摘要
建立了超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UPLC-Q-Orbitrap HRMS)对豆芽中药物残留的非靶向筛查和定量分析方法。筛查时样品用乙腈提取,采用全扫描/数据依赖二级扫描(full MSddMS2)模式进行数据采集,在无标准品条件下,根据母离子精确质量数和二级碎片离子信息结合数据库进行定性分析。定量时样品采用优化的分散固相萃取(d-SPE)方法进行净化,并基于母离子峰面积,对筛查出的9种化合物进行定量分析。9种化合物在一定浓度范围内线性关系良好(R^(2)>0.990),检出限在2.0~5.0μg/kg之间,3个添加水平(5, 10, 50μg/kg)的回收率在80.1%~111.1%之间,相对标准偏差均小于15%。
A method for the untargeted screening and quantitative analysis of drug residues in bean sprouts by ultra performance liquid chromatography-quadrupole/orbitrap high resolution mass spectrometry(UPLC-QOrbitrap HRMS)was developed.In the process of screning,the samples were extracted by acetonitrile and the data were gathered via the full MS-ddMS’mode.In the absence of standards,qualitative analysis was carried out according to the exact mass number of precursor ions and secondary fragment ions information combined with the database.The optimized dispersive solid-phase extraction(d-SPE)method was used to purify the samples.9 compounds in bean sprouts were screened and quantified on the basis of the peak areas of the precursor ions.9 compounds showed good linear relationships(R^(2)>0.990)in the linear concentration ranges.The limits of detection of this method were between 2.0-5.0μg/kg.The recoveries of 9 compounds at three spiked levels of 5,10,50μg/kg ranged from 80.1%to 111.1%,and the relative standard deviations were less than 15%.
作者
马凯
杨昌彪
崔姗姗
申鹰
李林竹
范金旭
杨春萍
MA Kai;YANG Changbiao;CUI Shanshan;SHEN Ying;LI Linzhu;FAN Jinxu;YANG Chunping(Guizhou Academy of Testing and Analysis,Guiyang 550000,China)
出处
《分析试验室》
EI
CAS
CSCD
北大核心
2023年第8期1074-1079,共6页
Chinese Journal of Analysis Laboratory
基金
中央引导地方科技发展资金(黔科中引地[2021]4026)
贵州科学院青年基金(黔科院J字[2021]46号)资助。
