiment appears a weak broad signal of g=4.3 and a signal of g=2.17 which belongs to the signal of Fe^(3+)and Cu^(2+),respectively.This phenomenon indicates that Fe^(3+)and Cu^(2+)ions are contained in the scorpion itself.(5)Atom emission test on the dissolution-experiment-acqueous solution confirmed that the Mn^(2+)in the scorpion originated from salt,rather than the scorpion itself.Conclusion:The combined application of PXRD and ESR technology can establish a non-destructive test technology,which can be used for the quality control of Scorpion and the source of transition metal elements.

关 键 词：全蝎 粉末X射线衍射 电子自旋共振 盐分 质量控制 过渡金属离子 

分 类 号：R282.74[医药卫生—中药学]