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

General Chemical State Laboratory of Greece, Athínai, Attica, Greece
Journal of Chromatography A (Impact Factor: 4.17). 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.

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Available from: Nikolaos S. Thomaidis, Sep 28, 2015
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    • "In contrast, the polymeric sorbent ENV + (hydroxylated polystyrene-divinylbenzene) has been used for the extraction of highly polar compounds from water (Majzik et al., 2006). Octadecyl-bonded silica sorbents have proven superior for low polarity compounds such as BPA (Maragou et al., 2006; Samaras et al., 2011). The other sorbent tested was ENVI-Carb, a graphitized carbon black sorbent that retains nonpolar compounds in addition to highly polar compounds such as alcohols, nitrophenols, perfluorinated carboxylic acids, and relatively polar herbicides (carbamates, phenylureas and phenoxy acids) with no need to adjust the pH of the sample (Seen et al., 2014). "
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    ABSTRACT: Bottled water consumption is a putative source of human exposure to endocrine-disrupting chemicals (EDCs). Research has been conducted on the presence of chemicals with estrogen-like activity in bottled waters and on their estrogenicity, but few data are available on the presence of hormonal activities associated with other nuclear receptors (NRs). The aim of this study was to determine the presence of endocrine activities dependent on the activation of human estrogen receptor alpha (hERa) and/or androgen receptor (hAR) in water in glass or plastic bottles sold to consumers in Southern Spain. Hormone-like activities were evaluated in 29 bottled waters using receptor-specific bioassays based on reporter gene expression in PALM cells [(anti-)androgenicity] and cell proliferation assessment in MCF-7 cells [(anti-)estrogenicity] after optimized solid phase extraction (SPE). All of the water samples analyzed showed hormonal activity. This was estrogenic in 79.3% and anti-estrogenic in 37.9% of samples and was androgenic in 27.5% and anti-androgenic in 41.3%, with mean concentrations per liter of 0.113 pM 17β-estradiol (E2) equivalent units (E2Eq), 11.01 pM anti-estrogen (ICI 182780) equivalent units (ICI 182780Eq), 0.33 pM methyltrienolone (R1881) equivalent units (R1881Eq), and 0.18 nM procymidone equivalent units (ProcEq). Bottled water consumption contributes to EDC exposure. Hormone-like activities observed in waters from both plastic and glass bottles suggest that plastic packaging is not the sole source of contamination and that the source of the water and bottling process may play a role, among other factors. Further research is warranted on the cumulative effects of long-term exposure to low doses of EDCs.
    Environment International 01/2015; 74. DOI:10.1016/j.envint.2014.10.006 · 5.56 Impact Factor
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    • "beverages or foods that have been in contact with polycarbonate plastic containers or epoxy resins in 76 food packaging (Kubwabo et al., 2009; Maragou et al., 2006; Lopez-Espinosa et al., 2007). BPA is 77 readily chlorinated by reaction with residual chlorine molecules, e.g. "
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    ABSTRACT: The aim of this study is to obtain data on the exposure of non-breast-fed infants to polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/F), polychlorinated biphenyls (PCB), organochlorine pesticides (OCP), and bisphenol A (BPA) and its chlorinated derivatives through consumption of commercial infant foods with largest shares of the market in 22 European Union countries. The E-Screen bioassay was employed to assess the oestrogenicity of the baby foods and the ethoxyresorufin-O-deethylase (EROD) induction was measured to determine the levels of PCDD/F and PCB. Consequently, the highest total effective xenoestrogen burden (TEXB) of 73.60 pM Eeq g(-1) was found in the soy-based formula and the EROD bioassay was always below the limit of quantification (LOQ) (3.5 pg g(-1)). Overall, the estimated dietary exposure to BPA via commercial baby foods was lower than the tolerable daily intake (TDI) of 50 µg kg(-1) body weight (bw). Furthermore, the findings indicated that the dietary exposure of 0-9-month-old infants through the products investigated here does not exceed the maximum TDI of 4 pg WHO-TEQ (toxic equivalents) kg(-1) bw. However, exposure to more than 2 pg WHO-TEQ kg(-1) bw day(-1) might occur for 0-4-month-old infants consuming 'starting' hypoallergenic formula. Moreover, analysis of OCP indicated that the dietary exposure of non-breast-fed infants was not harmful. Considering the importance of early development and the vulnerability of infants and children, it is essential to determine their dietary exposure to contaminants in order to decide which efforts of risk reduction should receive highest priority.
    Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment 06/2011; 28(8):1110-22. DOI:10.1080/19440049.2011.583281 · 1.80 Impact Factor
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    • "Fig. 2 shows the product ion scan of BPA, OP and NP using LC–MS/MS. Although the relative abundance of the product ions depends on the collision energy used, other authors (Maragou et al., 2006; Shao et al., 2005) (to monitor BPA), choose the same transitions to monitor these compounds , and, explaining that the BPA fragment ion at m/z 212 is related to the loss of the CH 3 group from the deprotonated molecule, and the OP and NP fragment ion at m/z 106 indicated the loss of C 7 H 16 (for OP) and C 8 H 18 (for NP) groups from the deprotonated molecule. To detect the trace levels of these compounds, multiple-reaction monitoring (MRM) mode has been used. "
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    ABSTRACT: a b s t r a c t A new analytical method, using pressurised liquid extraction (PLE) and liquid chromatography–tandem mass spectrometry (LC–MS/MS), was developed for the simultaneous determination of bisphenol A (BPA), octylphenol (OP) and nonylphenol (NP) in powdered infant formulas (IF) and powdered skimmed milk (PM). The analytes were extracted by PLE, using this optimised conditions: ethyl acetate as solvent, 70 °C of temperature, reversed-phase silica C 18 as dispersing agent and three cycles of extraction. The extracts were then injected in LC–MS/MS using a Gemini C 18 column and a mixture of 5% water and 95% methanol/acetonitrile, both with 0.1% ammonia, as a mobile phase. Recoveries at different fortifica-tion levels (0.5 and 0.05 mg kg À1), were between 89% and 92% for BPA, 84 and 98% for OP, and 93% and 101% for NP. The method was applied to the analysis of samples of PM and IF, bought in Italian and Span-ish markets. In positive samples, phenols concentration ranged from 0.07 to 1.29 mg kg À1 for BPA, from 0.028 to 1.55 mg kg À1 for OP and from 0.026 to 1.47 mg kg À1 for NP.
    Food Chemistry 10/2010; 126(1). DOI:10.1016/j.foodchem.2010.10.098 · 3.39 Impact Factor
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