PMID- 37439707 OWN - NLM STAT- MEDLINE DCOM- 20231108 LR - 20231108 IS - 1944-7922 (Electronic) IS - 1060-3271 (Linking) VI - 106 IP - 6 DP - 2023 Nov 2 TI - Quantitative Determination of Organophosphorus, Pyrethroid, and Dithiolane Pesticide Residues in Brown Rice Using Supercritical Fluid Extraction and Liquid Chromatography-Tandem Mass Spectrometry. PG - 1532-1541 LID - 10.1093/jaoacint/qsad080 [doi] AB - 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 OP, PYR, and DIT pesticide residues in brown rice. HIGHLIGHTS: The proposed SFE method satisfies EU and Japanese maximum residue limits (MRLs). The consumption of solvent can be reduced to one-fourth of that of SLE using the proposed SFE method. CI - (c) The Author(s) 2023. Published by Oxford University Press on behalf of AOAC INTERNATIONAL. All rights reserved. For permissions, please email: journals.permissions@oup.com. FAU - Nakamura, Keisuke AU - Nakamura K AUID- ORCID: 0000-0001-7782-1040 AD - National Metrology Institute of Japan (NMIJ), National Institute of Advanced Industrial Science and Technology (AIST), Central 3, 1-1-1 Umezono, Tsukuba, Ibaraki 305-8563, Japan. FAU - Otake, Takamitsu AU - Otake T AUID- ORCID: 0000-0001-8213-996X AD - National Metrology Institute of Japan (NMIJ), National Institute of Advanced Industrial Science and Technology (AIST), Central 3, 1-1-1 Umezono, Tsukuba, Ibaraki 305-8563, Japan. FAU - Hanari, Nobuyasu AU - Hanari N AUID- ORCID: 0000-0003-3093-2450 AD - National Metrology Institute of Japan (NMIJ), National Institute of Advanced Industrial Science and Technology (AIST), Central 3, 1-1-1 Umezono, Tsukuba, Ibaraki 305-8563, Japan. LA - eng GR - Health and Labour Sciences Research/ GR - 20KA1001/Ministry of Health, Labour, and Welfare/ GR - Japan Society for the Promotion of Science/ GR - KAKENHI/ GR - JP21 K14657/Grant-in-Aid for Early-Career Scientists/ PT - Journal Article PL - England TA - J AOAC Int JT - Journal of AOAC International JID - 9215446 RN - 0 (Pesticide Residues) RN - 0LD7P9153C (ethofenprox) RN - 88HCS898G6 (isoprothiolane) RN - W8M4X3Y7ZY (Fenitrothion) RN - 0 (Pyrethrins) RN - 0 (Solvents) SB - IM MH - *Pesticide Residues/analysis MH - *Oryza MH - *Chromatography, Supercritical Fluid/methods MH - Tandem Mass Spectrometry MH - Fenitrothion/analysis MH - *Pyrethrins/analysis MH - Chromatography, Liquid/methods MH - Solvents/chemistry EDAT- 2023/07/13 12:32 MHDA- 2023/11/08 06:44 CRDT- 2023/07/13 10:13 PHST- 2022/11/29 00:00 [received] PHST- 2023/06/26 00:00 [revised] PHST- 2023/06/26 00:00 [accepted] PHST- 2023/11/08 06:44 [medline] PHST- 2023/07/13 12:32 [pubmed] PHST- 2023/07/13 10:13 [entrez] AID - 7223728 [pii] AID - 10.1093/jaoacint/qsad080 [doi] PST - ppublish SO - J AOAC Int. 2023 Nov 2;106(6):1532-1541. doi: 10.1093/jaoacint/qsad080.