Department of Chemistry and Physics, Analytical Chemistry Area, University of Almería, Research Centre for Mediterranean Intensive Agrosystems and Agri-Food Biotechnology (CIAIMBITAL), Agrifood Campus of International Excellence ceiA3, Carretera de Sacramento s/n, E-04120 Almería, Spain.
Department of Chemistry and Physics, Analytical Chemistry Area, University of Almería, Research Centre for Mediterranean Intensive Agrosystems and Agri-Food Biotechnology (CIAIMBITAL), Agrifood Campus of International Excellence ceiA3, Carretera de Sacramento s/n, E-04120 Almería, Spain.
J Chromatogr A. 2021 Feb 22;1639:461940. doi: 10.1016/j.chroma.2021.461940. Epub 2021 Jan 24.
The development and validation of a method for the analysis of traces of 3-monochloropropanediol (3-MCPD) esters (19) and glycidyl esters (7) of fatty acids in vegetable oils, margarine, biscuits and croissants was performed. An extraction method based on the use of solvents (tert‑butyl methyl ether (20% ethyl acetate, v/v)) was carried out and cleaning of the extract with a mixture of sorbents (Si-SAX, PSA and Z-sep+) was optimized for the elimination of fatty interferents. The analysis of the targeted compounds was carried out by ultra-high-performance liquid chromatography coupled to tandem mass spectrometry, using a triple quadrupole analyzer (UHPLC-MS/MS-QqQ). The validation of the method provided trueness values between 72 and 118% and precision lower than 20%. The limits of quantification ranged from 0.01 to 0.1 mg kg, which were below the current legal limits. Twenty samples of vegetable oils as well of 4 samples of margarine, biscuits and croissants were analyzed. Six out of the 24 samples (25%) exceeded the limits set by European legislation, and a maximum contamination of 3-MCPD esters at 2.52 mg kg was obtained in a sample of corn oil (being 1-myristoyl-3-MCPD the compound detected at the highest concentration). A maximum concentration of glycidyl esters at 7.84 mg kg was determined in a soybean oil sample (glycidyl linoleate as the main compound). Only one sample of olive oil exceeded the maximum allowable limit for 3-MCPD esters with a value of 1.72 mg kg, expressed as 3-MCPD.
开发并验证了一种分析植物油、人造黄油、饼干和羊角面包中痕量 3-单氯丙二醇（3-MCPD）酯（19）和脂肪酸缩水甘油酯（7）的方法。该方法基于使用溶剂（叔丁基甲基醚（20%乙酸乙酯，v/v））进行提取，并优化了用混合吸附剂（Si-SAX、PSA 和 Z-sep+）对提取物进行净化，以去除脂肪酸干扰物。目标化合物的分析采用超高效液相色谱-串联质谱法（UHPLC-MS/MS-QqQ），使用三重四极杆分析器。方法验证提供了 72%至 118%的准确度值和低于 20%的精密度。定量限范围为 0.01 至 0.1mg/kg，低于现行法定限量。分析了 24 个植物油样品以及 4 个人造黄油、饼干和羊角面包样品。24 个样品中有 6 个（25%）超过了欧洲法规规定的限量，在玉米油样品中检测到的 3-MCPD 酯最高污染水平为 2.52mg/kg（检测到的化合物为 1-肉豆蔻酰基-3-MCPD）。在大豆油样品中测定到的缩水甘油酯最高浓度为 7.84mg/kg（主要化合物为亚油酸缩水甘油酯）。只有一个橄榄油样品的 3-MCPD 酯允许限量超标，值为 1.72mg/kg，以 3-MCPD 表示。
