Abstract
In the present study, the ammonium formate version of the QuEChERS method, considered highly advantageous in relation to instrument maintenance and other issues, was applied for the first time to extract a group of twelve phthalic acid esters (PAEs, i.e. dipropyl phthalate, DPP; diisobutyl phthalate, DIBP; dibutyl phthalate, DBP; diisopentyl phthalate, DIPP; di-n-pentyl phthalate, DNPP; dihexyl phthalate, DHP; butyl benzyl phthalate, BBP; dicyclohexyl phthalate, DCHP; di(2-ethylhexyl) phthalate, DEHP; di-n-octyl phthalate, DNOP; diisononyl phthalate, DINP; and diisodecyl phthalate, DIDP) and one adipate (di(2-ethylhexyl) adipate, DEHA) from two species of fish (Scomber colias and Katsuwonus pelamis) and one of squid (Loligo gahi). The method was validated in terms of linearity, trueness and matrix effects. Determination coefficients (R2) for matrix-matched calibration curves were higher than 0.99 in all cases, being the lowest calibration levels in the range 0.5–10 ng/g. Mean recovery values were between 70 and 117% with relative standard deviation values ≤20%. Matrix effects were soft (between −20 and +20%) for most analytes and matrices, except in squid samples, which was mostly medium with a moderate ion suppression. The analysis of 10 samples of each type showed the presence of DIBP, DBP and DEHP at concentrations up to 44.2 ± 2.1 ng/g of wet weight in some of the samples and species, still not representing concerning values when considering the daily intake of such species of seafood in the human diet (tolerable daily intake -TDI- values were not exceeded). Results demonstrated that the ammonium formate version of the QuEChERS method can be applied with success for the extraction and determination of the selected PAEs and DEHA in fish and squid samples.
Highlights
Phthalic acid esters (PAEs) are manufactured chemicals which were first introduced in the 1920s
Many public organizations/administrations have initiated actions to control/limit their use. This is the case of the EU, which banned di(2-ethylhexyl) phthalate (DEHP), dibutyl phthalate (DBP) and benzyl butyl phthalate (BBP) in all toys and childcare articles, and diisononyl phthalate (DINP), diisodecyl phthalate (DIDP) and di-noctyl phthalate (DNOP) in those articles that children could take to their mouth (The European Comission, 2006)
The EU through its REACH regulation restricted the use of the four phthalates DEHP, DBP, diisobutyl phthalate (DIBP), and BBP coming into force in July 2020 (The European Comission, 2018), due to their demonstrated endocrine disrupting properties with effects on human health (Endo crine, 2019)
Summary
Phthalic acid esters (PAEs) are manufactured chemicals which were first introduced in the 1920s. Some of them are used as solvents and fragrances fixers, as well as additives in medical devices, household, cosmetics and personal care products (Katsikantami et al, 2016) Since they are not chemically bonded to the polymeric matrix, they migrate to their surrounding environment and, as a result, they are considered ubiquitous chemicals (Fasano, Cirillo, Espo sito, & Lacorte, 2015; Katsikantami et al, 2016). Many public organizations/administrations have initiated actions to control/limit their use This is the case of the EU, which banned di(2-ethylhexyl) phthalate (DEHP), dibutyl phthalate (DBP) and benzyl butyl phthalate (BBP) in all toys and childcare articles, and diisononyl phthalate (DINP), diisodecyl phthalate (DIDP) and di-noctyl phthalate (DNOP) in those articles that children could take to their mouth (The European Comission, 2006). In 2011 and 2012, these PAEs were identified as substances of very high concern (SVHCs) and added to the EU authorization list for being toxic and affecting reproduction mechanisms (European Chemicals Agency, 2021)
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