National Institute of Agricultural Sciences, 166 Nongsaengmyeong-ro, Iseo-myeon, Wanju-gun, Jeollabuk-do 55365, Korea.
Anal Methods. 2023 Aug 3;15(30):3709-3716. doi: 10.1039/d3ay00612c.
QuEChERS is widely used for the analysis of pesticide residues. However, d-SPE, which is commonly utilized in QuEChERS, demonstrates lower clean-up effectiveness than that achieved using conventional SPE, leading to an inadequate reduction of matrix effects. Hence, methods, such as internal standards and matrix-matched calibration (MMC), are frequently employed to address matrix effects. The most effective way to minimize matrix effects is to enhance the clean-up efficiency. In this study, the analytical efficiencies of conventional QuEChERS, d-SPE, SPE, and FaPEx, a novel analytical method, were compared for the clean-up of apple and Korean cabbage samples. The proportion of test pesticides within the appropriate recovery range was 94-99% for QuEChERS, d-SPE, and SPE, while it was 80-95% for FaPEx. When evaluating the recovery results by group, the proportion of pesticides in group III (90-105%) was lower for FaPEx (3-70%) than that for d-SPE (85-92%) and SPE (79-89%). The matrix effect reduction was satisfactory for all clean-up methods, with more than 94% of the test pesticides showing low levels of matrix effects within ±20%. In FaPEx, over 98% of the test pesticides exhibited low matrix effects, indicating better reduction effects than in QuEChERS-based d-SPE and SPE. Method validation results at 0.01 and 0.1 mg kg concentration levels using QuEChERS, SPE (PSA), and FaPEx (amine + C18) demonstrated that more than 95% of the test pesticides were within the appropriate recovery range. Overall, our study contributes to the development of efficient and reliable analytical methods for ensuring the safety and quality of agricultural products.
QuEChERS 广泛用于农药残留分析。然而,d-SPE 在 QuEChERS 中常用,其净化效果不如传统 SPE,导致基质效应降低不足。因此,经常采用内标和基质匹配校准(MMC)等方法来解决基质效应。最小化基质效应的最有效方法是提高净化效率。在这项研究中,比较了传统 QuEChERS、d-SPE、SPE 和 FaPEx(一种新的分析方法)对苹果和韩国白菜样品的净化效果。在适当的回收率范围内,QuEChERS、d-SPE 和 SPE 的测试农药比例为 94-99%,而 FaPEx 为 80-95%。按组评估回收率结果时,FaPEx 组 III(90-105%)中农药的比例(3-70%)低于 d-SPE(85-92%)和 SPE(79-89%)。所有净化方法的基质效应降低都令人满意,超过 94%的测试农药在±20%范围内表现出低水平的基质效应。在 FaPEx 中,超过 98%的测试农药表现出低基质效应,表明其基质效应降低效果优于基于 QuEChERS 的 d-SPE 和 SPE。使用 QuEChERS、SPE(PSA)和 FaPEx(胺+C18)在 0.01 和 0.1 mg kg 浓度水平进行方法验证的结果表明,超过 95%的测试农药在适当的回收率范围内。总的来说,我们的研究为确保农产品的安全和质量开发了高效可靠的分析方法。