Abstract
A simple methodology was developed for the determination of four Endocrine Disrupting Chemicals (EDCs) in dairy products. The EDCs included alkylphenols (4-tert-octylphenol, technical nonylphenol isomers, 4-nonylphenol) and bisphenol-A. The methodology consisted of a quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction followed by liquid chromatography (LC) coupled to the hybrid LTQ/Orbitrap mass spectrometer (MS). The high resolution (HR) analysis provided the required selectivity demonstrating excellent sensitivity and enabled the high-mass accuracy of the analytes within short time of analysis, after a chemometric optimization of the instrument parameters. An experimental design was employed for the estimation of the effect of different parameters on the QuEChERS extraction efficiency to obtain the optimum conditions. Method validation proved that analysis exhibited excellent linearity (R2 > 0.9966), low enough precision (0.6 to 13.3%) and recoveries in the range of 91 to 108%. Limits of detection (LOD < 6.5 ng g−1) and quantification (LOQ < 20 ng g−1) as well as matrix effects (ME) were also evaluated. The optimized method was successfully applied to analyze dairy commodities varying in fat content and packaging material including milk, yogurts and infant formulae. Detected concentration levels (MDL-10.4 ng g−1) for bisphenol-A BPA in milk samples resulted in 0.36% of TDI for the medium case (average BPA concentrations) and 1.15% of TDI for the worst case (maximum BPA concentration).
Highlights
Over the last few years, the exposure levels and the associated effects of endocrine disrupting chemicals (EDCs) on the environment, wildlife and humans has received increased awareness [1,2]
Concerning bisphenol A (BPA), it is a high-production volume chemical mainly used as an important precursor for the production of several resins and polymers used in food packing materials
To perform QuEChERS extraction, Teflon centrifuge tubes of 15 mL and 50 mL were used while the salt-sorbent materials included anhydrous magnesium sulphate (MgSO4), LiChroprep RP-18 (40–64 μm) and tri-sodium citrate dehydrate purchased from Merck KGaA (Darmstadt, Germany); sodium acetate and sodium chloride (NaCl) of analytical reagent grade from Riedel de Haën (Hannover, Germany); sodium citrate dibasic sesquihydrate from Sigma-Aldrich (Bellefonte, PA, USA); bondesil-primary secondary amine (PSA; 40 μm) and SampliQ Carbon SPE (GCB, graphitized carbon black) from Agilent Technologies (Waldbronn, Germany)
Summary
Over the last few years, the exposure levels and the associated effects of endocrine disrupting chemicals (EDCs) on the environment, wildlife and humans has received increased awareness [1,2]. The long overdue list of EDCs includes estrogen mimic compounds such as bisphenol A (BPA), 4-tert-octylphenol (OP) and nonylphenol isomers, known widely as industrial chemicals. They present multiple modes of endocrine disruption activity, with the most emphasized being the binding to the estrogen receptors (estrogen receptors α and β) and acting competitively towards regular hormones (e.g., 17 β–estradiol). Concerning BPA, it is a high-production volume chemical mainly used as an important precursor for the production of several resins and polymers used in food packing materials. One of the main sources of exposure to BPA and APs for newborns and infants derive from migration from the lining of cans into infant formulas (IF) and from the polycarbonate baby bottles [9]
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