Li Heli, Chen Dawei, Miao Hong, Zhao Yunfeng, Shen Jianzhong, Wu Yongning
College of Veterinary Medicine, China Agricultural University, Beijing 100193, China; Key Laboratory of Food Safety Risk Assessment, Ministry of Health; China National Center for Food Safety Risk Assessment, Beijing 100021, China.
Key Laboratory of Food Safety Risk Assessment, Ministry of Health; China National Center for Food Safety Risk Assessment, Beijing 100021, China.
J Chromatogr A. 2015 Sep 4;1410:99-109. doi: 10.1016/j.chroma.2015.07.080. Epub 2015 Jul 26.
A selective and sensitive ultra-high performance liquid chromatography - triple quadrupole mass spectrometry (UHPLC-MS/MS) method coupled with matrix solid phase dispersion (MSPD) extraction was developed for the direct determination of fatty acid esters of 3-chloro-1,2-propanediol (3-MCPD esters) in edible vegetable oils. The method integrated the isotope dilution technique, MSPD extraction and UHPLC - MS/MS analysis with multi-reaction monitoring mode (MRM). Matrix-matched calibration curves showed good linearity within the range of 0.01-10mgL(-1) with the correlation coefficient not less than 0.999. Limits of detection (LODs) and limit of quantification (LOQs) of the 3-MCPD esters fell into the range of 0.0001-0.02mgkg(-1) and 0.0004-0.05mgkg(-1), respectively. The recoveries for the spiked extra virgin olive oils ranged from 94.4% to 108.3%, with the relative standard deviations (RSD) ranging from 0.6% to 10.5%. The method was applied for the oil sample (T2642) of the official Food Analysis Performance Assessment Scheme (FAPAS) in 2014 and other real samples from supermarket, and the results showed that the present method was comparative to the gas chromatography-mass spectrometry (GC-MS) method based on the improved German Society for Fat Science (DGF) standard method C-III 18 (09) except for palm oil.
建立了一种选择性和灵敏的超高效液相色谱-三重四极杆质谱联用（UHPLC-MS/MS）方法，并结合基质固相分散（MSPD）萃取，用于直接测定食用植物油中3-氯-1,2-丙二醇脂肪酸酯（3-MCPD酯）。该方法将同位素稀释技术、MSPD萃取和UHPLC-MS/MS分析与多反应监测模式（MRM）相结合。基质匹配校准曲线在0.01-10mgL(-1)范围内显示出良好的线性，相关系数不低于0.999。3-MCPD酯的检测限（LOD）和定量限（LOQ）分别在0.0001-0.02mgkg(-1)和0.0004-0.05mgkg(-1)范围内。添加了特级初榨橄榄油的样品回收率在94.4%至108.3%之间，相对标准偏差（RSD）在0.6%至10.5%之间。该方法应用于2014年官方食品分析性能评估计划（FAPAS）的油样（T2642）和来自超市的其他实际样品，结果表明，除棕榈油外，本方法与基于改进的德国油脂科学协会（DGF）标准方法C-III 18（09）的气相色谱-质谱联用（GC-MS）方法相当。
