Tran MinhPhuong, Turner Erica B, Segro Scott S, Fang Li, Seyyal Emre, Malik Abdul
Department of Chemistry, University of South Florida, 4202 E. Fowler Avenue, CHE 205, Tampa, FL 33620-5250, USA.
Department of Chemistry, University of South Florida, 4202 E. Fowler Avenue, CHE 205, Tampa, FL 33620-5250, USA.
J Chromatogr A. 2017 Nov 3;1522:38-47. doi: 10.1016/j.chroma.2017.09.048. Epub 2017 Sep 22.
A sol-gel organic-inorganic hybrid sorbent, consisting of chemically integrated tantalum (V) ethoxide (TaEO) and polypropylene glycol methacrylate (PPGM), was developed for capillary microextraction (CME). The sol-gel sorbent was synthesized within a fused silica capillary through hydrolytic polycondensation of TaEO and chemical incorporation of PPGM into the evolving sol-gel tantala network. A part of the organic-inorganic hybrid sol-gel network evolving in the vicinity of the capillary walls had favorable conditions to get chemically bonded to the silanol groups on the capillary surface forming a surface-bonded coating. The newly developed sol-gel sorbent was employed to isolate and enrich a variety of analytes from aqueous samples for on-line analysis by high-performance liquid chromatography (HPLC) equipped with a UV detector. CME was performed on aqueous samples containing trace concentrations of analytes representing polycyclic aromatic hydrocarbons, ketones, alcohols, amines, nucleosides, and nucleotides. This sol-gel hybrid coating provided efficient extraction with CME-HPLC detection limits ranging from 4.41pM to 28.19 pM. Due to direct chemical bonding between the sol-gel sorbent coating and the fused silica capillary inner surface, this sol-gel sorbent exhibited enhanced solvent stability. The sol-gel tantala-based sorbent also exhibited excellent pH stability over a wide pH range (pH 0-pH 14). Furthermore, it displayed great performance reproducibility in CME-HPLC providing run-to-run HPLC peak area relative standard deviation (RSD) values between 0.23% and 3.83%. The capillary-to-capillary RSD (n=3), characterizing capillary preparation method reproducibility, ranged from 0.24% to 4.11%. The results show great performance consistency and application potential for the sol-gel tantala-PPGM sorbent in various fields including biomedical, pharmaceutical, and environmental areas.
一种由化学整合的乙醇钽（V）（TaEO）和聚丙二醇甲基丙烯酸酯（PPGM）组成的溶胶-凝胶有机-无机杂化吸附剂被开发用于毛细管微萃取（CME）。该溶胶-凝胶吸附剂是通过TaEO的水解缩聚以及PPGM化学掺入到不断形成的溶胶-凝胶钽酸盐网络中，在熔融石英毛细管内合成的。在毛细管内壁附近形成的部分有机-无机杂化溶胶-凝胶网络具有良好的条件，能够与毛细管表面的硅醇基团发生化学键合，形成表面键合涂层。新开发的溶胶-凝胶吸附剂用于从水样中分离和富集各种分析物，以便通过配备紫外检测器的高效液相色谱（HPLC）进行在线分析。对含有痕量分析物（代表多环芳烃、酮、醇、胺、核苷和核苷酸）的水样进行了CME。这种溶胶-凝胶杂化涂层提供了高效萃取，CME-HPLC检测限范围为4.41pM至28.19pM。由于溶胶-凝胶吸附剂涂层与熔融石英毛细管内表面之间的直接化学键合，这种溶胶-凝胶吸附剂表现出增强的溶剂稳定性。基于溶胶-凝胶钽酸盐的吸附剂在很宽的pH范围（pH 0 - pH 14）内也表现出优异的pH稳定性。此外，它在CME-HPLC中表现出出色的性能重现性，HPLC峰面积的逐次运行相对标准偏差（RSD）值在0.23%至3.83%之间。表征毛细管制备方法重现性的毛细管间RSD（n = 3）范围为0.24%至4.11%。结果表明，溶胶-凝胶钽酸盐-PPGM吸附剂在生物医学、制药和环境等各个领域具有出色的性能一致性和应用潜力。
