Simultaneous determination of bisphenol A and bisphenol B in beverages and powdered infant formulae by dispersive liquid-liquid microextraction and heart-cutting multidimensional gas chromatography-mass spectrometry - Archive ouverte HAL Accéder directement au contenu
Article Dans Une Revue Food Additives and Contaminants Année : 2011

Simultaneous determination of bisphenol A and bisphenol B in beverages and powdered infant formulae by dispersive liquid-liquid microextraction and heart-cutting multidimensional gas chromatography-mass spectrometry

Sara Cunha
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Résumé

The purpose of this study was to establish a reliable, cost-effective, fast and simple method to quantify simultaneously both bisphenol A (BPA) and bisphenol B (BPB) in liquid food matrixes such as canned beverages (soft drinks and beers) and powdered infant formulae using dispersive liquid-liquid microextraction (DLLME) with in situ derivatization coupled with heart-cutting gas chromatography-mass spectrometry (GC-MS). For the optimization of the DLLME procedure different amounts of various extractive and dispersive solvents as well as different amounts of the derivative reagent were compared for their effects on extraction efficiency and yields. The optimised procedure consisted in the injection of a mixture containing tetrachloroethylene (extractant), acetonitrile (dispersant) and acetic anhydride (derivatizing reagent) directly into an aliquot of beverage samples or into an aqueous extract of powdered milk samples obtained after a pretreatment of the samples. Given the compatibility of the solvents used, and the low volumes involved, the procedure was easily associated with GC-MS end-point determination, which was accomplished by means of an accurate GC dual column (heart-cutting) technique. Careful optimization of heart-cutting GC-MS conditions, namely pressure of front and auxiliary inlets, have resulted in a good analytical performance. The linearity of the matrix-matched calibration curves was acceptable, with coefficients of determination (R2) always higher than 0.99. Average recoveries of the BPA and BPB spiked at two concentration levels into beverages and powdered infant formulae ranged from 68% to 114% and the relative standard deviation (RSD) was < 15%. The limits of detection (LOD) in canned beverages were 5.0 and 2.0 ng L-1 for BPA and BPB, respectively, whereas LOD in powdered infant formulae were 60.0 and 30.0 ng L-1, respectively. The limits of quantification (LOQ) in canned beverages were 10.0 and 7.0 ng L-1 for BPA and BPB, respectively, whereas LOQ in powdered infant formulae were 200.0 and 100.0 ng L-1, respectively. BPA was detected in 21 of 30 canned beverages (ranging from 0.03 to 4.70 µg L-1) and in 2 of 7 powdered infant formulae samples (0.23 and 0.40 µg L-1) collected in Portugal. BPB was only detected in canned beverages being positive in 15 of 30 samples analysed (ranging from 0.06 to 0.17 µg L-1). This is the first report about the presence of BPA and BPB in canned beverages and powdered infant formulae in the Portuguese market.

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Dates et versions

hal-00659525 , version 1 (13-01-2012)

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Sara Cunha. Simultaneous determination of bisphenol A and bisphenol B in beverages and powdered infant formulae by dispersive liquid-liquid microextraction and heart-cutting multidimensional gas chromatography-mass spectrometry. Food Additives and Contaminants, 2011, pp.1. ⟨10.1080/19440049.2010.542551⟩. ⟨hal-00659525⟩

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