A LC–MS/MS method for the determination of BADGE-related and BFDGE-related compounds in canned fish food samples based on the formation of [M+NH₄]⁺ aducts
2012
Míguez, J. | Herrero, C. | Quintás, I. | Rodríguez, C. | Gigosos, P.G. | Mariz, O.C.
A new and simple liquid chromatography tandem mass-spectrometry method for the determination of different bisphenol A (BPA) derivatives such as bisphenol A diglycidyl ether (BADGE), bisphenol F diglycidyl ether (BFDGE) and their reaction products with water and hydrochloric acid in different fish food products was developed. The extraction procedure and the chromatographic conditions were optimised for complex food matrices such as fish products. Food samples were homogenised and extracted with a 1:1 solution of acetonitrile-hexane, the solvent was eliminated in a N₂ stream and the extract was reconstituted with 0.5mL of a 0.01M solution of ammonium formate. The sample solution obtained was directly measured by LC–MS/MS without any further purification under the developed conditions. The use of a mobile phase composed by ammonium formate–methanol in a binary gradient mode produced [M+NH₄]⁺ aducts for the different BADGEs and BFDGEs. These aduct’s fragmentations were employed for the LC–MS/MS quantification of BPA derivatives in canned fish samples. The results of the validation were appropriate: the method was linear for BADGE and its hydrolysed derivatives up to 1000μgkg⁻¹, for the remaining compounds linearity achieved up to 100μgkg⁻¹. Quantification limits were in the range 2–10μgkg⁻¹. RSD (intra and inter-day) was 6–12% and the recovery was comprised between 89% and 109%. Under the optimised conditions, the chromatographic separation was performed in 8min per sample. The method was applied to the determination of BADGE, BFDGE and their reaction products in different samples of canned fish from Spanish origin. Migration results obtained were in compliance with the EU regulations.
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