Article

Determination of bisphenol A in milk by solid phase extraction and liquid chromatography-mass spectrometry.

Laboratory of Analytical Chemistry, Department of Chemistry, University of Athens, Panepistimioupolis Zografou, Athens, Greece.
Journal of Chromatography (Impact Factor: 4.61). 10/2006; 1129(2):165-73. DOI:10.1016/j.chroma.2006.06.103
Source: PubMed

ABSTRACT A simple and reliable analytical method based on solid phase extraction (SPE) and liquid chromatography coupled with electrospray ionization mass spectrometry was developed for the determination of bisphenol A (BPA) in milk. The effects of the experimental parameters of the LC-ESI-MS system (mobile phase and additives, flow rate, temperature of the ionization source, cone voltage and capillary potential) on the obtained signal were assessed and the parameters were optimized to provide maximum sensitivity and detectability. In addition, the performance of three commercial SPE sorbents (C18, PS-DVB and hydroxylated PS-DVB) was evaluated using spiked water and milk, diluted with a mixture of water-methanol (8:1). By using C18 cartridges and BPA-d(16) as internal standard, the mean relative recoveries at three fortification levels ranged between 97 and 104% and the corresponding inter-day precision (RSD%) was below 6% for 50 and 500 ng/g and below 20% for 5 ng/g fortification levels. It is shown that the ion suppression during ESI, the losses from the sample preparation procedure and the inter-day instability of LC-ESI-MS were overcome by the use of the deuterated internal standard. The concentration of BPA found in commercial canned milk samples ranged from <1.7 to 15.2 ng/g.

0 0
 · 
0 Bookmarks
 · 
89 Views
  • [show abstract] [hide abstract]
    ABSTRACT: A selective and highly sensitive liquid chromatography-tandem mass spectrometry method has been developed and validated for determination of Bisphenol A (BPA) in human urine using labeled d6-BPA as internal standard. BPA was purified from human urine by affinity chromatography on solid extraction AFFINIMIP® Bisphenol A cartridges, based on molecularly imprinted polymers. After purification, the samples were analyzed on a Phenomenex Kinetex 100 × 4.6 mm, 2.6 μm particle PFP reversed-phase HPLC column, coupled to a triple quadrupole mass spectrometer by an electrospray ion source. Analyses were performed in the multiple reaction monitoring mode and negative ionization; the product ions at 133.2 and 212.1 m/z for BPA and at 138.2 and 215.0 m/z for d6-BPA were monitored to assess unambiguous identification. The linearity of the detector response was verified in human urine over the concentration range 0.100-200 ng/mL. The detection limit was calculated as 0.03 ng/mL and the limit of quantification of the method is 0.10 ng/mL. This LC/ESI-MS/MS method was in-house validated evaluating specificity, trueness, within-day and between-days precision. The mean recoveries of BPA from spiked urine samples were higher than 94 % and good reproducibility (relative standard deviations ≤ 8.1 %) was observed. The developed method was applied to a pilot study involving 105 children, aged from 6 to 14 years (16 normal weight and 89 obese children), from the Regione Campania (Southern Italy). The aim of this study was to determine the concentrations of BPA in urine of children and possible correlations with childhood obesity.
    Analytical and Bioanalytical Chemistry 09/2013; · 3.66 Impact Factor
  • [show abstract] [hide abstract]
    ABSTRACT: Food safety can be compromised by the presence of a wide variety of substances, deriving from both natural and anthropogenic sources. Among these substances, compounds exhibiting various degrees of estrogenic activity have been widely studied in environmental samples, whereas less attention has been devoted to food matrices. The aim of the present review is to give a general overview on the recent analytical methods based on gas or liquid chromatography coupled to mass spectrometry for the determination of estrogen-like compounds in foods, including new developments, improvements and upcoming trends in the field. Attention will be focused on four representative groups of compounds, i.e. natural and synthetic estrogens, mycoestrogens, phytoestrogens, and alkylphenols.
    Journal of chromatography. A 06/2013; · 4.19 Impact Factor
  • [show abstract] [hide abstract]
    ABSTRACT: Enzyme-linked immunosorbent assays (ELISAs) are investigated in this work for the detection of bisphenol-A (BPA), a plastic monomer and a critical contaminant in food and environment. A series of polyclonal antibodies generated in vivo using BPA-butyrate-protein conjugate and BPA-valerate-protein conjugate were evaluated on direct and indirect competitive assay formats with five competing haptens (BPA-butyrate, BPA-valerate, BPA-crotonate, BPA-acetate, and BPA-2-valerate). Two indirect ELISAs and one direct ELISA exhibiting high sensitivity and specificity for BPA were developed. The 50 % inhibition of antibody binding (IC(50)) values were 0.78 ± 0.01-1.20 ± 0.26 μg L(-1), and the limits of detection as measured by the IC(20) values were 0.10 ± 0.03-0.20 ± 0.04 μg L(-1). The assays were highly specific to BPA, only displaying low cross-reactivity (3-8 % for the indirect assays and 26 % for the direct assay) for 4-cumylphenol (4-CP), at pH 7.2. The degree of cross-reaction of 4-CP was influenced by the antibody/hapten conjugate combination, assay conditions, and the assay format. The assays were optimized for the analysis of BPA in canned vegetables, bottled water and carbonated drinks. The limits of quantification for these three evaluated sample types, based on the spike and recovery data, were 0.5, 2.5, and 100 μg L(-1), respectively.
    Analytical and Bioanalytical Chemistry 04/2012; 403(6):1607-18. · 3.66 Impact Factor

Full-text

View
109 Downloads
Available from
Feb 19, 2013