Garballo-Rubio A, Soto-Chinchilla J, Moreno A, Zafra-Gómez A
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.
Department of Analytical Services - Biosearch S.A., Camino de Purchil 66, E-18004 Granada, Spain.
Talanta. 2017 Apr 1;165:267-273. doi: 10.1016/j.talanta.2016.12.060. Epub 2016 Dec 23.
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 and 50ngg 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.
如今，食品安全是最重要的全球性问题之一，食品质量控制以及食品和饮料中污染物的识别对于人类健康和安全至关重要。本文验证了一种通过气相色谱串联质谱法（GC-MS/MS）同时测定冬化和未冬化鱼油样品中3-一氯丙二醇（3-MCPD）和缩水甘油酯的新型单步方法。该方法基于室温下酯的碱性水解，仅使用3-MCPD-d5作为内标，并在90°C下用苯硼酸（PBA）进行衍生化步骤。使用GC-MS/MS简化了样品处理，提高了分析方法的定量限和精密度，无需对提取物进行额外浓缩。在两根HP-5 MS UI柱（15m×0.25µm×0.25mm）之间放置了一个反吹三通，以尽量减少常规分析中通常观察到的基质效应和峰形降解。该方法在冬化和未冬化鱼油中得到验证，3-MCPD和缩水甘油的定量限分别为100ng/g和50ng/g。通过将我们实验室的结果与认可的参考实验室（德国SGS有限公司）获得的结果进行比较，并计算加标样品测定中的回收率来完成方法验证。对于缩水甘油的定量，开发了一个数学方程以补偿3-MCPD向缩水甘油的部分转化。该表达式涉及水解反应过程中生成的3-MBPD-d5的定量。
