PDF(Pubmed)
Abstract：
Generic extraction methods for the multi-compound pesticide analysis of food have found their solid place in laboratories. Ethyl acetate and acetonitrile extraction methods have been developed as fast and easy to handle standard multi-compound methods, both feature benefits and limitations. The direct injection to gas chromatography can be impaired by a high burden of coextracted matrix, resulting in deterioration of the chromatographic system and matrix effects, requiring frequent maintenance. Therefore, common clean-up methods, such as dispersive solid-phase extraction, freeze-out of fats, or gel permeation chromatography, have been applied in clean-up. Automated clean-up using micro-solid-phase extraction (µSPE) is a recent development with several demonstrated advantages when employed in the analysis of pesticides and other contaminants in foods extracted with acetonitrile, but it has not yet been evaluated in this application using ethyl acetate for extraction. In this study, an automated procedure using µSPE cartridges was developed and established on an x,y,z robotic sampler for the raw extract clean-up and preparation of diluted samples for injection on a GC-MS/MS system. Validation experiments for 212 pesticides, polychlorinated biphenyls, and polycyclic aromatic hydrocarbons in lettuce, avocado, raspberry, paprika, egg, and liver extracts were performed using µSPE with MgSO4, PSA, C18, and CarbonX. The performance in routine operation is briefly discussed.
摘要：
用于食品多化合物农药分析的通用提取方法已在实验室中找到了坚实的地位。乙酸乙酯和乙腈萃取方法已被开发为快速且易于处理的标准多化合物方法，两者都有优点和局限性。直接注入气相色谱可能会受到高负担的共提取基质的损害，导致色谱系统和基体效应的恶化，需要经常维护。因此,常见的清理方法，如分散固相萃取，冷冻脂肪，或凝胶渗透色谱法，已用于清理。使用微固相萃取（µSPE）进行自动清理是一项最新发展，在分析用乙腈萃取的食品中的农药和其他污染物时，具有多种优势。但在本申请中尚未使用乙酸乙酯进行萃取评估。在这项研究中,在x上开发并建立了使用µSPE墨盒的自动程序，y,z机器人采样器，用于在GC-MS/MS系统上进行原始提取物清理和稀释样品的制备。212种农药的验证实验,多氯联苯,和生菜中的多环芳烃，鳄梨,覆盆子,辣椒粉,鸡蛋,和肝脏提取物使用µSPE与MgSO4，PSA，C18和CarbonX。简要讨论了常规操作中的性能。
