首页> 中文期刊>色谱 >9,10-蒽醌-2-磺酰氯用于液相色谱柱前相转移衍生测定水中酚的评价

9,10-蒽醌-2-磺酰氯用于液相色谱柱前相转移衍生测定水中酚的评价

     

摘要

A new reagent, anthraquinone-2-sulfonyl chloride (ASC), has been used for the derivatization of phenols. Several compounds with different polarity were selected to evaluate the new reagent and derivatives of these phenols prepared via a facile pathway. The optimal conditions for analytical derivatization and mechanism of the derivatization reaction are discussed. The derivatization procedure involves an ion-pair extraction of the deprotonated phenols with a tetrabutylammonium counter ion to an organic phase. At the interface of two phases, the derivatization reaction occurs quantitatively at room temperature within 3 min. The derivatives are stable and readily amenable to analysis by normal-phase and reversed-phase high performance liquid chromatography (HPLC). Excellent linearity response was demonstrated over the concentration range of 0.2 μmol/L to 200 μmol/L at 320 nm for normal-phase HPLC, at 256 nm for reversed-phase HPLC. Combined with preconcentration using a Waters Sep-Pak Plus C18 cartridge, detection limits of phenols for water sample analysis were as low as 1×10-9 mol/L (ca. 0.1 μg/L).%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3 min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320 nm或256 nm波长处检测),其浓度和响应在0.2 μmol/L~200 μmol/L内存在很好的线性关系.结合采用Waters Sep-Pak Plus C18 Cartridge 预浓缩,可以检测水中浓度低至10-9 mol/L(约0.1μg/L)的酚.上述4种酚在10-9 mol/L、10-7 mol/L及10-5 mol/L等3种浓度水平的加样回收率均大于87.1%.

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