摘要
目的:建立微波消解-电感耦合等离子质谱(ICP-MS)法。测定穿心莲内酯磺化物中铅(Pb)、镉(Cd)、汞(Hg)、砷(As)、铜(Cu)、铁(Fe)、钴(Co)、铬(Cr)、镍(Ni)、钒(V)、银(Ag)、锂(Li)、铋(Bi)、锑(Sb)、锡(Sn)、钡(Ba)、铝(Al)17种金属元素的含量。方法:HNO3作为消解酸体系,采用微波消解法前处理样品后,以钪(45 Sc)、锗(72Ge)、铟(115 In)、碲(125Te)作为内标,通过ICP-MS法同时测定中间体中17种金属元素的量。结果:各元素线性关系均良好(r≥0.9990),方法检出限为0.6395~154.5942μg·kg-1,平均回收率为77.5%~117.1%,RSD均小于3%(n=9);20批穿心莲内酯磺化物的17种有害重金属元素的残留量均符合中国药典2015年版、人用药品注册技术要求国际协调会(ICH)Q3D及国标GB2760-2014的规定。结论:该方法准确快捷,灵敏度高,可推荐用于穿心莲内酯总磺化物中金属元素的定量测定及质量控制。
Objective:To establish a microwave digestion-inductively coupled plasma mass spectrometry(ICP-MS)method for the determination of 17 metals including Pb,Cd,Hg,As,Cu,Fe,Co,Cr,Ni,V,Ag,Li,Bi,Sb,Sn,Ba and Al in andrographolide sulfonates.Methods:HNO3 was used as the acid digestion system.The samples were conducted pretreatment by a microwave digestion instrument;45Sc,72Ge,115 In and 125Te were used as the internal standard elements,and the 17 metal elements were determined by ICP-MS simultaneously.Results:The elements all had a good linear relationship(r≥0.9990).The limit of detection ranged from 0.6395 to 154.5942μg·kg-1,the average recovery ranged from 77.5%to 117.1%,and the RSDs were all less than 3%(n=9).The determination of 17 metal elements in twenty samples of andrographolide sulfonates all met the requirements of Chinese Pharmacopoeia(2015 edition),ICH and GB2760-2014.Conclusion:The method is simple and fast with good accuracy and high precision,so it can be recommended for the determination of metal elements in andrographolide sulfonates,which provides reference for its quality control.
作者
刘艳红
刘芳芳
刘尧奇
方礼
古丽萍
周舟
邓双炳
谢华萍
刘地发
Liu Yanhong;Liu Fangfang;Liu Yaoqi;Fang Li;Gu Liping;Zhou Zhou;Deng Shuangbing;Xie Huaping;Liu Difa(Jiangxi Qingfeng Pharmaceutical Co.Ltd.,Jiangxi Ganzhou 341000,China;State Key Laboratory of Innovative Natural Medicine and TCM Injections)
出处
《中国药师》
CAS
2020年第5期961-965,共5页
China Pharmacist
基金
国家中药标准化项目(编号:ZYBZH-C-JX-41)。
