Development and Validation of a Three Liquid Phase Extraction Method for Simultaneous Determination of Phthalates and Bisphenols in Seafood by GC–MS
摘要
A three-phase liquid extraction (TLPE) approach was developed and validated for the simultaneous determination of phthalates and bisphenols in seafood using gas chromatography–mass spectrometry (GC–MS). The most optimized TLPE system consisted of a mixture of hexane, dimethylformamide, and water added with Na2SO4 salt in a volume ratio of 2:4:4 (v/v/v), under neutral pH conditions at room temperature. The method achieved limits of detection ranging from 0.0071 to 0.0330 μg g⁻1 for six phthalates and from 0.0400 to 0.0513 μg g⁻1 for two bisphenols in mussel matrices. Recoveries in spiked mussel, shrimp, fish, and squid samples were found to be within the ranges of 68.1–73.1%, 63.4–69.0%, 62.1–69.5%, and 62.5–68.4%, respectively, with relative standard deviations below 3%. Inter-day precision values were 1.03–2.62%. Analysis of real samples demonstrated the presence of di(2-ethylhexyl) phthalate (DEHP) as a matrix contaminant in most samples, ranging from 0.0575–0.1125 μg g−1. Dibutyl phthalate (DBP), benzyl butyl phthalate (BBP) and di-n-octyl phthalate (DnOP) were found in some samples. In comparison to other extraction methods, the proposed TLPE showed superiority in terms of simultaneous extraction in a single step, low solvent consumption, small sample amount, ease of extraction, utilization of cost-effective and widely available equipment, and reduced overall extraction time.