【作者】 赵琴； 魏芳； 肖能； 余琼卫； 袁必锋； 冯钰锜；

【Author】 Qin Zhao 1,Fang Wei 2,Neng Xiao 1,Qiong-Wei Yu 1,Bi-Feng Yuan 1,Yu-Qi Feng,1 1(Key Laboratory of Analytical Chemistry for Biology and Medicine,Department of Chemistry,Wuhan University,Wuhan 430072,China) 2(Oil Crops Research Institute,Chinese Academy of Agricultural Sciences,Ministry of Agriculture Key Laboratory of Oil Crops Biology,Wuhan,Hubei,430062,China)

【机构】 生物医学分析化学教育部重点实验室,武汉大学化学与分子科学学院；

【摘要】 3-氯-1,2-丙二醇(3-MCPD)是一种国际公认的的食品污染物,它不仅具有致癌作用,而且可以降低精子活性,造成肾小管增生及肝功能损伤[1,2]。液相微萃取(LPME)技术是1996年Jeannot等人提出的一种利用悬挂于微量进样器针端的有机溶剂微滴进行萃取的样品预处理技术,是微型化的液液萃取(LLE)[3,4]。最近,磁性固相萃取(MSPE)技术由于其传质快、高效、快速分离等优点在样品预处理中得到广泛应用。[5,6,7]本文发展了一种新型的分散微萃取方法,并应用该方法对食用油中的3-MCPD进行纯化和富集。这种方法结合了LPME和MSPE的优点,操作简单,快捷。在该方法中,痕量的水通过移液枪直接加到裸露的,未经任何修饰的Fe3O4上。加入疏水的油性样品溶液后,在剧烈的涡旋搅拌作用下,加入的水破裂成无数以Fe3O4为核的细小液滴,形成水涂层的四氧化三铁(water-coatedFe3O4,W-Fe3O4),并分散在样品溶液中完成快速的萃取。萃取完成后,吸附了分析物的W-Fe3O4在外加磁场的作用下快速从样品溶液中分离。值得注意的是在该方法中,水作为萃取剂,Fe3O4作为水的载体,并且在萃取完成后起到回收水珠的重要作用。萃取的3-MCPD在经硅烷化试剂(三甲基硅烷咪唑,TMSI)衍生后,进入气相色谱质谱联用仪(GC-MS)检测。该方法在2-10000ng/g范围内线性良好(r2=0.9998),检出限低至1.1ng/g,实际样品的加标回收率在70.0%到104.9%之间,相对标准偏差小于6.4%。结果表明,本文所建立的新型分散微萃取方法适用于复杂的油性样品溶液中极性有机小分子的分离富集。更多还原

【Abstract】 In the present work,we developed a novel dispersive microextraction technique by combining the advantages of liquid-phase microextraction(LPME) and magnetic solid-phase extraction(MSPE).In this method,trace amount of water was directly absorbed on bare Fe3O4 to form water-coated Fe3O4(W-Fe 3 O 4) and rapid extraction can be achieved while W-Fe3O4 dispersed in the sample solution.The analyte adsorbed W-Fe3O4 can be easily collected and isolated from sample solution by a magnet.It was worth noting that in the proposed method water was used as extractant and Fe3O4 was served as the supporter and retriever of water.The performance of this method was evaluated by extraction of 3-monochloropropane-1,2-diol(3-MCPD) from edible oils.The extracted 3-MCPD was derived by a silylanization reagent(1-trimethylsilylimidazole) before gas chromatography-mass spectometry(GC-MS) analysis.Several parameters that affect the extraction and derivatization efficiency were investigated.Our results showed that the limit of detection for 3-MCPD was 1.1 ng/g.The recoveries in spiked oil sample were in the range of 70.0-104.9% with the RSDs less than 5.6%(intra-day) and 6.4%(inter-day).Taken together,the simple,rapid and cost-effective method developed in current study,offers a potential application for the extraction and preconcentration of hydrophilic analytes from complex fatty samples.更多还原