Japan Food Research Laboratories, 7-4-41, Saito-Asagi, Ibaraki-shi, Osaka 567-0085, Japan.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2013;30(1):52-68. doi: 10.1080/19440049.2012.713031. Epub 2012 Aug 21.
A new, direct analytical method for the determination of 3-chloro-1,2-propanediol fatty acid esters (3-MCPD esters) was developed. The targeted 3-MCPD esters included five types of monoester and 25 [corrected] types of diester. Samples (oils and fats) were dissolved in a mixture of tert-butyl methyl ether and ethyl acetate (4:1), purified using two solid-phase extraction (SPE) cartridges (C(18) and silica), then analysed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Five monoesters and five diesters with the same fatty acid group could be separated and quantified. Pairs of 3-MCPD diesters carrying the same two different fatty acid groups, but at reversed positions (sn-1 and sn-2), could not be separated and so were expressed as a sum of both compounds. The limits of quantification (LOQs) were estimated to be between 0.02 to 0.08 mg kg(-1), depending on the types of 3-MCPD ester. Repeatability expressed as relative standard deviation (RSD(r)%) varied from 5.5% to 25.5%. The new method was shown to be applicable to various commercial edible oils and showed levels of 3-MCPD esters varying from 0.58 to 25.35 mg kg(-1). The levels of mono- and diesters ranged from 0.10 to 0.69 mg kg(-1) and from 0.06 to 16 mg kg(-1), respectively.
开发了一种新的、直接的分析方法，用于测定 3-氯-1,2-丙二醇脂肪酸酯（3-MCPD 酯）。目标 3-MCPD 酯包括五种单酯和 25 种[更正]二酯。样品（油和脂肪）溶解在叔丁基甲基醚和乙酸乙酯（4:1）的混合物中，用两个固相萃取（SPE）小柱（C(18)和硅胶）纯化，然后用液相色谱-串联质谱（LC-MS/MS）分析。五种单酯和五种具有相同脂肪酸基团的二酯可以分离和定量。携带相同两个不同脂肪酸基团但位置相反（sn-1 和 sn-2）的 3-MCPD 二酯不能分离，因此表示为两种化合物的总和。定量限（LOQ）估计在 0.02 至 0.08mg/kg 之间，具体取决于 3-MCPD 酯的类型。重复性表示为相对标准偏差（RSD(r)％），变化范围为 5.5%至 25.5%。新方法适用于各种商业食用油，显示 3-MCPD 酯的水平在 0.58 至 25.35mg/kg 之间。单酯和二酯的水平分别在 0.10 至 0.69mg/kg 和 0.06 至 16mg/kg 之间。
