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一种新的衍生试剂9,10 蒽醌 2 磺酰氯(ASC)首次用于酚类衍生。几种不同极性的酚被用于评价该试剂。为便于考察ASC对酚衍生的机理及优化衍生条件,制备了不同酚的标准衍生物并对它们进行了结构确证。衍生过程涉及去质子酚与特丁基铵阴离子形成离子对后被有机溶剂提取。衍生反应可以在室温下3min内在两相界面上定量完成。衍生产物很稳定,可以分别被正相色谱和反相色谱分离(相应地在320nm或256nm波长处检测),其浓度和响应在0 2μmol/L～200μmol/L内存在很好的线性关系。结合采用WatersSep PakPlusC18Cartridge预浓缩,可以检测水中浓度低至10-9mol/L(约0 1μg/L)的酚。上述4种酚在10-9mol/L、10-7mol/L及10-5mol/L等3种浓度水平的加样回收率均大于87 1%。
A new derivatization reagent 9,10 anthraquinone 2 sulfonyl chloride (ASC) was first used for phenolic derivatization. Several different polar phenols were used to evaluate the reagent. To facilitate the investigation of the mechanism of ASC derivatization of phenol and to optimize the derivatization conditions, standard derivatives of different phenols were prepared and their structures confirmed. The derivatization process involves the deprotonation of protonated phenols with t-butylammonium anion to form an ion pair and then extracted with an organic solvent. The derivatization can be done quantitatively at the two-phase interface within 3 min at room temperature. Derivatives are very stable and can be separated by normal phase and reverse phase chromatography (respectively at 320 nm or 256 nm) with good linearity in the concentration range of 0 2 μmol / L to 200 μmol / L. Combined with WatersSep PakPlusC18Cartridge Preconcentration, phenol concentrations in water as low as 10-9 mol / L (about 0 1 μg / L) can be detected. The recoveries of the above four kinds of phenols were higher than 87 1% at the concentrations of 10-9mol / L, 10-7mol / L and 10-5mol / L.