Jillani Shehzada Muhammad Sajid, Alhooshani Khalid
Department of Chemistry, King Fahd University of Petroleum & Minerals, Dhahran, Saudi Arabia.
J Sep Sci. 2019 Jul;42(14):2435-2443. doi: 10.1002/jssc.201900179. Epub 2019 May 27.
This work about the development of yttria-based polymeric coating using [bis(hydroxyethyl) amine] terminated polydimethylsiloxanes and yttrium trimethoxyethoxide inside the capillary. The coated capillary was utilized for online capillary microextraction and high-performance liquid chromatography analysis. The prepared coating material was characterized using scanning electron microscopy, X-ray photoelectron spectroscopy, energy dispersive X-ray spectrometry, and thermogravimetric analysis. The coated capillary with polymer presented better extraction efficiency compared with the pure yttria-based coated capillary with applicability in extreme pH environments (pH 0-pH 14). Excellent extraction towards polyaromatic hydrocarbons, aldehydes, ketones, alcohols, phenols, and amides was observed with limit of detection ranging from 0.18 to 7.35 ng/mL (S/N = 3) and reproducibility in between 0.6 and 6.8% (n = 3). Capillary-to-capillary extraction analysis has presented reproducibility between 4.1 and 9.9%. The analysis provided linear response for seven selected phenols in the range of 5-200 ng/mL with R values between 0.9971 and 0.9998. The inter-day, intra-day, and capillary-to-capillary reproducibility for phenols was also <10%. Real sample analysis by spiking 5, 50, and 200 ng/mL of phenols in wastewater and pool-water produced recovery between 84.7 and 94.3% and reproducibility within 7.6% (n = 3).
这项工作是关于在毛细管内使用[双（羟乙基）胺]封端的聚二甲基硅氧烷和三甲氧基乙醇钇开发氧化钇基聚合物涂层。涂覆的毛细管用于在线毛细管微萃取和高效液相色谱分析。使用扫描电子显微镜、X射线光电子能谱、能量色散X射线光谱和热重分析对制备的涂层材料进行了表征。与纯氧化钇基涂覆毛细管相比，聚合物涂覆的毛细管在极端pH环境（pH 0 - pH 14）中具有更好的萃取效率，且适用性更强。观察到对多环芳烃、醛、酮、醇、酚和酰胺具有优异的萃取效果，检测限在0.18至7.35 ng/mL之间（S/N = 3），重现性在0.6%至6.8%之间（n = 3）。毛细管间萃取分析的重现性在4.1%至9.9%之间。该分析对七种选定的酚在5 - 200 ng/mL范围内提供了线性响应，R值在0.9971至0.9998之间。酚的日间、日内和毛细管间重现性也<10%。通过在废水和池水中加入5、50和200 ng/mL的酚进行实际样品分析，回收率在84.7%至94.3%之间，重现性在7.6%以内（n = 3）。
