Quantitative Determination of Organophosphorus, Pyrethroid, and Dithiolane Pesticide Residues in Brown Rice Using Supercritical Fluid Extraction and Liquid Chromatography–Tandem Mass Spectrometry

作者：Keisuke Nakamura, Takamitsu Otake, Nobuyasu Hanari · 发表于：Journal of AOAC International · 年份：2023 · DOI：10.1093/jaoacint/qsad080 · 被引用次数：7 · 研究领域：Pesticide Residue Analysis and Safety、Metabolomics and Mass Spectrometry Studies、Analytical Chemistry and Chromatography

BACKGROUND: Supercritical fluid extraction (SFE) is a fast, versatile, and solvent-efficient automatic extraction method. Despite its advantages, the results of our proficiency tests imply that the applicability assessments of SFE for pesticide residues were insufficient. OBJECTIVE: In this study, as analytical method using SFE was optimized and validated by testing the incurred and fortified brown rice samples with organophosphorus (OP), pyrethroid (PYR), and dithiolane (DIT) pesticides. METHOD: A validation study using the incurred sample with etofenprox, fenitrothion, and isoprothiolane was performed by comparing the analytical results obtained using the SFE and solid-liquid extraction with homogenization (SLE), which is a well-validated official multi-residue extraction method. The tests on the fortified samples were also performed for seven pesticide residues, chlorpyrifos, diazinon, O-ethyl O-4-nitrophenyl phenylphosphonothioate (EPN), etofenprox, fenitrothion, isoxathion, and isoprothiolane, at three fortification levels, 0.001, 0.01, and 0.1 mg/kg. RESULTS: In the test on the incurred samples, optimized SFE-to-SLE analytical values (CSFE/CSLE) were 99.2-100.1%, with RSD lower than 3%. In contrast, the analytical-to-spiked concentrations in the tests on the fortified samples were 96.4-105.0%, with RSD lower than 8.8%. CONCLUSIONS: These results indicate that the proposed SFE method, which is well validated with the incurred brown rice sample, is useful for determining ...