SCIEX has produced an application note describing a fast and sensitive multi-component single method using LC-MS/MS for the detection and quantitation of Fipronil and its associated metabolites, along with Amitraz and its associated metabolites in eggs and other poultry products.
Introduction
During August 2017, Fipronil was detected in eggs produced from poultry farms in Belgium and The Netherlands. Fifteen other European countries were also affected prompting the recall of millions of eggs from human consumption. By the end of August 2017, contaminated eggs were also found across the globe including China and Hong Kong. Fipronil, a broad spectrum insecticide which belongs to the phenylpyrazole chemical family, is used in the application of red mite, flea, cockroach and ant control. It is the main active ingredient in many flea prevention pet care products. The World Health Organisation (WHO) has classed Fipronil as a class II moderately hazardous pesticide.
Overview
The developed assay uses a modified QuEChERS sample preparation method for the extraction of the egg and poultry matrices. Chromatography was performed using a reversed-phase water/methanol gradient at a complete runtime of 7 mins injection to injection using a Phenomenex Kinetex Polar C18 column. Mass spectrometry is performed on a SCIEX Triple Quad™ 6500+ LC-MS/MS instrument using electrospray ionization, scheduled MRM detection with simultaneous positive/negative ionization switching throughout the run. Results from the assay easily meet the EU regulation MRL of 5 μg/kg in terms of LODs, LOQs, signal-to-noise, MRM ion ratio accuracy and CV and data is shown within the application note to highlight such on both spiked samples and ‘real’ samples where positive results were found.
Conclusions
The analytical method described here is found to be suitable to detect and confirm the presence of the insecticides Fipronil, Amitraz and their associated metabolites in egg and poultry products. The results of the analytical assay showed excellent linearity and reproducibility of detection for all compounds. Detection limits were in line with the EU set MRL levels of 5 μ/kg, with compounds being able to be detected below this level with high reproducibility in the presence of matrix.
