Department of Chemistry, King Fahd University of Petroleum & Minerals, Dhahran 31261, Saudi Arabia.
Department of Chemistry, King Fahd University of Petroleum & Minerals, Dhahran 31261, Saudi Arabia.
J Chromatogr A. 2018 Mar 30;1543:14-22. doi: 10.1016/j.chroma.2018.02.033. Epub 2018 Feb 19.
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-14.29 ng mL) 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).
用于从水样中进行毛细管微萃取-高效液相色谱分析的溶胶-凝胶尿素功能化-[双（羟乙基）胺]封端聚二甲基硅氧烷涂层被开发出来。将涂覆有表面结合涂层材料的熔融石英毛细管从内部涂覆，并通过原位溶胶-凝胶反应进行涂覆。尿素功能化涂层通过毛细管和溶胶溶液中的硅醇基团的缩合反应固定在毛细管的内表面上。通过 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 射线光谱仪成功地对涂层材料进行了表征。为了建立在线毛细管微萃取-高效液相色谱的设置，将尿素功能化毛细管安装在 HPLC 手动进样口。将感兴趣的分析物在涂覆的取样环中预浓缩，通过流动相解吸，在 C-18 柱上进行色谱分离，并用 UV 检测器进行分析。溶胶-凝胶涂覆的毛细管用于在线提取和高效液相色谱分析酚类、酮类、醛类和多环芳烃。这种新开发的涂层对各种分析物表现出优异的萃取性能，范围从高度极性到非极性。使用溶胶-凝胶涂层进行分析时，分析物的检测限（S/N=3）较低（0.10ng mL-1-4.29ng mL-1），重现性良好，小于 12.0%RSD（n=3）。此外，还通过更换相同尺寸的毛细管来测试分析的毛细管到毛细管重现性。这提供了小于 10.0%的出色%RSD（n=3）。
