A comparative study of three modifications of the QuEChERS method for determination of endocrine disrupting pesticide residues in lemon matrices by fast GC-MS

Abstract

Three modifications of the QuEChERS (quick, easy, cheap, effective, rugged and safe) method for determination of 35 endocrine disrupting pesticides in samples with high acid content such as lemons were studied. Pesticides extraction was performed using the original QuEChERS method, citrate buffered QuEChERS method (EU version) and acetate buffered QuEChERS method (AOAC version). Final extracts were evaluated by fast gas chromatography-mass spectrometry (GC-MS) analysis. Validation experiments for all three methods were performed using a spiked pesticide free lemon matrix and matrix-matched standard solutions. Four concentration levels (1, 20, 50 and 250 mg kg À1 ) were tested. Recoveries from 70 to 120% with a relative standard deviation <20% were obtained for the majority of pesticides. Linearity was evaluated at a concentration range of 1-250 mg kg À1 for the buffered QuEChERS (AOAC) method with coefficients of determination (R 2 ) higher than 0.9552 and for the original QuEChERS method with R 2 higher than 0.9232. The best linearity was obtained for the citrate buffered method with R 2 higher than 0.9656. The limit of detection (LOD) of the buffered QuEChERS (AOAC) method ranged between 0.1 and 18.4 mg kg À1 , for the citrate buffered QuEChERS method between 0.1 and 23.6 mg kg À1 and for the original QuEChERS method between 0.1 and 14.2 mg kg À1 . Results obtained by the three different QuEChERS methods were compared. The citrate buffered method is more suitable for the tested pesticides than the other two QuEChERS methods.Although the QuEChERS method is widely applied, it was shown that in difficult matrices such as lemons, the choice of modifications is analyte/matrix dependent. The three developed and validated methods were applied to the analysis of real citrus samples.

QuEChERS LC–MS/MS Screening Method for Mycotoxin Detection in Cereal Products and Spices

“…The QuEChERS (Quick Easy Cheap Effective Rugged and Safe) method is becoming one of the most used dispersive solid-phase extraction (d-SPE) methods in food safety [ 69 , 85 , 86 , 87 , 88 ]. According to Web of Science, more than 1200 scientific papers cover aspects or use QuEChERS for extraction procedures.…”

Follow-up of the fate of imazalil from post-harvest lemon surface treatment to a baking experiment

“…The results showed no significant differences between imazalil concentration levels; however, the authors studied spiked samples instead of targeting real samples inherently containing pesticides. Andraščíková and Hrouzková (2013) compared the two methods to whole lemon matrix by GC-MS. The citrate buffered method was found more suitable for the tested pesticides than the AOAC method was in terms of recovery, limit of detection (LOD), and linearity.…”

Limonun evde işlenmesi sırasında bazı insektisitlerin kalıntılarının değerlendirilmesi

“…Active ingredients for lemon fruits were selected based on their popularity on the agricultural farming applications and their residue occurrence frequency (Andrascikova & Hrouzkova, 2013;Bakirci et al, 2014;Cicero et al, 2015;Dincay & Civelek, 2017;Besil et al, 2019;Chen et al, 2021;EU, 2021;Aslantas et al, 2023;Karaağaçlı, 2023). The commercial formulations of abamectin, buprofezin and etoxazole were selected as Asmition (18 g/L, emulsified concentrate), Korfezin (400 g/L, suspension concentrate) and Novamite (110 g/L, suspension concentrate), respectively and purchased from a local market.…”

“…There are some reported studies in literature dedicated to analysis of pesticide residue level in the lemon fruit and lemon products. Based on those studies, registered insecticides including abamectin and buprofezin and non-registered insecticide residues were reported in lemon fruits (Andrascikova & Hrouzkova, 2013;Bakirci et al, 2014;Cicero et al, 2015;Dincay & Civelek, 2017;Besil et al, 2019;Chen et al, 2021;Aslantas et al, 2023;Karaagaçlı, 2023). Moreover, the number of Rapid Alert System for Food and Feed (RASFF) notifications in 2021 for Turkey which was the most reported origin, increased from 191 to 361.…”