A novel method for the determination of glycidyl and 3-monochloropropanediol esters in fish oil by gas chromatography tandem mass spectrometry.
Today, food security is one of the most important global issues with food quality control and identification of contaminants in foods and beverages, being crucial for human health and safety. In this paper, a novel single-step method for the simultaneous determination of 3-monochloropropanediol (3-MCPD) and glycidyl esters in samples of winterized and non-winterized fish oil by using gas chromatography tandem mass spectrometry (GC-MS/MS) is validated. The method is based on alkaline hydrolysis of esters at room temperature, using only 3-MCPD-d5 as internal standard, and a derivatization step with phenylboronic acid (PBA) at 90°C. The use of GC-MS/MS results in a simplified sample treatment and improvement of the limits of quantification and precision of the analytical method with no need of additional concentration of the extracts. A backflush tee placed between two HP-5 MS UI columns (15m×0.25µm×0.25mm) was used in order to minimize matrix effects and peak shape degradation usually observed in routine analyses. The method was validated in winterized and non-winterized fish oil, achieving a limit of quantification of 100ngg-1and 50ngg-1for 3-MCPD and glycidol, respectively. Method validation was accomplished by comparing our laboratory results with results obtained by an accredited reference laboratory (SGS Germany GmbH) and by calculating the recoveries obtained in an assay with spiked samples. For glycidol quantification, a mathematical equation was developed in order to compensate for the partial conversion of 3-MCPD into glycidol. This expression involves the quantification of 3-MBPD-d5 generated during hydrolysis reaction.
Department of Analytical Services - Biosearch S.A., Camino de Purchil 66, E-18004 Granada, Spain; Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, University of Granada, Campus of Fuentenueva, E-18071 Granada, Spain.
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Garballo-Rubio
Department of Analytical Services - Biosearch S.A., Camino de Purchil 66, E-18004 Granada, Spain.
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Soto-Chinchilla
Department of Analytical Services - Biosearch S.A., Camino de Purchil 66, E-18004 Granada, Spain.
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Moreno
Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, University of Granada, Campus of Fuentenueva, E-18071 Granada, Spain. Electronic address: azafra@ugr.es.
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Zafra-Gómez
3-Monochloropropanediol, Glycidol; Fish oil; Food Safety; GC-MS/MS