摘要
目的：建立采用电感耦合等离子体质谱法（ICP-MS）测定中药材侧柏叶中18种重金属及微量元素（Pb，TI，Hg，Dy，Ba，Sb，Sn，Cd，Ag，Mo，Se，As，Cu，Ni，Mn，Cr，A1，Be，Ge，In）的方法，该方法的建立对全面修订完善侧柏叶质量标准，提高侧柏叶质量控制水平提供实验基础。方法：侧柏叶样品经微波消解后，18种元素中质量〈100的元素采用Ge作为内标，质量〉100的元素采用In作为内标，采用ICP-MS法进行测定。结果：检测的Pb，TI，Hg，Dy，Ba，sb，sn，cd，Ag，Mo，Se，As，Cu，Ni，Mn，cr，Al，Be18种元素线性关系良好．相关系数R。≥0．9746。各元素的检出限在0．224-1．792μg·L^-1，回收率在81．0％～117．1％。测定来自不同产地63批侧柏叶样品，Hg，Cu，Cd，Sb4种元素的量均较低，As均未检出，Ba有部分样品超出限度要求，Pb绝大部分样品超出限度要求，Al超出限度范围较高，分析测定结果，Ni，Cr，Mn，A1，Cu，Ba是侧柏叶无机元素的主成分，可作为特征元素，来自不同产区的侧柏叶样品表现出一定的聚类性特征。结论：建立的方法操作简便，分析速度快，灵敏度高，内标法更能提高测定结果的精密度和准确性，该方法适用于中药材侧柏叶中重金属及微量元素的测定。
Objective： To establish a method for the simultaneous determination and analysis of 18 trace elements and heavy metals in Platycladi Cacumen, including Pb, TI, Hg, Dy, Ba, Sb, Sn, Cd, Ag, Mo, Se, As, Cu, Ni, Mn, Cr, Al, Be, Ge and In by using Inductively Coupled Plasma Mass Spectrometry （ICP- MS）, and provide an experimental basis for revising and improving the quality standard of the Platycladi Cacumen and improving the quality control of the Platycladi Cacumen. Method： After the samples were digested via microwave, Ge was used as the internal standard for the elements with the mass number of less than 100, and In was used as the internal standard for the elements with the mass number of more than 100 to analyze the contents of the 18 trace elements and heavy metals by using ICP-MS. Result： The detection limits of the 18 elements were in the range of 0. 224-1. 792 μg · L-1. The 18 trace elements and heavy metals showed the good linearity in the selected concentration ranges （R2 ≥ 0.974 6 ）, with the average recovery from 81.0%-117. 1%. In the determination of 63 batches of Platycladi Cacumen samples from different regions, four elements of Hg, Cu, Cd and Sb were low, As was not detected, some of Ba samples exceeded the limit, most of Pb samples was beyond the limit, A1 was far beyond the limit; Ni, Cr, Mn, A1, Cu and Ba were the main inorganic elements in Platycladi Cacumen, whcih can be used as the characteristic elements; and Platycladi Cacumen samples from different regions showed some clustering characteristics. Conclusion： The established method is simple with fast analysis and high sensitivity; the internal standard method can improve the precision and accuracy of test results, and the method is suitable for determination of heavy metals and trace elements in Platycladi Cacumen.
作者
张平
马潇
张明童
李冬华
杨静
王娟弟
杨平荣
王晓琳
ZHANG Ping1,2 , MA Xiao1,2 , ZHANG Ming-tong1,2 , LI Dong-hua1,2 , YANG Jing1,2 , WANG Juan-di1,2, YANG Ping-rong1,2, WANG Xiao-lin3,4.(1. Gansu Institute for Drug Control, Lanzhou 730070 China ; 2. Gansu Tibetan Medicine in the Examination Engineering Laboratory, Lanzhou 730070, China; 3. Gansu Provincial Hospital of Traditional Chinese Medicine （TCM） , Lanzhou 730050, China; 4. Gansu Institute of TCM, Lanzhou 730050, China)
出处
《中国实验方剂学杂志》
CAS
CSCD
北大核心
2018年第7期75-81,共7页
Chinese Journal of Experimental Traditional Medical Formulae
基金
名贵中药资源可持续利用能力建设项目(2060302-1508-13)
作者简介
张平，主管中药师，从事中药材鉴定与检验，中药材藏药质量标准控制和评价，Tel：0931-7822987，E-mail：58735870@qq．com;王晓琳，硕士，执业中药师，主管中药师，从事中药炮制及制剂质量标准研究，E-mail：253656393@qq．com
