藏药佐太的粉末X射线衍射指纹图谱及微观结构形态研究  

Fingerprint of X-ray diffraction of Tibetan medicine Zuotai and its study on microstructure and morphology

作　　者：干泓侠 冯楠 李远飞 顾健 韩泳平 GAN Hong-xia;FENG Nan;LI Yuan-fei;GU Jian;HAN Yong-ping(College of Pharmacy,Southwest Minzu University,Chengdu 610041,China)

机构地区：[1]西南民族大学药学院,四川成都610041

出　　处：《中草药》2022年第11期3321-3328,共8页Chinese Traditional and Herbal Drugs

基　　金：国家自然科学基金资助项目(82174083);西南民族大学中央高校基本科研业务费专项资金项目资助(ZYN2022039)。

摘　　要：目的建立藏药佐太的X射线衍射(X-ray diffraction,XRD)指纹图谱;测定佐太中主要物相的成分及含量;检测佐太的微观结构。方法采用XRD法对15批佐太样品进行分析,建立佐太样品的指纹图谱;通过全谱拟合对佐太样品进行定性和定量分析;运用扫描电子显微镜(SEM)分析佐太微粒的微观特征;运用K值法和滴定法测定佐太中主要成分HgS的含量。结果建立了佐太的XRD指纹图谱,相似度均达90%以上。确定9个共有峰,2、4~7号共有峰为HgS的特征峰,1、3号共有峰为S的特征峰;全谱拟合结果显示,佐太中主要存在立方晶系HgS(空间群为F-43m 216)、六方晶系HgS(空间群为P3221154)以及斜方晶系S8(空间群为Fddd 70),其质量分数分别为56.87%、3.570%、39.56%;SEM观测表明佐太的形态为松散的团簇状球状颗粒,粒径大致为200~800 nm。K值法测得15批样品中HgS的总含量平均值为56.90%,与滴定法所测结果基本一致。结论建立的XRD指纹图谱专属性较强,可作为其质量评价的依据;K值法的应用简易便捷、准确度高,为佐太的含量测定提供重要方法。Objective To establish the X-ray diffraction(XRD)fingerprint of Zuotai,determine the composition and content of main phases in it and detect the microstructure of these simples.Methods XRD was used to analyze 15 batches of Zuotai samples,and the fingerprint of Zuotai samples was established;Full spectrum fitting was used for qualitative and quantitative analysis of Zuotai samples;Scanning electron microscope(SEM)was used to analyze the micro characteristics of Zuotai particles,k-value method and titration method were used to determine the content of HgS,the main component of Zuotai.Results Fingerprint of Zuotai was established,and the similarity was more than 90%.There were nine common peaks,peaks 2,4—7 were the characteristic peaks of HgS,and peaks 1 and 3 were the characteristic peaks of S.The full spectrum fitting analysis of Zuotai showed that there were mainly cubic-HgS(space group F-43m 216),hexagonal-HgS(space group P3221154)and orthorhombic S8(space group Fddd 70),and their contents were 56.87%,3.573%and 39.56%respectively;Scanning electron microscopy(SEM)showed that the morphology of Zuotai was loose cluster spherical particles,and the particles size about 200-800 nm.The average content of HgS in 15 batches of samples measured by K-value method is 56.90%.Conclusion The established X-ray diffraction fingerprint has strong specificity and can be used as the basis for its quality evaluation;The application of K-value method is simple,convenient and accurate,which provides an important method for the content determination of Zuotai.

关 键 词：藏药 佐太 X射线衍射 指纹图谱 全谱拟合 微观结构 K值法 滴定法 HGS 立方晶系 六方晶系 斜方晶系 质量评价 

分 类 号：R283.6[医药卫生—中药学]