A Simple, Efficient, Eco-Friendly Sample Preparation Procedure for the Simultaneous Determination of Hormones in Meat and Fish Products by Gas Chromatography—Mass Spectrometry

Abstract

Food safety can be severely compromised by the presence of chemical contaminants. This has raised a pressing need to develop efficient analytical methods for their determination at very low levels in complex food matrices. In this manuscript, we developed a simple, sensitive, fast, green analytical method for the determination of thirteen natural and synthetic hormones from different families including progestogens, estrogens and androgens in meat and fish products. The method involves direct extraction with a (9:1) acetonitrile−water mixture and subsequent purification of the extract by semi-automated solid-phase extraction on a sorbent column (hydrophilic−lipophilic copolymer of N-vinylpyrrolidone and divinylbenzene). This treatment enriches samples with the target compounds while removing proteins, lipids and other potential interferences from their matrix for the accurate determination of the analytes by gas chromatography−mass spectrometry, all within 15 min. The proposed method exhibits good linearity (r ≥ 0.996), low limits of detection (0.4–15 ng/kg), acceptable recoveries (90–105%) and relative standard deviations (≤7%); in addition, it is scarcely subject to matrix effects (1–20%). The method was successfully used to determine natural and synthetic hormones in meat and fish products from Spain, Portugal, Italy, Germany, Greece, Norway, Morocco and the USA. The analytes were found at especially high levels (30−1900 ng/kg) in mussels, beef and pork.