Comparison of recovery efficiency and matrix effect reduction in pesticide residue analysis: QuEChERS with d-SPE, SPE, and FaPEx in apples and Korean cabbage

Abstract

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⁻¹ 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.