Dubois Mathieu, Empl Anna-Maria, Jaudzems Greg, Basle Quentin, Konings Erik
Nestlé Research, 57 Route du Jorat, Vers-chez-les-Blanc, Lausanne 1000, Switzerland.
Nestlé Quality Assurance Center, 1 Menninger St, Polling 84570, Germany.
J AOAC Int. 2019 May 1;102(3):903-914. doi: 10.5740/jaoacint.18-0266. Epub 2018 Nov 26.
Monochloropropanediol (MCPD) and its fatty acid esters as well as glycidyl fatty acid esters are substances generated during oil refining or food processing. The free form released during digestion, 3-MCPD and glycidol, have shown adverse effects in animal studies. So far, the available analytical methods have not been validated in a collaborative study for infant and adult nutritional formulas. This manuscript describes a single-laboratory validation method in view of a future multilaboratory validation trial. The method described is for the direct determination of 2- and 3-MCPD and indirect determination of 2- and 3-MCPD esters and glycidyl esters in infant and adult/pediatric nutritional formulas by GC coupled to MS. The analytical range was found to be 4-2000 μg/kg powder formula and 0.7-333 μg/kg liquid formula for fatty acid esters of MCPD and glycidol, and 2.5-750 μg/kg samples for free MCPD. The recovery rates were within 91-124% for all samples. Repeatability precision was <20% at levels close to the LOQ. The results met the (SMPR) set by the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals. The AOAC Expert Review Panel approved the present method as AOAC 2018.03.
3-氯-1,2-丙二醇(MCPD)及其脂肪酸酯以及缩水甘油脂肪酸酯是在炼油或食品加工过程中产生的物质。在消化过程中释放出的游离形式,即3-MCPD和缩水甘油,在动物研究中已显示出不良影响。到目前为止,现有的分析方法尚未在婴儿和成人营养配方食品的协同研究中得到验证。鉴于未来的多实验室验证试验,本手稿描述了一种单实验室验证方法。所描述的方法用于通过气相色谱-质谱联用直接测定婴儿和成人/儿科营养配方食品中的2-和3-MCPD,并间接测定2-和3-MCPD酯以及缩水甘油酯。发现MCPD和缩水甘油脂肪酸酯的分析范围为4-2000μg/kg粉末配方食品和0.7-333μg/kg液体配方食品,游离MCPD的分析范围为2.5-750μg/kg样品。所有样品的回收率在91-124%之间。在接近定量限的水平下,重复性精密度<20%。结果符合AOAC婴儿配方食品和成人营养成分利益相关者小组设定的性能特征要求(SMPR)。AOAC专家评审小组批准本方法为AOAC 2018.03。