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Development and validation of an analytical methodology for the determination of p,p′-DDT, p,p′-DDE and p,p′-DDD in fish oil pills
Authors:Juan Jos Berzas Nevado  Rosa Carmen Rodríguez Martín-Doimeadis  Francisco Javier Guzmn Bernardo  Nuria Rodríguez Farias
Institution:aDepartment of Analytical Chemistry and Food Technology, University of Castilla-La Mancha, Spain;bFaculty of Chemical Sciences, Av. Camilo José Cela, 9. E-13071, Ciudad Real, Spain;cFaculty of Environmental Sciences, Avda. Carlos III, s/n. E-45071, Toledo, Spain
Abstract:An analytical methodology was proposed and validated to be applied to the determination of p,p′-DDT and its metabolites p,p′-DDE and p,p′-DDD in fish oil. The analytical procedure presented in this paper involves a single-step clean up process prior to the analysis. A solution of 1,2,3,4-tetrachloronaphtalene was used as internal standard.The analytical technique used was gas chromatography coupled to an electron capture detector. Details on the validation process are provided.The limits of detection ranged from 2.6 to 4.7 pg μL− 1. The BCR 598 standard reference material (cod liver oil) was used to evaluate the performance of the methodology with satisfactory recoveries for all the compounds.The analytes were determined in three different fish oil pills sold in Spain as a supplementary vitamin support. The sum of p,p′-DDT and metabolites was from 13.2 to 51.3 ng g− 1, the dominant compound being p,p′-DDE.
Keywords:Fish oil  DDT  DDD  DDE  Gas chromatography  Electron capture detector
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