In situ continuous derivatization/pre-concentration of carbonyl compounds with 2,4-dinitrophenylhydrazine in aqueous samples by solid-phase extraction Application to liquid chromatography determination of aldehydes
In situ continuous derivatization/pre-concentration of carbonyl compounds with 2,4-dinitrophenylhydrazine in aqueous samples by solid-phase extraction Application to liquid chromatography determination of aldehydes
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DOI：
10.1016/j.talanta.2008.09.053
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发表时间：
2009-03-15
期刊：
影响因子：
6.1
通讯作者：
Silva, Manuel
中科院分区：
文献类型：
--
作者：
Banos, Clara-Eugenia;Silva, Manuel
建立了一种快速、简便的连续固相萃取系统，用于水中羰基化合物的现场衍生和预富集。首先将衍生剂2，4-二硝基苯肼吸附在C-18微型柱上，然后将15 ml样品连续吸入流动系统，其中同时进行分析物（低分子量醛）的衍生化和预浓缩。洗脱后，将20 μ l提取物注入LC-DAD系统。在RP-C-18柱上，以乙腈-水（60-100%乙腈）为流动相，线性梯度移动的，流速0.5 ml/min，流动相为乙腈-水，流动相为乙腈，流动相为水，流动相为乙腈，流动相为乙腈，流动相为水，流动相为乙腈，流动相为乙腈，流动相为水，流动相为乙腈，流动相为乙腈在最佳条件下，检测限为0.3和1.0 μ g/L之间，RSD（粘土间精密度）为1.2%至4.6%。最后介绍了该方法在实际水样中的应用，回收率为95.8 ~ 99.4%。(C)2008 Elsevier B. V.保留所有权利。
A rapid and straightforward continuous solid-phase extraction system has been developed for in situ derivatization and pre-concentration of carbonyl compounds in aqueous samples Initially 2,4-dinitrophenylhydrazine, the derivatizing agent, was adsorbed on a C-18 mini-column and then 15-ml of sample were continuously aspirated into the flow system, where the derivatization and pre-concentration of the analytes (low-molecular mass aldehydes) were performed simultaneously. Following elution, 20 mu l of the extract were injected into a LC-DAD system. in which hydrazones were successfully separated in 12 min on a RP-C-18 column using a linear gradient mobile phase of acetonitrile-water of 60-100% acetonitrile for 8 min. flowing at 0.5 ml/min. The whole analytical process can be accomplished within ca. 35 min. Under optimum conditions, limits of detection were obtained between 0.3 and 1.0 mu g/l and RSDs (inter-clay precision) from 1.2 to 4.6%. Finally, some applications on water samples are presented with recoveries ranged from 95.8 to 99.4%. (C) 2008 Elsevier B.V. All rights reserved.