Center for Food Safety and Applied Nutrition, United States Food and Drug Administration, 5100 Paint Branch Parkway, College Park, MD 20740, USA.
J Agric Food Chem. 2013 May 22;61(20):4737-47. doi: 10.1021/jf4005803. Epub 2013 May 9.
A new analytical method has been developed and validated for the detection of glycidyl esters (GEs) and 3-monochloropropanediol (3-MCPD) monoesters in edible oils. The target compounds represent two classes of potentially carcinogenic chemical contaminants formed during the processing of edible oils. Target analytes are separated from edible oil matrices using a two-step solid-phase extraction (SPE) procedure. The extracts are then analyzed using liquid chromatography-tandem mass spectrometry (LC-MS/MS) with electrospray ionization (ESI). Chromatographic conditions that separate sn-1 and sn-2 monoesters of 3-MCPD have been developed for the first time. The method has been validated for GEs, sn-1 3-MCPD monoesters of lauric, myristic, linolenic, linoleic, oleic, and stearic acids, and sn-2 3-MCPD monoesters of oleic and palmitic acids in coconut, olive, and palm oils using an external calibration curve. The range of average recoveries and relative standard deviations (RSDs) across the three oil matrices at three spiking concentrations are 84-115% (3-16% RSD) for the GEs, 95-113% (1-10% RSD) for the sn-1 3-MCPD monoesters, and 76.8-103% (5.1-11.2% RSD) for the sn-2 3-MCPD monoesters, with limits of quantitation at or below 30 ng/g for the GEs, 60 ng/g for sn-1 3-MCPD monoesters, and 180 ng/g for sn-2 3-MCPD monoesters.
已开发并验证了一种用于检测食用油中缩水甘油酯 (GEs) 和 3-单氯丙二醇 (3-MCPD) 单酯的新分析方法。目标化合物代表在食用油加工过程中形成的两类潜在致癌化学污染物。使用两步固相萃取 (SPE) 程序将目标化合物与食用油基质分离。然后使用液相色谱-串联质谱 (LC-MS/MS) 联用电喷雾电离 (ESI) 对提取物进行分析。首次开发了可分离 3-MCPD sn-1 和 sn-2 单酯的色谱条件。该方法已通过外部校准曲线验证,可用于椰子油、橄榄油和棕榈油中的 GEs、月桂酸、肉豆蔻酸、亚油酸、亚麻酸、油酸和硬脂酸的 sn-1 3-MCPD 单酯,以及油酸和棕榈酸的 sn-2 3-MCPD 单酯。在三个油基质中,三个加标浓度的平均回收率和相对标准偏差 (RSD) 的范围为 GEs 为 84-115%(3-16% RSD),sn-1 3-MCPD 单酯为 95-113%(1-10% RSD),sn-2 3-MCPD 单酯为 76.8-103%(5.1-11.2% RSD),GEs 的定量限为 30 ng/g 或以下,sn-1 3-MCPD 单酯为 60 ng/g,sn-2 3-MCPD 单酯为 180 ng/g。