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Urea functionalized surface-bonded sol-gel coating for on-line hyphenation of capillary microextraction with high-performance liquid chromatography
Journal of Chromatography A ( IF 3.8 ) Pub Date : 2018-02-19 , DOI: 10.1016/j.chroma.2018.02.033
Shehzada Muhammad Sajid Jillani , Khalid Alhooshani

Sol-gel urea functionalized-[bis(hydroxyethyl)amine] terminated polydimethylsiloxane coating was developed for capillary microextraction-high performance liquid chromatographic analysis from aqueous samples. A fused silica capillary is coated from the inside with surface bonded coating material and is created through in-situ sol-gel reaction. The urea-functionalized coating was immobilized to the inner surface of the capillary by the condensation reaction of silanol groups of capillary and sol-solution. The characterization of the coating material was successfully done by using X-ray photoelectron spectroscopy, thermogravimetric analysis, field emission scanning electron microscope, and energy dispersive X-ray spectrometer. To make a setup of online capillary microextraction-high performance liquid chromatography, the urea functionalized capillary was installed in the HPLC manual injection port. The analytes of interest were pre-concentrated in the coated sampling loop, desorbed by the mobile phase, chromatographically separated on C-18 column, and analyzed by UV detector. Sol-gel coated capillaries were used for online extraction and high-performance liquid chromatographic analysis of phenols, ketones, aldehydes, and polyaromatic hydrocarbons. This newly developed coating showed excellent extraction for a variety of analytes ranging from highly polar to non-polar in nature. The analysis using sol-gel coating showed excellent overall sensitivity in terms of lower detection limits (S/N = 3) for the analytes (0.10 ng mL−1–14.29 ng mL−1) with acceptable reproducibility that is less than 12.0%RSD (n = 3). Moreover, the capillary to capillary reproducibility of the analysis was also tested by changing the capillary of the same size. This provided excellent%RSD of less than 10.0% (n = 3).



中文翻译:

尿素功能化的表面键合溶胶-凝胶涂料,用于高效液相色谱法对毛细管微萃取进行在线联用

开发了溶胶-凝胶尿素官能化-[双(羟乙基)胺]封端的聚二甲基硅氧烷涂料,用于从含水样品中进行毛细管微萃取-高效液相色谱分析。熔融石英毛细管从内部涂有表面结合的涂料,并通过原位溶胶-凝胶反应产生。通过毛细管的硅烷醇基团和溶胶溶液的缩合反应,将尿素官能化的涂层固定在毛细管的内表面上。通过使用X射线光电子能谱,热重分析,场发射扫描电子显微镜和能量色散X射线能谱仪成功地完成了涂层材料的表征。要建立在线毛细管微萃取-高效液相色谱仪,将尿素功能化的毛细管安装在HPLC手动进样口中。感兴趣的分析物在涂层的定量环中进行预浓缩,通过流动相解吸,在C-18色谱柱上进行色谱分离,并通过UV检测器进行分析。溶胶-凝胶涂覆的毛细管用于酚,酮,醛和聚芳烃的在线提取和高效液相色谱分析。这种新开发的涂层对自然界中从高极性到非极性的各种分析物均具有出色的萃取性能。使用溶胶-凝胶涂层进行的分析显示出优异的整体灵敏度,因为对分析物(0.10 ng mL)的检测限较低(S / N = 3)经流动相解吸,在C-18色谱柱上进行色谱分离,并通过紫外检测器进行分析。溶胶-凝胶涂覆的毛细管用于酚,酮,醛和聚芳烃的在线提取和高效液相色谱分析。这种新开发的涂层对自然界中从高极性到非极性的各种分析物均具有出色的萃取性能。使用溶胶-凝胶涂层进行的分析显示出优异的整体灵敏度,因为对分析物(0.10 ng mL)的检测限较低(S / N = 3)经流动相解吸,在C-18色谱柱上进行色谱分离,并通过紫外检测器进行分析。溶胶-凝胶涂覆的毛细管用于酚,酮,醛和聚芳烃的在线提取和高效液相色谱分析。这种新开发的涂层对自然界中从高极性到非极性的各种分析物均具有出色的萃取性能。使用溶胶-凝胶涂层进行的分析显示出优异的整体灵敏度,因为对分析物(0.10 ng mL)的检测限较低(S / N = 3)这种新开发的涂层对自然界中从高极性到非极性的各种分析物均具有出色的萃取性能。使用溶胶-凝胶涂层进行的分析显示出优异的整体灵敏度,因为对分析物(0.10 ng mL)的检测限较低(S / N = 3)这种新开发的涂层对自然界中从高极性到非极性的各种分析物均具有出色的萃取性能。使用溶胶-凝胶涂层进行的分析显示出优异的整体灵敏度,因为对分析物(0.10 ng mL)的检测限较低(S / N = 3)-1 –14.29 ng mL -1)的可接受的再现性小于12.0%RSD(n = 3)。此外,还通过更改相同尺寸的毛细管来测试毛细管对毛细管的重现性分析。这提供了低于10.0%(n = 3)的出色%RSD。

更新日期:2018-02-19
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