Kuhlmann Jan
SGS Germany GmbH, Weidenbaumsweg 137, D-21035 Hamburg, Germany.
J AOAC Int. 2019 Jul 1;102(4):1205-1220. doi: 10.5740/jaoacint.19-0026. Epub 2019 Apr 16.
Fatty acid esters of glycidol, 2-Monochloropropanediol (MCPD), and 3-MCPD are heat-induced foodborne processing contaminants with possible adverse health effects. These compounds occur frequently in refined edible oils. Consequently, glycidyl esters and 2- and 3-MCPD esters might also be present in foods that contain refined edible oils. This manuscript describes the single-laboratory validation of an analytical method for the quantitative determination of glycidol, 2-MCPD, and 3-MCPD present as fatty acid esters or as free 2- or 3-MCPD in infant and adult/pediatric nutritional formula. Technically, the presented method is based on the combination of a Heat-Ultrasound Pressure-supported Solvent Extraction and a GC-MS determination of glycidol, 2-MCPD, and 3-MCPD. From a chemical perspective, the method includes an alkaline catalyzed transesterification, conversion of the unstable glycidol into monobromopropanediol, and the parallel derivatization of all analytes with phenylboronic acid. Validation results showed that method linearity for all analytes in powdered and liquid infant formula ranged from 0.9981 to 0.9999 ( = 18). Repeatability relative standard deviation values for concentration levels between 1.3 μg/kg and 331 μg/kg were in the range of 1 to 12%. Relative recoveries were found to be between 93 and 107%. The analytes were quantifiable down to 5-10 μg/kg in powdered samples and 1-2 μg/kg in liquid samples. The reported results met actual AOAC In terms of consumer protection, the presented method is a novel approach for the sensitive and accurate determination of glycidol, 2-MCPD, and 3-MCPD in infant formula and related foodstuffs.
缩水甘油脂肪酸酯、2-一氯丙二醇(MCPD)和3-一氯丙二醇是热诱导产生的食源性加工污染物,可能对健康产生不良影响。这些化合物在精炼食用油中频繁出现。因此,缩水甘油酯以及2-和3-MCPD酯也可能存在于含有精炼食用油的食品中。本手稿描述了一种分析方法的单实验室验证,该方法用于定量测定婴儿及成人/儿童营养配方奶粉中以脂肪酸酯形式或游离2-或3-MCPD形式存在的缩水甘油、2-MCPD和3-MCPD。从技术上讲,所提出的方法基于热超声压力辅助溶剂萃取与缩水甘油、2-MCPD和3-MCPD的气相色谱-质谱联用测定相结合。从化学角度来看,该方法包括碱催化的酯交换反应、将不稳定的缩水甘油转化为一溴丙二醇,以及所有分析物与苯硼酸的平行衍生化反应。验证结果表明,粉状和液态婴儿配方奶粉中所有分析物的方法线性范围为0.9981至0.9999(n = 18)。浓度水平在1.3μg/kg至331μg/kg之间时,重复性相对标准偏差值在1%至12%之间。相对回收率在93%至107%之间。粉状样品中分析物的可定量下限为5 - 10μg/kg,液态样品中为1 - 2μg/kg。所报告的结果符合实际的AOAC标准。就消费者保护而言,所提出的方法是一种用于灵敏且准确测定婴儿配方奶粉及相关食品中缩水甘油、2-MCPD和3-MCPD的新方法。