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使用毛细管管收集分散液液微萃取后比水轻的萃取溶剂及其在气相色谱-火焰离子化检测法中不同样品中对羟基苯甲酸酯的测定中的应用。

Use of a capillary tube for collecting an extraction solvent lighter than water after dispersive liquid-liquid microextraction and its application in the determination of parabens in different samples by gas chromatography--flame ionization detection.

机构信息

Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, 29 Bahman Bolvar, Tabriz, Iran.

出版信息

Talanta. 2010 Jun 15;81(4-5):1360-7. doi: 10.1016/j.talanta.2010.02.035. Epub 2010 Feb 13.

Abstract

In this study a new dispersive liquid-liquid microextraction (DLLME) method is presented on the basis of a safe organic solvent, octanol, which is lighter than water. The proposed method is used for the extraction and pre-concentration of some preservatives including methyl paraben (Mep), ethyl paraben (Etp) and propyl paraben (Prp) from different matrices. The extracted compounds are monitored by gas chromatography-flame ionization detector (GC-FID). A mixture of suitable extraction and dispersive solvents including 20microL octanol and 0.5mL acetone is quickly injected into the aqueous sample. The mixture is centrifuged for 10min at 6000rpm, so a small drop of extraction solvent collects on the water surface. A portion of the collected solvent is removed by a capillary tube through simple dipping the tube into organic solvent drop. 0.4microL of extract into the tube is removed by a microsyringe and injected into GC. Some effective parameters such as kinds and volumes of extraction and dispersive solvents as well as extraction time have to be investigated. Under optimum conditions, enrichment factors and recoveries of the studied compounds were obtained in the range of 100-276 and 25-72%, respectively. Linear ranges of the calibration curves were between 0.05 and 30 for methyl- and 0.02 and 30microgmL(-1) for ethyl- and propyl parabens, respectively. Limit of detection for methyl paraben was 0.015microgmL(-1) and those of ethyl- and propyl parabens were 0.005microgmL(-1). Relative standard deviations (RSDs %) for six repeated measurements (C=2microgmL(-1)) were 2% for methyl-, and ethyl parabens and 3% for propyl parabens, respectively.

摘要

在这项研究中,提出了一种基于安全有机溶剂辛醇的新的分散液 - 液微萃取(DLLME)方法,辛醇比水轻。该方法用于从不同基质中提取和预浓缩一些防腐剂,包括对羟基苯甲酸甲酯(Mep),对羟基苯甲酸乙酯(Etp)和对羟基苯甲酸丙酯(Prp)。提取的化合物通过气相色谱 - 火焰离子化检测器(GC-FID)监测。包括 20μL 辛醇和 0.5mL 丙酮在内的合适萃取和分散溶剂的混合物被快速注入水样品中。混合物在 6000rpm 下离心 10min,因此一小滴萃取溶剂在水面上收集。通过简单地将管浸入有机溶剂滴中,用毛细管管去除收集的溶剂的一部分。通过微量进样器将 0.4μL 萃取物吸入管中并注入 GC。必须研究一些有效参数,例如萃取和分散溶剂的种类和体积以及萃取时间。在最佳条件下,研究化合物的富集因子和回收率分别在 100-276 和 25-72%的范围内。甲基和乙基对羟基苯甲酸酯的校准曲线的线性范围分别为 0.05-30 和 0.02-30μgmL(-1),丙基对羟基苯甲酸酯的线性范围为 0.02-30μgmL(-1)。甲基对羟基苯甲酸的检测限为 0.015μgmL(-1),乙基和丙基对羟基苯甲酸的检测限为 0.005μgmL(-1)。对于六个重复测量(C=2μgmL(-1)),甲基和乙基对羟基苯甲酸的相对标准偏差(RSD)为 2%,丙基对羟基苯甲酸的相对标准偏差为 3%。

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