Validation of determination for pesticides including fipronil in hen eggs by LC-MS/MS and GC/MS/MS

Ozgur Golge¹, Turan Lİman², Bulent Kabak³^,^*

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¹Alanya Alaaddin Keykubat University, Faculty of Tourism, Department of Gastronomy and Culinary Arts, Alanya, Antalya, Turkey

²STA Food Quality Control Laboratory, Mersin 33010, Turkey.

³3Hitit University, Faculty of Engineering, Department of Food Engineering, TR-19030 Corum, Turkey

^*Corresponding Author: Bulent Kabak, Hitit University, Faculty of Engineering, Department of Food Engineering, Corum 19030, Turkey. E-mail: bulentkabak@hitit.edu.tr.

© Copyright 2021 Korean Society for Food Science of Animal Resources. This is an Open-Access article distributed under the terms of the Creative Commons Attribution Non-Commercial License (http://creativecommons.org/licenses/by-nc/3.0/) which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited.

Received: May 05, 2021 ; Revised: Jun 16, 2021 ; Accepted: Jul 28, 2021

Published Online: Jul 29, 2021

Abstract

This study aims to validate a fast method of simultaneous analysis of 365 LC-amenable and 142 GC-amenable pesticides in hen eggs by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS), respectively, operating in multiple reaction monitoring (MRM) acquisition modes. The sample preparation was based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction. Key method performance parameters investigated were specificity, linearity, limit of quantification (LOQ), accuracy, precision and measurement uncertainty. The method was validated at two spiking levels (10 and 50 mg/kg), and good recoveries (70–120%) and relative standard deviations (RSDs) (≤20) were achieved for 92.9% of LC-amenable and 86.6% of GC-amenable pesticide residues. The LOQs were ≤10 µg/kgfor 94.2% of LC-amenable and 92.3% of GC-amenable pesticides. The validated method was further applied to 100 egg samples from caged hens, and none of the pesticides was quantified.

Keywords: pesticides; hen eggs; food safety; monitoring; method validation