CAJ | 학술논문

目的针对植物样品中存在的多种未知农药残留,研究建立基于 GPC-GC-MS、LC-QToF 和GC-MS/MS技术为主的筛选和确证方法,满足相关的定量分析需求.方法以FAPAS国际实验室能力比对的玉米粉为典型样品,采用水浸泡、乙腈缓冲体系提取、分散性固相萃取净化(d-SPE)、浓缩后,分别依托GPC-GC-MS和LC-QToF的全扫描图谱,采用自动数据库匹配和手工匹配的方法,进行协同筛选可疑目标物,并对筛选的可疑目标分析物采用GC-MS/MS确证和测定.结果 GPC-GC-MS和LC-QToF两种筛选方法成功筛选了4种可疑目标分析物,经GC-MS/MS确证并测定,与FAPAS盲样比对的阳性结果一致,统计Z分数的绝对值≤0.5.结论该方法确证了本实验室的3种质谱系统联合使用在农药残留筛选和确证中的可行性和可靠性.
목적침대식물양품중존재적다충미지농약잔류,연구건립기우 GPC-GC-MS、LC-QToF 화GC-MS/MS기술위주적사선화학증방법,만족상관적정량분석수구.방법이FAPAS국제실험실능력비대적옥미분위전형양품,채용수침포、을정완충체계제취、분산성고상췌취정화(d-SPE)、농축후,분별의탁GPC-GC-MS화LC-QToF적전소묘도보,채용자동수거고필배화수공필배적방법,진행협동사선가의목표물,병대사선적가의목표분석물채용GC-MS/MS학증화측정.결과 GPC-GC-MS화LC-QToF량충사선방법성공사선료4충가의목표분석물,경GC-MS/MS학증병측정,여FAPAS맹양비대적양성결과일치,통계Z분수적절대치≤0.5.결론해방법학증료본실험실적3충질보계통연합사용재농약잔류사선화학증중적가행성화가고성.
Objective To establish a method for the screening and confirmation of non-target pesticides in plant samples based on the techniques of gel permeation chromatography-gas chromatography-mass spec-trometry (GPC-GC-MS) and liquid chromatography-quaqrupole-time of flight mass spectrometry (LC-QToF). Methods After a sample pretreatment including extraction with acetic acid/acetonitrile buffer system follow-ing water immersion, cleaning up with dispersive solid-phase extraction and concentration, the sample was separately analysed with GPC-GC-MS and LC-QToF in full scan mode and subsequently selected. Based on the suspicious target analytes of the screening, gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) was used to confirm the analytes and determine them. Results Four suspicious target analytes were suc-cessfully screened by the combined techniques based on GPC-GC-MS and LC-QToF, and subsequently con-firmed and determined by GC-MS/MS. The results were in accord with FAPAS test. Conclusion The method based on a combined system with GPC-GC-MS, LC-QToF and GC-MS/MS is feasible and accurate for screening and confirmation of non-target pesticides in plant samples.