植物性样品中农药残留多色谱质谱筛选和确证体系的研究

Screening and confirmation of non-target pesticide residues in plant samples using a combined system of GPC-GC-MS, LC-ToF and GC-MS/MS

中文关键词:  农药残留物筛选  农药残留物确证  GPC-GCMS  LC-QToF  GC-MS/MS

英文关键词:pesticides residue screening  pesticides residue confirmation  GPC-GC-MS  LC-QToF  GC- MS/MS

中文摘要:

      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。

英文摘要:

      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 spectro-metry (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 following 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 successfully screened by the combined techniques based on GPC-GC-MS and LC-QToF, and subsequently confirmed 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.