科研之友
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摘要
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 (GCMS/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 degrees C. The use of GCMS/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 III columns (15 mx 0.25 mu m x 0.25 mm) 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 100 ng g(-1) and 50 ng g(-1) for 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.
- 出版日期2017-4-1
