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改进的中空纤维液相微萃取结合色谱-电子捕获检测在超痕量水平定量废水样品中丙烯酰胺的应用。

Application of modified hollow fiber liquid phase microextraction in conjunction with chromatography-electron capture detection for quantification of acrylamide in waste water samples at ultra-trace levels.

作者信息

Sobhi Hamid Reza, Ghambarian Mahnaz, Behbahani Mohammad, Esrafili Ali

机构信息

Department of Chemistry, Payame Noor University, Tehran, Iran.

Iranian Research and Development Center for Chemical Industries, ACECR, Tehran, Iran.

出版信息

J Chromatogr A. 2017 Mar 3;1487:30-35. doi: 10.1016/j.chroma.2017.01.051. Epub 2017 Jan 23.

Abstract

Herein, a simple and sensitive method was successfully developed for the extraction and quantification of acrylamide in water samples. Initially, acrylamide was derivatized through a bromination process. Subsequently, a modified hollow-fiber liquid-phase microextraction was applied for the extraction of the brominated acrylamide from a 10-ml portion of an aqueous sample. Briefly, in this method, the derivatized acrylamide (2,3-dibromopropionamide) was extracted from the aqueous sample into a thin layer of an organic solvent sustained in pores of a porous hollow fiber. Then, it was back-extracted using a small volume of organic acceptor solution (acetonitril, 25μl) located inside the lumen of the hollow fiber followed by gas chromatography-electron capture detection (GC-ECD). The optimal conditions were examined for the extraction of the analyte such as: the organic solvent: dihexyl ether+10% tri-n-octyl phosphine oxide; stirring rate: 750rpm; no salt addition and 30min extraction time. These optimal extraction conditions allowed excellent enrichment factor values for the method. Enrichment factor, detection limit (S/N=3) and dynamic linear range of 60, 2ngL and 50-1000ngL to be determined for the analyte. The relative standard deviations (RSD%) representing precision of the method were in the range of 2.2-5.8 based on the average of three measurements. Accuracy of the method was tested by the relative recovery experiments on spiked samples, with results ranging from 93 to 108%. Finally, the method proved to be simple, rapid, and cost-effective for routine screen of acrylamide-contaminated highly-complicated untreated waste water samples.

摘要

在此,成功开发了一种简单且灵敏的方法用于水样中丙烯酰胺的萃取和定量分析。首先,通过溴化过程使丙烯酰胺衍生化。随后,采用改进的中空纤维液相微萃取法从10毫升水样中萃取溴化丙烯酰胺。简要来说,在该方法中,将衍生化的丙烯酰胺(2,3 - 二溴丙酰胺)从水样中萃取到多孔中空纤维孔道内维持的一薄层有机溶剂中。然后,使用位于中空纤维内腔的少量有机接受液(乙腈,25微升)进行反萃取,接着进行气相色谱 - 电子捕获检测(GC - ECD)。考察了分析物萃取的最佳条件,如:有机溶剂:二己醚 + 10% 三正辛基氧化膦;搅拌速率:750转/分钟;不添加盐且萃取时间为30分钟。这些最佳萃取条件使该方法具有出色的富集因子值。分析物的富集因子、检测限(S/N = 3)和动态线性范围分别为60、2纳克/升和50 - 1000纳克/升。基于三次测量的平均值,代表该方法精密度的相对标准偏差(RSD%)在2.2 - 5.8范围内。通过对加标样品的相对回收率实验测试了该方法的准确度,结果在93%至108%之间。最后,该方法被证明对于丙烯酰胺污染的高度复杂未处理废水样品的常规筛查而言简单、快速且具有成本效益。

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