National Food Institute, Technical University of Denmark, DTU-Food, Lyngby, Denmark.
Anal Methods. 2024 Jun 13;16(23):3784-3797. doi: 10.1039/d4ay00226a.
Newly designed micro-solid phase extraction cartridges are now available, reflecting the increasing shift towards laboratory automation, especially in the clean-up step for the analysis of pesticide residues in food and feed. In the present study, the introduction of different sorbents on the newly designed PAL µSPE CTC cartridges was investigated for the removal of matrix interferents and the recovery of pesticides. Eight cartridges containing different sorbent combinations and different amounts were used including EMR-lipid (not activated), Z-sep, chitin, C18, PSA, and GCB. The evaluation of co-extractive removal for each cartridge showed that the optimal choice for removing fatty acids was the cartridges containing PSA and Z-sep as clean-up sorbents. However, the presence of C18 and EMR-lipid was still required for the removal of sterols and tocopherols. Two grams of sample, fish feed (FF) and rapeseed cake (RSC) were extracted using QuEChERS citrate buffer, followed by a freeze-out step. The recoveries and repeatability of QuEChERS using µ-SPE clean-up were evaluated for 216 pesticide residues (112 compounds analyzed by GC-MS/MS and 143 compounds by LC-MS/MS, from which 39 compounds were analyzed using both techniques). The best results, with recovery between 70 and 120% and RSD <20%, were achieved when FF samples were cleaned-up with 15 mg EMR-lipid and 20 mg MgSO. This was achieved for 94% of GC-amenable compounds and 86% of LC-amenable compounds. In the case of RSC, the best results were seen when samples were cleaned-up with the cartridge containing only 20 mg Z-sep and 20 mg MgSO. This was achieved for 88% of GC-amenable compounds and 90% of LC-amenable compounds. Although these cartridges yielded optimal results in terms of recovery, their use could require more instrument maintenance, especially for GC-MS/MS, due to the lower removal of co-extractives.
现已推出全新设计的微固相萃取小柱，反映出实验室自动化的趋势日益增强，尤其是在食品和饲料中农药残留分析的净化步骤中。在本研究中，研究了在新设计的 PAL µSPE CTC 小柱上引入不同的吸附剂，以去除基质干扰物并回收农药。使用了八种包含不同吸附剂组合和不同量的小柱，包括 EMR-lipid（未活化）、Z-sep、甲壳素、C18、PSA 和 GCB。对每个小柱的共萃取去除效果的评估表明，去除脂肪酸的最佳选择是含有 PSA 和 Z-sep 作为净化吸附剂的小柱。然而，仍然需要 C18 和 EMR-lipid 来去除甾醇和生育酚。使用 QuEChERS 柠檬酸盐缓冲液提取 2 克样品，鱼饲料（FF）和油菜籽饼（RSC），然后进行冷冻浓缩步骤。评估 QuEChERS 使用 µ-SPE 净化后的回收率和重复性，共分析了 216 种农药残留（112 种用 GC-MS/MS 分析，143 种用 LC-MS/MS 分析，其中 39 种用两种技术分析）。FF 样品用 15mg EMR-lipid 和 20mg MgSO4 净化时，回收率在 70%至 120%之间，RSD<20%，获得最佳结果。这适用于 94%的 GC 相容化合物和 86%的 LC 相容化合物。对于 RSC，当样品用仅包含 20mg Z-sep 和 20mg MgSO4 的小柱净化时，获得最佳结果。这适用于 88%的 GC 相容化合物和 90%的 LC 相容化合物。虽然这些小柱在回收率方面取得了最佳结果，但由于共提取物的去除效果较低，它们的使用可能需要更多的仪器维护，尤其是对于 GC-MS/MS 而言。
