Validation and Use of an Accurate, Sensitive Method for Sample Preparation and Gas Chromatography–Mass Spectrometry Determination of Different Endocrine-Disrupting Chemicals in Dairy Products

Abstract

Endocrine disrupting chemicals (EDCs) are exogenous substances capable of altering the human hormone system and causing various diseases such as infertility and cancer as a result. In this work, a method for determining twenty-three different EDCs including parabens, alkylphenols, phenylphenols, organophosphorus pesticides, bisphenol A and triclosan in dairy products was developed. Samples are conditioned by addition of acetonitrile containing 1% formic acid, centrifugation and clean-up of the extract by continuous solid-phase extraction. EDCs in the extract are derivatised by heating in a microwave oven and quantified by gas chromatography–mass spectrometry. The proposed method features good limits of detection (6–40 ng/kg) and precision (relative standard deviation < 7.6%); also, it is scarcely subject to matrix effects (1–20%). EDC recoveries from spiked samples ranged from 80 to 108%. The method was used to analyse a total of 33 samples of dairy products including cow, sheep and goat milk, yoghourt, milkshakes, cheese, cream, butter and custard. Bisphenol A was the individual contaminant detected in the greatest number of samples, at concentrations from 180 to 4800 ng/kg. 2-Phenylphenol and ethylparaben were found in more than one-half, at concentrations over the range 130–3500 and 89–4300 ng/kg, respectively. In contrast, alkylphenols, organophosphorus pesticides and triclosan were detected in none.