PMID- 37311390 OWN - NLM STAT- MEDLINE DCOM- 20230619 LR - 20230619 IS - 1090-2414 (Electronic) IS - 0147-6513 (Linking) VI - 261 DP - 2023 Aug TI - Multivariate response surface methodology assisted modified QuEChERS method for the rapid determination of 39 pesticides and metabolites in medlar. PG - 115102 LID - S0147-6513(23)00606-1 [pii] LID - 10.1016/j.ecoenv.2023.115102 [doi] AB - A modified QuEChERS method coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was established for residue analysis of 39 pollutants (34 commonly used multi-class pesticides and 5 metabolites) in medlar matrices (fresh, dried, and medlar juice). Samples were extracted using water with 0.1 % formic acid: acetonitrile (5: 10, v/v). The phase-out salts and five different cleanup sorbents (including N-propyl ethylenediamine (PSA), octadecyl silane bonded silica gel (C18), graphitized carbon black (GCB), Carbon nanofiber (C-Fiber) and MWCNTs) were investigated to improve the purification efficiency. The Box-Behnken Design (BBD) study was employed for an optimal solution of the volume of extraction solvent, phase-out salt, and the purification sorbents for the analytical method. The average recoveries of the target analytes in the three medlar matrices ranged from 70 % to 119 % with relative standard deviations (RSDs) of 1.0 %-19.9 %. Screening of market samples (fresh and dried medlars) collected from the major producing regions in China showed that 15 pesticides and metabolites were detected in the samples at concentrations of 0.01-2.22 mg/kg, and none of which exceeded the maximum residue limits (MRLs) set in China. The results showed that the risk of food safety by consumption of medlar products caused by the use of pesticides was low. The validated method could be used for rapid and accurate screening of multi-class multi-pesticide residues in Medlar for food safety. CI - Copyright (c) 2023 The Authors. Published by Elsevier Inc. All rights reserved. FAU - Zhuang, Ming AU - Zhuang M AD - Innovation Center of Pesticide Research, Department of Applied Chemistry, College of Science, China Agricultural University, Beijing 100193, China. FAU - Yao, Wei AU - Yao W AD - Innovation Center of Pesticide Research, Department of Applied Chemistry, College of Science, China Agricultural University, Beijing 100193, China; Beijing Vocational College of Agriculture, Beijing 102500, China. FAU - Han, Lijun AU - Han L AD - Innovation Center of Pesticide Research, Department of Applied Chemistry, College of Science, China Agricultural University, Beijing 100193, China. Electronic address: hlj2000@cau.edu.cn. FAU - Bi, Yingying AU - Bi Y AD - Innovation Center of Pesticide Research, Department of Applied Chemistry, College of Science, China Agricultural University, Beijing 100193, China. FAU - Qiao, Chengkui AU - Qiao C AD - Zhengzhou Fruit Research Institute, Chinese Academy of Agricultural Sciences, Zhengzhou 450009, China. FAU - Lv, Xinru AU - Lv X AD - Innovation Center of Pesticide Research, Department of Applied Chemistry, College of Science, China Agricultural University, Beijing 100193, China. FAU - Cao, Mengyuan AU - Cao M AD - Innovation Center of Pesticide Research, Department of Applied Chemistry, College of Science, China Agricultural University, Beijing 100193, China. FAU - Xie, Hanzhong AU - Xie H AD - Zhengzhou Fruit Research Institute, Chinese Academy of Agricultural Sciences, Zhengzhou 450009, China. LA - eng PT - Journal Article DEP - 20230611 PL - Netherlands TA - Ecotoxicol Environ Saf JT - Ecotoxicology and environmental safety JID - 7805381 RN - 0 (Pesticides) RN - 0 (Pesticide Residues) SB - IM MH - *Pesticides/analysis MH - Tandem Mass Spectrometry/methods MH - *Pesticide Residues/analysis MH - Chromatography, High Pressure Liquid MH - Vegetables/chemistry MH - Solid Phase Extraction/methods OTO - NOTNLM OT - Box-behnken design OT - Environmental contaminants OT - HPLC-MS/MS OT - Method optimization OT - Residue analysis COIS- Declaration of Competing Interest The authors declare the following financial interests/personal relationships which may be considered as potential competing interests: Lijun Han reports financial support was provided by Beijing Natural Science Foundation. Lijun Han reports financial support was provided by Tianjin Municipal Natural Science Foundation. Lijun Han reports financial support was provided by Hebei Provincial Natural Science Foundation. EDAT- 2023/06/14 01:10 MHDA- 2023/06/19 13:08 CRDT- 2023/06/13 18:04 PHST- 2023/03/01 00:00 [received] PHST- 2023/05/18 00:00 [revised] PHST- 2023/06/01 00:00 [accepted] PHST- 2023/06/19 13:08 [medline] PHST- 2023/06/14 01:10 [pubmed] PHST- 2023/06/13 18:04 [entrez] AID - S0147-6513(23)00606-1 [pii] AID - 10.1016/j.ecoenv.2023.115102 [doi] PST - ppublish SO - Ecotoxicol Environ Saf. 2023 Aug;261:115102. doi: 10.1016/j.ecoenv.2023.115102. Epub 2023 Jun 11.