Laboratory Department of Food and Environmental Chemistry, Central Institute of Medical Service, German Federal Armed Forces Koblenz, Andernacher Strasse 100, 56070 Koblenz, Germany.
J Agric Food Chem. 2010 Jun 9;58(11):6570-7. doi: 10.1021/jf100416w.
This paper describes for the first time a micromethod for the simultaneous determination of 3-monochloropropane-1,2-diol (3-MCPD) and fatty acid esters of 3-MCPD (3-MCPD esters) in different foodstuffs. 3-MCPD and 3-MCPD esters were isolated from food products using a single extraction step separating hydrophilic and lipophilic compounds. An aliquot of the aqueous layer was analyzed for the content of 3-MCPD while a part of the organic layer was analyzed for 3-MCPD esters after cleavage with sodium methoxide. After a simple derivatization procedure with phenylboronic acid (PBA), the determination was achieved by isotope dilution GC-MS using isotope-labeled 3-MCPD and 3-MCPD ester as internal standards. The method was validated for various foodstuffs like bakery products, meat and fish products, and soups as well as seasonings with LOD of 1-2 microg/kg (3-MCPD) and 6 microg/kg (3-MCPD esters), respectively. Recoveries ranged within 95 +/- 9% and 96 +/- 10% at spiking levels of 15 and 25 microg/kg in all matrices for 3-MCPD and 84 +/- 9% and 85 +/- 7% at spiking levels of 0.05 mg/kg and 2 mg/kg for 3-MCPD esters. The method avoids tedious and laborious sample preparation and was successfully applied to the rapid screening of samples conforming to the EU performance criteria for methods of analysis for 3-MCPD.
本文首次描述了一种用于同时测定不同食品中 3-氯-1,2-丙二醇（3-MCPD）和 3-MCPD 脂肪酸酯（3-MCPD 酯）的微量方法。3-MCPD 和 3-MCPD 酯通过单步提取分离亲水性和疏水性化合物从食品中分离出来。将一部分水层用于分析 3-MCPD 的含量，而将一部分有机层在与甲醇钠裂解后用于分析 3-MCPD 酯。用苯硼酸（PBA）进行简单的衍生化后，使用同位素标记的 3-MCPD 和 3-MCPD 酯作为内标，通过同位素稀释 GC-MS 进行测定。该方法已针对各种食品进行了验证，如面包制品、肉类和鱼类制品以及汤料和调味料，LOD 分别为 1-2μg/kg（3-MCPD）和 6μg/kg（3-MCPD 酯）。在所有基质中，3-MCPD 的加标水平为 15 和 25μg/kg 时，回收率在 95%±9%和 96%±10%之间，3-MCPD 酯的加标水平为 0.05mg/kg 和 2mg/kg 时，回收率在 84%±9%和 85%±7%之间。该方法避免了繁琐的样品制备，成功应用于符合欧盟分析方法性能标准的 3-MCPD 快速筛选样品。
