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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Analysis of volatile aldehyde biomarkers in human blood by derivatization and dispersive liquid-liquid microextraction based on solidification of floating organic droplet method by high performance liquid chromatography
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Analysis of volatile aldehyde biomarkers in human blood by derivatization and dispersive liquid-liquid microextraction based on solidification of floating organic droplet method by high performance liquid chromatography

机译:浮游有机液滴固化高效液相色谱衍生化-分散液-液微萃取分析人血中的挥发性醛类生物标志物

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摘要

A new dispersive liquid-liquid microextraction based on solidification of floating organic droplet method (DLLME-SFO) was developed for the determination of volatile aldehyde biomarkers (hexanal and heptanal) in human blood samples. In the derivatization and extraction procedure, 2,4-dinitrophenylhydrazine (DNPH) as derivatization reagent and formic acid as catalyzer were injected into the sample solution for derivatization with aldehydes, then the formed hydrazones was rapidly extracted by dispersive liquid-liquid microextraction with 1-dodecanol as extraction solvent. After centrifugation, the floated droplet was solidified in an ice bath and was easily removed for analysis. The effects of various experimental parameters on derivatization and extraction conditions were studied, such as the kind and volume of extraction solvent and dispersive solvent, the amount of derivatization reagent, derivatization temperature and time, extraction time and salt effect. The limit of detections (LODs) for hexanal and heptanal were 7.90 and 2.34 nmol L-1, respectively. Good reproducibility and recovery of the method were also obtained. The proposed method is an alternative approach to the quantification of volatile aldehyde biomarkers in complex biological samples, being more rapid and simpler and providing higher sensitivity compared with the traditional dispersive liquid-liquid microextraction (DLLME) methods.
机译:建立了一种基于漂浮有机液滴凝固法的分散液-液微萃取新方法(DLLME-SFO),用于测定人血样品中的挥发性醛生物标志物(己醛和庚醛)。在衍生和提取过程中,将2,4-二硝基苯肼(DNPH)作为衍生试剂和甲酸作为催化剂注入样品溶液中,用醛进行衍生化,然后通过分散液-液微萃取(1-十二烷醇为萃取溶剂。离心后,将漂浮的液滴在冰浴中固化,可以轻松取出进行分析。研究了各种实验参数对衍生化和萃取条件的影响,例如萃取溶剂和分散溶剂的种类和体积,衍生化试剂的量,衍生化温度和时间,萃取时间和盐分效应。己醛和庚醛的检出限(LOD)分别为7.90和2.34 nmol L-1。还获得了该方法的良好重现性和回收率。与传统的分散液-液微萃取(DLLME)方法相比,该方法是定量分析复杂生物样品中挥发性醛类生物标志物的另一种方法,它更快速,更简单且灵敏度更高。

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