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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。
OBJECTIVE To target a variety of unknown pesticide residues in plant samples, a screening and confirmation method based on GPC-GC-MS, LC-QToF and GC-MS / MS techniques was established to meet the needs of quantitative analysis. Methods The corn flour with the capacity of FAPAS was used as a typical sample. The samples were soaked in water, extracted with acetonitrile buffer system, dispersed SPE (d-SPE), and concentrated by GPC-GC-MS and LC- The QToF full-scan map was screened for the synergistic screening of suspected targets using automated database matching and manual matching, and the screening of suspected target analytes was confirmed and determined by GC-MS / MS. Results Four screening methods were successfully screened by GPC-GC-MS and LC-QToF. The results were confirmed by GC-MS / MS and consistent with the positive results of FAPAS blind mapping. The absolute Value ≤ 0.5. Conclusion This method confirms the feasibility and reliability of the combined use of three mass spectrometry systems in pesticide residue screening and validation.