红外光谱与X射线光谱结合电感耦合等离子体质谱对蒙药禹粮土质量控制方法的研究  

Infrared Spectroscopy and X-Ray Spectroscopy Combined With Inductively Coupled Plasma Mass Spectrometry for Quality Control of Mongolian Medicine Yu Grain Soil

作　　者：朱禹奇 张鑫 杜盼盼 刘舒[1] 张贵鑫 关松磊[2] 郑重[1] ZHU Yu-qi;ZHANG Xin;DU Pan-pan;LIU Shu;ZHANG Gui-xin;GUAN Song-lei;ZHENG Zhong(Laboratory of Chemical Biology,Changchun Institute of Applied Chemistry,Chinese Academy of Sciences,Changchun 130022,China;School of Life Sciences,Jilin Agricultural University,Changchun 130118,China)

机构地区：[1]中国科学院长春应用化学研究所化学生物学实验室,吉林长春130022 [2]吉林农业大学生命科学学院,吉林长春130118

出　　处：《光谱学与光谱分析》2023年第10期3163-3169,共7页Spectroscopy and Spectral Analysis

基　　金：国家重点研发计划项目(2018YFC1708202);内蒙古自治区科技重大专项课题(2019ZD004);国家级大学生创新创业训练计划项目(202210193011)资助。

摘　　要：禹粮土在蒙药中使用历史悠久,但由于缺乏质量指标,质量得不到保证,极大地影响了其应用。采用FTIR、XRD及ICP-MS法测定9批禹粮土样品的物质组成、结构及元素含量,探究禹粮土的质量控制方法。结果显示,9批生品禹粮土在FTIR波数为3696、3620、1621、1164、913、797、778、695、537和469 cm^(-1)存在共有峰,其中797 cm^(-1)为Fe—O—Fe伸缩振动吸收峰,695 cm^(-1)为Fe—O—Fe对称伸缩振动吸收峰,469 cm^(-1)为Si—O—Si特征峰。禹粮土的XRD主要物相为Fe_(2)O_(3)和SiO_(2),并有Al 4(OH)8(Si_(4)O_(10))、K(Al_(4)Si_(2)O_(9))(OH)_(3)、CaCO_(3)以及一些磷酸盐等其他矿物伴生。生品禹粮土XRD衍射光谱的衍射角度2θ中24.870、33.116、38.436为Fe 2O 3的X射线衍射峰,衍射角度2θ中20.837、26.608、36.512、39.437、40.235、42.423、45.759、50.102和54.827为SiO_(2)的X射线衍射峰。通过ICP-MS对禹粮土中元素进行测定,结果显示,禹粮土的元素组成十分丰富,且不同产地及不同批次元素含量差异较大;禹粮土中Fe元素含量最高,其均值为56.9 mg·g^(-1),限量标准为生品禹粮土全铁量不低于4.55%,生品禹粮土中Pb、As、Hg、Cu和Cd元素限量不得超过50μg·g^(-1)。元素聚类结果显示,在欧式距离10~15将样品S3、S5、S6、S7分为一类,将S1、S2、S4、S8、S9分为一类,聚类分析结果表明,不同产地禹粮土元素组成和含量存在差异,可以将河南与内蒙古产地的禹粮土分为一类,山东和青海的禹粮土分为一类。生品禹粮土主成分分析筛取了4个主成分,累计贡献率为90.462%,筛选K、Sr、Be、As作为禹粮土样品的特征元素。Yu grain soil has been used in Mongolian medicine for a long time,but due to the lack of quality indicators,the quality cannot be guaranteed,which significantly affects its application.In this study,the material composition,structure and element content of 9 batches of Yu grain soil samples were determined by FTIR,XRD and ICP-MS,and the quality control method of Yu grain soil was explored.The results showed that the FTIR wavelengths of 9 batches of raw Yu grain soil were 3696,3620,1621,1164,913,797,778,695,537 and 469 cm^(-1)have common peaks,of which 797 cm^(-1)is Fe—O—Fe stretching absorption peak,695 cm^(-1)is Fe—O—Fe symmetrical stretching absorption peak,469 cm^(-1)is the characteristic peak of Si—O—Si.The main phases of XRD of Yu grain soil are Fe_(2)O_(3)and SiO_(2),and are accompanied by other minerals such as Al_(4)(OH)_(8)(Si_(4)O_(10)),K(Al_(4)Si_(2)O_(9))(OH)_(3),CaCO_(3)and some phosphates.The diffraction angles 24.870,33.116,38.436 in the XRD diffraction spectrum of raw product Yu grain soil are the X-ray diffraction peaks of Fe_(2)O_(3),and the diffraction angles 20.837,26.608,36.512,39.437,40.235,42.423,45.759,50.102,54.827 are SiO_(2)X-ray diffraction peaks.ICP-MS determined the elements in Yu grain soil.The results showed that the element composition of Yu grain soil was very rich,and the element content of different production areas and batches were quite different.The content of Fe in Yu grain soil was the highest,and its average value was 56.9 mg·g^(-1).The limit standard is that the total iron content of raw Yu grain soil should not be less than 4.55%,and the limit of Pb,As,Hg,Cu and Cd elements in raw Yu grain soil should not exceed 50μg·g^(-1).The element clustering results show that the samples S3,S5,S6,and S7 are classified into one class at the Euclidean distance of 10—15,and the samples S1,S2,S4,S8,and S9 are classified into one class,the results of cluster analysis showed that there were differences in the element composition and content of Yu grain soil in different

关 键 词：禹粮土 红外光谱 X射线衍射光谱 等离子体质谱 质量控制 

分 类 号：O657.63[理学—分析化学]