微波消解-ICP-MS法测定不同工艺鲜竹沥中28种元素含量  

Determination of 28 elements in Xianzhuli under different processes by microwave digestion and ICP-MS

作　　者：朱迪 汪元亮 任琦 肖小武 常亮 郎淑琴 李灿灿 付辉政 ZHU Di;WANG Yuan-liang;REN Qi;XIAO Xiao-wu;CHANG Liang;LANG Shu-qing;LI Can-can;FU Hui-zheng(Jiangxi University of Traditional Chinese Medicine,Nanchang 330004,China;Jiangxi Provincial Institute for Drug Control,National Medical Products Administration Key Laboratory of Quality Evaluation of Traditional Chinese Patent Medicine,Jiangxi Provincial Engineering Research Center for Drug and Medical Device Quality,Nanchang 330029,China)

机构地区：[1]江西中医药大学,南昌330004 [2]江西省药品检验检测研究院,国家药品监督管理局中成药质量评价重点实验室,江西省药品与医疗器械质量工程技术研究中心,南昌330029

出　　处：《药物分析杂志》2024年第12期2114-2126,共13页Chinese Journal of Pharmaceutical Analysis

基　　金：江西省重大科技研发专项“揭榜挂帅”企业需求类项目(20223AAG2020)。

摘　　要：目的:采用电感耦合等离子体质谱法(ICP-MS法)测定鲜竹沥中28种元素的含量,考察干馏和火制2种不同工艺的鲜竹沥元素分布情况,并评价企业目前干馏工艺温度的合理性以及市售样品的制备工艺是否符合传统或现代工艺。方法:采用硝酸对鲜竹沥样品进行微波消解前处理,用ICP-MS法测定59批鲜竹沥样品中28种元素含量,并进行方法学考察,结合聚类分析和主成分分析对测定结果进行分析。结果:28种元素标准曲线的线性关系良好,r≥0.9992,检测限在0.0071~1.2495 ng·mL^(-1),精密度RSD在0.30%~3.5%,重复性RSD在0.69%~6.4%,稳定性RSD在1.1%~3.3%,回收率在88.6%~105.5%,RSD在1.0%~3.2%。59批鲜竹沥中Na、Mg、K、Ca、Mn、Fe、Zn、Rb元素含量较高,重金属元素含量均未超过限度要求。聚类分析结果显示,干馏法和火制法2种工艺制备的样品聚为一类。主成分分析得到7个主成分,累计方差率达75.6%。确定Mg、K、Ca、Cr、Fe、Co、Cu、Rb、Cd、Ba、Tl、Pb元素为鲜竹沥的特征元素。结论:综合有益和有害元素的含量发现,干馏160℃样品的有毒有害元素含量低于火制法,有益元素含量与火制法相近,该温度与目前经省级药监局认证的企业干馏工艺温度一致。市售样品大部分符合传统或现代工艺的要求,少数可能因工艺不同产生质量差异。通过对不同工艺鲜竹沥中重金属及其他元素的测定和分析,为鲜竹沥的安全生产和合理使用提供了科学依据。Objective:To determine the contents of 28 elements in Xianzhuli under processes of dry distillation and fire preparation by inductively coupled plasma mass spectrometry(ICP-MS),and evaluate the rationality of the current temperature used in the dry distillation process as well as whether the preparation process of commercial samples conforms to the traditional or modern one.Methods:The samples of Xianzhuli were pre-treated with nitric acid before microwave digestion.The contents of 28 elements in 59 batches of Xianzhuli samples were determined by inductively coupled plasma mass spectrometry(ICP-MS),and the methodology was investigated.Results:The standard curve of 28 elements had a good linear relationship with r≥0.9992.The detection limits were 0.0071-1.2495 ng·mL^(-1),the RSDs for precision,repeatability and repeatability tests were 0.30%-3.5%,0.69%-6.4%and 1.1%-3.3%,respectively and the recovery rates were 88.6%-105.5%with RSDs ranged from 1.0%to 3.2%.The contents of Na,Mg,K,Ca,Mn,Fe,Zn and Rb in 59 batches of Xianzhuli were high,and the contents of heavy metal elements did not exceed the limit requirements.The results of cluster analysis showed that the samples prepared by dry distillation and fire preparation were clustered into one class.By principal component analysis,7 principal components were obtained,and the cumulative variance rate was 75.6%.Mg,K,Ca,Cr,Fe,Co,Cu,Rb,Cd,Ba,Tl and Pb were identified as the characteristic elements of Xianzhuli.Conclusion:Based on the contents of beneficial and harmful elements,it is found that the contents of toxic and harmful elements in the sample processed with 160℃dry distillation are lower than processed with fire preparation.And the contents of beneficial elements are similar in two kinds of samples.This temperature is consistent with the dry distillation process temperature approved by provincial drug regulatory authorities for currently certified enterprises.Most of the commercially available samples meet the requirements of traditional or modern processes,and

关 键 词：鲜竹沥 干馏和火制 微波消解 电感耦合等离子体质谱 元素 

分 类 号：R917[医药卫生—药物分析学]