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涡流溶剂搅拌棒微萃取法用于从水基质中提取邻苯二甲酸酯。

Vortex solvent bar microextraction for phthalate esters from aqueous matrices.

机构信息

Beijing Key Laboratory of Microanalytical Methods and Instrumentation, Department of Chemistry, Tsinghua University, Beijing 100084, China.

出版信息

Talanta. 2012 Oct 15;100:64-70. doi: 10.1016/j.talanta.2012.08.009. Epub 2012 Aug 16.

Abstract

An improved hollow fiber solvent bar microextraction method termed as vortex solvent bar microextraction (VSBME) was developed. A short hollow fiber immobilized with organic extraction solvent was served as the solvent bar for microextraction of phthalate esters from aqueous matrices. The hydrophobic analytes were pre-focused at the bottom of the vortex under the vigorous magnetic stirring before extraction, which facilitated the mass transfer of analytes from aqueous matrix to organic extraction phase in the subsequent solvent bar microextraction. With the extraction solvent lost gradually from the hollow fiber under the stirring, the efficient extraction was maintained by the absorption of analytes in the porous membrane. After extraction, the analytes were desorbed from the hollow fiber membrane using 50 μL organic solvent. The phthalate esters with 1-octanol/water partition coefficients ranging from 1.69 to 8.83 were used as model compounds to investigate the extraction performance. Extraction conditions such as type and volume of extraction solvents, stirring intensity, extraction time, sample concentration and volume were investigated and optimized. Analysis was carried out with gas chromatography-mass spectrometry (GC-MS). Under the optimum conditions, this new method gave super high enrichment factors (over 1500), good reproducibility (<7.1%, n=6) in a rapid extraction within 5 min. It allowed the determination of phthalate esters at ng L(-1) level. Compared with the other microextraction methods, the proposed VSBME was simpler, more robust and had higher enrichment efficiency. The matrix effects on the extraction performance were also investigated with bottled ice red tea, red wine and human urine.

摘要

一种改进的中空纤维溶剂棒微萃取方法,称为涡旋溶剂棒微萃取(VSBME),已被开发出来。一根短的中空纤维被固定在有机溶剂中,作为溶剂棒,用于从水基质中萃取邻苯二甲酸酯。在萃取之前,在剧烈的磁力搅拌下,疏水性分析物在涡旋的底部被预浓缩,这促进了分析物从水基质向后续溶剂棒微萃取中的有机萃取相的传质。随着搅拌过程中中空纤维中萃取溶剂的逐渐损失,通过多孔膜吸收分析物来保持高效的萃取。萃取后,用 50μL 有机溶剂从中空纤维膜中解吸分析物。邻苯二甲酸酯的辛醇/水分配系数在 1.69 到 8.83 之间,用作模型化合物来研究萃取性能。考察并优化了萃取条件,如萃取溶剂的类型和体积、搅拌强度、萃取时间、样品浓度和体积。采用气相色谱-质谱(GC-MS)进行分析。在最佳条件下,这种新方法在 5 分钟内快速萃取,可获得超高的富集因子(超过 1500)和良好的重现性(<7.1%,n=6)。它可以在 ng L(-1)水平下测定邻苯二甲酸酯。与其他微萃取方法相比,所提出的 VSBME 更简单、更稳健,且具有更高的富集效率。还研究了瓶装冰红茶、红酒和人尿对萃取性能的基质效应。

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