Jensen Sören, Lindqvist Dennis, Asplund Lillemor
Department of Applied Environmental Science (ITM), Stockholm University, SE-106 91 Stockholm, Sweden.
J Agric Food Chem. 2009 Jul 8;57(13):5872-7. doi: 10.1021/jf803971d.
A method was developed for the extraction of lipids and analysis of halogenated phenols and alkylphenols in marine organisms. The extraction efficiency was evaluated by comparing the extractable lipid content and the recovery of 13 added phenols from three different marine species (herring, cod, and blue mussel), with the corresponding results from three well-established extraction procedures, the Bligh and Dyer (B&D), the Smedes (S), and the Jensen (J) methods. The J method and the new method, Jensen centrifugation (Jc), gave phenol recoveries of 80-100% for all species, whereas the B&D and S methods gave relatively low recoveries for the most acidic phenols, with recoveries of only 20-50% for pentachlorophenol (PCP) depending on the species. It was concluded that this effect was governed by the dissociation of the phenols and adsorption to the protein tissue during the extraction (due to ionic interactions). To increase the sensitivity of the analysis, the phenols were converted to their pentafluorobenzoyl esters, by using a tetrabutylammonium-catalyzed extractive acylation. The reaction was quantitative within 2 min at room temperature, and the formed derivatives were persistent enough to withstand treatment with concentrated sulfuric acid.
开发了一种用于提取海洋生物中脂质以及分析卤代酚和烷基酚的方法。通过比较三种不同海洋物种（鲱鱼、鳕鱼和蓝贻贝）中可提取脂质含量以及13种添加酚的回收率，与三种成熟提取方法（布莱和戴尔法（B&D）、斯梅德斯法（S）和詹森法（J））的相应结果，来评估提取效率。詹森法和新方法詹森离心法（Jc）对所有物种的酚回收率为80 - 100%，而B&D法和S法对大多数酸性酚的回收率相对较低，五氯苯酚（PCP）的回收率仅为20 - 50%，具体取决于物种。得出的结论是，这种效应是由酚的解离以及提取过程中对蛋白质组织的吸附（由于离子相互作用）所控制的。为了提高分析的灵敏度，通过使用四丁基铵催化的萃取酰化反应，将酚转化为其五氟苯甲酰酯。该反应在室温下2分钟内定量完成，形成的衍生物足够稳定，能够承受浓硫酸处理。
