Rapid analysis of fipronil and fipronil sulfone in eggs by liquid chromatography and triple quadrupole mass spectrometry

Goal

Develop a quick and simple method for the determination of fipronil and fipronil sulfone in eggs using an in-house modified QuEChERS acetonitrile extraction protocol and LC-MS/MS determination.

Introduction

Recently, it was reported that millions of eggs contaminated with the insecticide fipronil have been distributed to more than 17 countries.1 On July 20th 2017, it was made public that in some cases the pesticide fipronil was mixed with another formulation and sprayed on chickens against ticks, fleas and lice.1 As the determined levels were in some cases substantially higher (up to 1.2 mg/kg) than the EU MRL of 0.005 mg/kg for the sum of fipronil and fipronil sulfone,2,3 there is a demand for quick and efficient methods for the determination of both substances in egg matrix and potentially in chicken meat.

This brief presents a quick and simple method for the determination of fipronil and fipronil sulfone in eggs using an in-house modified QuEChERS acetonitrile extraction protocol.

Experimental

Sample preparation

Egg samples purchased in a local store were extracted using the procedure described in Figure 1.

Sample preparation consumables

• 50 mL conical sterile polypropylene centrifuge tubes, P/N 339652
• 15 mL conical sterile polypropylene centrifuge tubes; P/N 339650
• Thermo Scientific™ HyperSep™ dispersive SPE Mylar pouch 4000 mg magnesium sulfate and 1000 mg NaCl, 50 pk, P/N 60105-340
• Magnesium sulfate, 99%, for analysis, anhydrous; 12198721

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