Unilever Research and Development Vlaardingen, P.O. Box 114, 3130 AC Vlaardingen, The Netherlands.
J Chromatogr A. 2013 Oct 25;1313:202-11. doi: 10.1016/j.chroma.2013.06.056. Epub 2013 Jun 28.
Glycidyl esters (GE), fatty acid esters of glycidol, are process contaminants formed during edible oil processing. A novel direct method for the determination of intact GE in oils and fats based on gas chromatography-mass spectrometry (GC-MS) is presented. The method consists of a simple extraction step of GE from the lipid matrix, purification of the extract and isolation of GE by normal phase liquid chromatography (NPLC). Individual GE in the final fraction are separated and quantified by standard GC-MS operated in selected ion monitoring (SIM) mode. The setup and conditions of the GC-MS were optimized in such a way that thermal degradation of GE and artifact formation were prevented. The method exhibits very good performance parameters: the limit of detection was approximately 0.01 mg/kg for the individual GE (corresponding to 0.002-0.003 mg/kg of free glycidol), the repeatability was in the range of 5-12% for individual GE at levels above 0.1mg/kg, and recovery values ranged from 85 to 115% depending on the level and the chain identity of the GE. The comparison of experimental values with spiked levels and with the results obtained by other methods confirmed a good trueness. Over a period of several months of extensive use the method was found to be very reliable and rugged.
缩水甘油酯（GE）是缩水甘油的脂肪酸酯，是食用油加工过程中形成的加工污染物。本文提出了一种基于气相色谱-质谱联用（GC-MS）测定油脂中完整 GE 的新的直接方法。该方法包括从脂质基质中提取 GE 的简单步骤、提取物的纯化以及通过正相液相色谱（NPLC）分离和分离 GE。通过标准 GC-MS 在选择离子监测（SIM）模式下分离和定量最终馏分中的各个 GE。GC-MS 的设置和条件进行了优化，以防止 GE 的热降解和形成假象。该方法表现出非常好的性能参数：对于单个 GE，检测限约为 0.01mg/kg（相当于游离缩水甘油的 0.002-0.003mg/kg），对于 0.1mg/kg 以上水平的单个 GE，重复性在 5-12%范围内，回收率值根据 GE 的水平和链身份在 85-115%之间变化。实验值与添加水平和其他方法的结果进行比较证实了良好的准确性。在广泛使用的几个月中，该方法被发现非常可靠和坚固。
