Progress in Plant Protection

Optymalizacja metody jednoczesnego oznaczania 248 pestycydów w suszonych owocach
Optimization of the method for the simultaneous determination of 248 pesticides in dry fruit

Ewa Rutkowska, e-mail: e.rutkowska@iorpib.poznan.pl

Instytut Ochrony Roślin – Państwowy Instytut Badawczy, Chełmońskiego 22, 15-195 Białystok, Polska

Bożena Łozowicka, e-mail: b.lozowicka@iorpib.poznan.pl

Instytut Ochrony Roślin – Państwowy Instytut Badawczy, Chełmońskiego 22, 15-195 Białystok, Polska

Piotr Kaczyński, e-mail: p.kaczynski@iorpib.poznan.pl

Instytut Ochrony Roślin – Państwowy Instytut Badawczy, Chełmońskiego 22, 15-195 Białystok, Polska
Abstract

Celem badań było przeprowadzenie optymalizacji metody jednoczesnego oznaczania 248 pestycydów w modelowych matrycach o niskiej zawartości wody (suszone owoce aronii, jabłek, porzeczek) przy wykorzystaniu techniki chromatografii gazowej sprzężonej z tandemową spektrometrią mas w oparciu o zmodyfikowany protokół QuEChERS. Badania koncentrowano na doborze 1) dodatku wody (5 ml; 7,5 ml; 10 ml), 2) masy próbki (2 g; 5 g; 10 g), 3) polarności rozpuszczalnika (aceton; acetonitryl; octan etylu) oraz 4) sorbentów etapu oczyszczania (PSA/ENVI-Carb/MgSO4; ChloroFiltr/PSA/MgSO4; Chitosan; Chityna). Zastosowanie układu 2 g próbki/10 ml wody/10 ml acetonitrylu/PSA/ENVI-Carb/MgSO4 umożliwiło uzyskanie akceptowalnych parametrów walidacyjnych. Odzyski analizowanych związków mieściły się w granicach 63−118%, a względne odchylenie standardowe poniżej 18% w zakresie stężeń (0,005−1,00 mg/kg). Nieistotnym efektem matrycy (-20% < ME < 20%) charakteryzowało się ponad 90% analizowanych związków. Metodę zaadaptowano do rutynowych badań i rozszerzono o inne matryce.

 

The aim of this study was to optimize the method of simultaneous determination of 248 pesticides in model matrices of fruit with a low water content (chokeberry, apples, currants) using the gas chromatography coupled with tandem mass spectrometry based on the modified QuEChERS protocol. The research focused on the selection of: 1) water addition (5 ml; 7.5 ml; 10 ml), 2) sample mass (2 g; 5 g; 10 g), 3) the polarity of the solvent (acetone, acetonitrile, ethyl acetate) and 4) clean-up sorbents (PSA/ENVI-Carb/MgSO4; ChloroFiltr/PSA/MgSO4; Chitosan; Chitin). The use of the 2 g sample/10 ml water/10 ml acetonitrile/PSA/ENVI-Carb/MgSO4 system allowed to obtain acceptable validation parameters. The recoveries of the analyzed compounds were within the range of 63−118%, and the relative standard deviation below 18% in the concentration range (0.005−1.00 mg/kg). More than 90% of the analyzed compounds had a negligible matrix effect (-20% < ME < 20%). The method was applied to routine analysis and extended to other matrices.

Key words
suszone owoce; pozostałości ś.o.r.; chromatografia gazowa; metoda analityczna; optymalizacja; dry fruit; pesticide residues; gas chromatography; analytical method; optimization
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Progress in Plant Protection (2022) 62: 57-65
First published on-line: 2022-03-14 12:40:33
http://dx.doi.org/10.14199/ppp-2022-008
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