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A new configuration for bar adsorptive microextraction (BAμE) for the quantification of biomarkers (hexanal and heptanal) in human urine by HPLC providing an alternative for early lung cancer diagnosis
Analytica Chimica Acta ( IF 5.7 ) Pub Date : 2017-03-31 09:39:06
Anderson Luiz Oenning, Lucas Morés, Adriana Neves Dias, Eduardo Carasek

In this paper, a remodeling of the bar adsorptive microextraction (BAμE) technique is proposed with impregnation of the derivatization reagent on the surface of the adsorptive bar containing a biosorbent material. The derivatization reagent was 2,4-dinitrophenylhydrazine (DNPH), which was adsorbed on the surface of the bar containing cork powder as the extractor phase for the determination of two aldehydes (hexanal and heptanal) which are known as lung cancer biomarkers in human urine samples. The derivatization reaction and the extraction occurred simultaneously on the surface of the bar (length 7.5 mm) under acidic conditions. The method optimization was carried out by univariate and multivariate analysis. The optimal conditions for the method were a DNPH to aldehydes ratio of 40:1, buffer solution of pH 4.0, extraction time of 60 min and liquid desorption of 10 min in 100 μL of acetonitrile. The aldehydes were analyzed by HPLC-DAD with a simple and fast (6 min) chromatographic run. The limits of detection (LODs) for hexanal and heptanal were 1.00 and 0.73 μmol L−1, respectively. The relative recoveries in urine samples ranged from 88 to 111% with relative standard deviations (RSDs) being less than 7%. The method developed is of low cost and can be successfully used for the quantification of these two lung cancer biomarkers in human urine samples, potentially providing an early diagnosis of lung cancer.

中文翻译:

条形吸附微萃取(BAμE)的新配置,用于通过HPLC定量人尿中的生物标志物(己醛和庚醛),为早期肺癌诊断提供了一种替代方法

在本文中,提出了一种对棒吸附微萃取(BAμE)技术的改造,其中将衍生化试剂浸渍在含有生物吸附材料的吸附棒表面上。衍生试剂为2,4-二硝基苯肼(DNPH),其吸附在含有软木粉的皂条表面作为萃取相,用于测定两种醛(己醛和庚醛),这两种醛被称为人尿中的肺癌生物标记物样品。在酸性条件下,棒的表面(长7.5 mm)同时发生衍生化反应和萃取。通过单变量和多变量分析进行方法优化。该方法的最佳条件是DNPH与醛的比例为40:1,缓冲溶液的pH为4.0,在100μL乙腈中的提取时间为60分钟,液体解吸时间为10分钟。通过HPLC-DAD以简单,快速(6分钟)的色谱运行对醛进行分析。己醛和庚醛的检出限(LOD)为1.00和0.73μmolL-1。尿液样品的相对回收率介于88%至111%之间,相对标准偏差(RSD)小于7%。所开发的方法成本低廉,可成功用于人类尿液样本中这两种肺癌生物标记物的定量分析,有可能为肺癌的早期诊断提供依据。
更新日期:2017-04-01
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