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在微柱液相色谱中使用硼酸酯柱在线预柱富集双酚A。

On-line precolumn enrichment of bisphenol A using boronate column in microcolumn liquid chromatography.

作者信息

Lim Lee Wah, Takeuchi Toyohide

机构信息

Department of Chemistry, Faculty of Engineering, Gifu University, 1-1 Yanagido, Gifu 501-1193, Japan.

出版信息

J Chromatogr A. 2006 Feb 17;1106(1-2):139-45. doi: 10.1016/j.chroma.2005.09.003. Epub 2005 Oct 5.

Abstract

The application of a boronate precolumn in the trace determination of 4,4'-isopropylidenediphenol (bisphenol A or BPA) in aqueous solution was investigated by microcolumn liquid chromatography (LC). BPA was enriched by a precolumn packed with TSK(gel) boronate and it was then injected (back-flushed) into an ODS separation column. Comparing to a conventional syringe injection, a better peak shape was obtained via the boronate precolumn injection, and the calculated theoretical plate number improvement was approximately two folds. The relative standard deviations for the retention time, peak area and peak height were 0.12, 3.0 and 1.8%, respectively. The system is linear (R2>0.99) within the working sample concentration and sample-volume ranges, and it presents a detection limit of 0.09 microg L(-1)(S/N=3) when a 0.2 mL sample was enriched. Recovery values of the proposed method were between 107 and 123%, and this method was applied satisfactorily to the determination of BPA in commercially available bottled drink samples. The boronate precolumn was proven to produce better sensitivity than that of an ODS or C30 precolumn as long as the enrichment of BPA in aqueous samples is concerned.

摘要

采用微柱液相色谱法研究了硼酸酯预柱在水溶液中痕量测定4,4'-异亚丙基二酚(双酚A或BPA)中的应用。双酚A通过填充有TSK(凝胶)硼酸酯的预柱进行富集,然后将其进样(反冲)到ODS分离柱中。与传统的注射器进样相比,通过硼酸酯预柱进样可获得更好的峰形,计算得到的理论塔板数提高了约两倍。保留时间、峰面积和峰高的相对标准偏差分别为0.12%、3.0%和1.8%。该系统在工作样品浓度和进样体积范围内呈线性(R2>0.99),当富集0.2 mL样品时,检测限为0.09 μg L-1(S/N=3)。该方法的回收率在107%至123%之间,并成功应用于市售瓶装饮料样品中双酚A的测定。就水样中双酚A的富集而言,硼酸酯预柱被证明比ODS或C30预柱具有更高的灵敏度。

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