Institute of Food Chemistry, University of Hohenheim, Garbenstraße 28, 70599 Stuttgart, Germany.
Institute of Food Chemistry, University of Hohenheim, Garbenstraße 28, 70599 Stuttgart, Germany.
J Chromatogr A. 2019 Jul 19;1597:9-17. doi: 10.1016/j.chroma.2019.03.020. Epub 2019 Mar 16.
Pesticide residue analysis in fruits and vegetables is generally performed with the QuEChERS method, when clean-up is mainly achieved with primary secondary amine (PSA) by dispersive solid phase extraction (dSPE). In this work, we present a rapid and efficient method for the clean-up of fruit and vegetable extracts with polyethyleneimine (PEI) as alternative to PSA. Clean-up of QuEChERS extracts with a mixture of branched PEI adsorbed on magnesium sulfate and silica gel was realized in 10 min, when several polar matrix components were clearly reduced. The success of the clean-up for representative matrices was visualized by both high-performance thin-layer chromatography with different detection options and total ion current chromatograms of liquid chromatography-mass spectrometry analyses. Generally, dSPE clean-up with PEI was at least equally effective as dSPE with PSA, but PEI clearly superimposed PSA in terms of adsorption capabilities towards fatty acids. After clean-up of fatty acid mixtures with 150 and 300 mg/L, total fatty acids were reduced by 98% and 99%, respectively, while PSA left two- and three-fold quantities. Additionally, the susceptibility of base-labile pesticides towards PEI as compared to PSA generally was negligible, further supporting the high suitability of PEI for clean-up in pesticide residue analysis. Thus, clean-up with PEI enables a clear reduction of various matrix compounds in fruit and vegetable extracts and provides a rapid, convenient and low-cost alternative to the existing dSPE methods with PSA.
果蔬中的农药残留分析通常采用 QuEChERS 方法,通过分散固相萃取(dSPE)主要用初级/次级胺(PSA)进行净化。在这项工作中,我们提出了一种使用聚乙烯亚胺(PEI)替代 PSA 对果蔬提取物进行快速高效净化的方法。使用吸附在硫酸镁和硅胶上的支化 PEI 的混合物对 QuEChERS 提取物进行净化,可在 10 分钟内完成,此时几种极性基质成分明显减少。通过不同检测选项的高效薄层色谱和液相色谱-质谱分析的总离子流色谱图,可视化了代表性基质的净化效果。一般来说,PEI 的 dSPE 净化与 PSA 的 dSPE 至少同样有效,但 PEI 在吸附脂肪酸方面明显优于 PSA。对 150 和 300 mg/L 的脂肪酸混合物进行净化后,总脂肪酸分别减少了 98%和 99%,而 PSA 则留下了两倍和三倍的数量。此外,与 PSA 相比,PEI 对不稳定碱农药的敏感性通常可以忽略不计,这进一步支持了 PEI 在农药残留分析中用于净化的高适用性。因此,PEI 的净化可显著减少果蔬提取物中各种基质化合物的含量,为现有使用 PSA 的 dSPE 方法提供了一种快速、简便且低成本的替代方法。