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Several food contact articles (FCAs) contaminated with unapproved brominated flame retardants (BFRs) purchased in the US market were analysed and subjected to migration tests. Migration tests were performed in food simulants (water, 3% acetic acid, 10% ethanol and 50% ethanol) and food (milk, coffee and chicken bouillon soup) to evaluate the BFRs mass transfer from the contaminated FCA. The BFRs studied, 2,4,6-tribromophenol (TBP), 3,3',5,5'-tetrabromobisphenol A (TBBPA), and 1,2,5,6,9,10-hexabromocyclododecane (HBCD) were analysed by UHPLC-MS/MS. The method validation parameters were r 2  ≥ 0.999, LOD ≤ 0.3 ng mL -1 , and RSD ≤ 1.7 % (n = 7). HBCD was not stable under our migration conditions and was not detected in any FCA, food or food simulant, including positive controls. Phenolic BFRs (TBP and TBBPA) migrated at concentrations ranging from non-detected to 73 µg kg -1 in food simulants, and from 1 to 23 µg kg -1 in food. Phenolic BFRs migrated into 50% ethanol food simulant at higher concentrations than in more aqueous food simulants and foods.

Traditionally, migration testing during 10 days at 40 °C has been considered sufficient and appropriate for simulating the potential migration of substances from food-contact materials into foods. However, some packages, such as food cans, may be stored holding food for extended time periods (years). This study attempts to verify whether common testing conditions accurately estimate long-term migration. Two types of can coatings, epoxy and acrylic-phenolic, were subjected to short-term and long-term migration testing (1 day-1.5 years) using food simulants (water, 3% acetic acid, 50% ethanol, and isooctane) at 40 °C. Using HPLC-DAD/CAD, HPLC-MS, UHPLC-HRMS (where HRMS is accurate mass, mass spectrometry), and DART-HRMS, we identified potential migrants before starting the experiment: BPA, BADGE, BADGE derivatives, benzoguanamine, and other relevant marker compounds. During the experiment using a water-based food simulant, migrants remained stable. Most of the cans in contact with 3% acetic acid did not survive the experimental conditions. Tracked migrants were not detected in isooctane. In the presence of 50% ethanol, the traditional migration test during 10 days at 40 °C did not predict migration during long-term storage. These results suggest that migration protocols should be modified to account for long-term storage.

Metal food and drink cans are commonly coated with epoxy films made from phenolic polymers produced from bisphenol A (BPA). It is well established that residual BPA monomer migrates into can contents during processing and storage. While a number of studies have reported BPA concentrations in foods from foreign markets and specialty foods on the U.S. market, very few peer-reviewed data for the BPA concentrations in canned food from the U.S. market were available. This study quantified BPA concentrations in 78 canned and two frozen food products from the U.S. market using an adaptation of a previously reported liquid chromatography-tandem mass spectrometry method. The tested products represented 16 different food types that are from the can food classifications that constitute approximately 65% of U.S. canned food sales and canned food consumption. BPA was detected in 71 of the 78 canned food samples but was not detected in either of the two frozen food samples. Detectable BPA concentrations across all foods ranged from 2.6 to 730 ng/g. Large variations in BPA concentrations were found between different products of the same food type and between different lots of the same product. Given the large concentration ranges, the only distinguishable trend was that fruits and tuna showed the lowest BPA concentrations. Experiments with fortified frozen vegetables and brine solutions, as well as higher BPA concentrations in canned food solids over liquid portions, clearly indicated that BPA partitions into the solid portion of foods.

Two unknown compounds were previously determined to be potential interferences in liquid chromatography/tandem mass spectrometry (LC/MS/MS) analysis of bisphenol A (BPA) in canned infant formula. Both yielded two identical MS/MS transitions to BPA. The identities of the unknowns were investigated using accurate mass LC/MS, LC/MS/MS, and elemental formula and structures proposed. Exact identities were confirmed through purification or synthesis followed by (1)H and (13)C nuclear magnetic resonance (NMR) experiments, as well as comparisons of one unknown with commercial standards. Comparisons of negative ion electrospray ionization (ESI) MS/MS and accurate mass spectra suggested both unknowns to be structurally identical (to BPA and each other). Positive ion ESI spectra confirmed both were larger molecules, suggesting that in the negative mode they likely fragmented to the deprotonated BPA ion in the source [corrected]. Elemental composition of positive ion accurate mass spectra and NMR analysis concluded the unknowns were oxidized forms of the known epoxy can coating monomer, bisphenol A diglycidyl ether (BADGE). One of the unknowns, 2,2-[bis-4-(2,3-dihydroxypropoxy)phenyl]propane, commonly known as BADGE*2H(2)O, is widely reported as an epoxy-phenolic can coating migrant, but has not been suggested to interfere with the MS/MS analysis of BPA. The other unknown, 2-[4-(2,3-dihydroxypropoxy)phenyl]-2-[4'-hydroxyphenyl]propane, or the oxidized form of bisphenol A monoglycidyl ether (BAMGE*H(2)O), has not been previously reported in food or packaging., (Published in 2011 by John Wiley & Sons, Ltd.)

An updated survey of U.S. infant formula was conducted to determine the concentrations of bisphenol A (BPA). The purpose was to accurately assess BPA concentrations across the infant formula market, accounting for lot variability, and determine if geographic location or can age influences BPA concentrations. A method was developed to measure BPA in formula utilizing isotope dilution, solid-phase extraction, and liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The method was tested and found to be reproducible (10% relative standard deviation), reliable (47 +/- 1% recovery), and sensitive (0.15 ng g(-1) method detection limit). Over 160 analyses were conducted using 104 formula containers representing 36 products. Samples from U.S. east and west coast markets demonstrated no significant difference, and concentrations in older cans were not higher. BPA concentrations in liquid formula (0.48-11 ng g(-1)) were consistent with previous studies, and BPA was detected in only 1 of 14 powder formula products analyzed.