Improved method for the extraction and determination of bromophenols in seafoods by high-performance liquid chromatography with fluorescence detection.
Improved method for the extraction and determination of bromophenols in seafoods by high-performance liquid chromatography with fluorescence detection.
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DOI：
10.1021/jf302882f
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发表时间：
2012-10
影响因子：
6.1
通讯作者：
Shijuan Zhang;Yanxin Li;J. You;Hua Wang;Yan E. Zheng;Y. Suo
中科院分区：
文献类型：
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作者：
Shijuan Zhang;Yanxin Li;J. You;Hua Wang;Yan E. Zheng;Y. Suo
建立了一种以10-甲基吖啶酮-2-磺酰氯（MASC）为衍生试剂的柱前衍生-高效液相色谱（HPLC）荧光检测法测定海产品中天然溴代酚的方法。采用硫酸水解-正己烷萃取-碱反萃取的方法代替传统的复杂的水蒸气蒸馏溶剂萃取方法，获得了较好的回收率和较少的干扰。由于样品量和分析时间大大减少，因此溴酚的批量分析变得更加可行。5种溴代酚的回收率均在80%以上，4-BP的回收率明显提高，而传统方法的回收率一般在40%以下。通过衍生化，大大提高了高效液相色谱法测定溴苯酚的灵敏度。在最佳条件下，对4.0g样品的定量限为0.60- 1.0ng/g。这是首次将衍生化应用于提高溴代酚类化合物的HPLC灵敏度。该方法成功地应用于海产品中目标化合物的测定，其灵敏度远高于传统的高效液相色谱法。
A sensitive precolumn derivatization method using 10-methylacridone-2-sulfonyl chloride (MASC) as derivatizing reagent followed by high-performance liquid chromatography (HPLC) with fluorescence detection has been developed for the determination of naturally occurring bromophenols in seafoods. Instead of using a traditional complex steam distillation solvent extraction method, the extraction method was modified by using sulfuric acid hydrolysis followed by hexane extraction and subsequent alkaline back extraction to obtain good recoveries and fewer interferences. Batch analysis of bromophenols thus became more performable because the sample amount and analysis time were greatly reduced. The recoveries of the five bromophenols were >80% with a noticeable improvement for 4-BP, the recoveries of which were usually <40% when analyzed by traditional methods. The HPLC sensitivity for the determination of bromophenols was greatly enhanced through derivatization. Under optimal conditions, the quantification limits obtained by using 4.0 g of sample were in the range of 0.60-1.0 ng/g. This is the first time that derivatization was applied to enhance the HPLC sensitivity of bromophenols. The proposed method was successfully applied to the determination of the target compounds in seafoods with a much higher sensitivity than traditional HPLC method.