Qu Qishu, Liu Yuanyuan, Shi Wenjun, Yan Chao, Tang Xiaoqing
Key Laboratory of Functional Molecule Design and Interface Process, School of Materials and Chemical Engineering, Anhui Jianzhu University, Hefei 230601, China.
School of Pharmacy, Shanghai Jiao Tong University, Shanghai 200240, China.
J Chromatogr A. 2015 Jun 19;1399:25-31. doi: 10.1016/j.chroma.2015.04.037. Epub 2015 Apr 27.
A simple coating procedure employing a multilayer-by-multilayer process to modify the inner surface of bare fused-silica capillaries with silica nanoparticles was established. The silica nanoparticles were adsorbed onto the capillary wall via a strong electrostatic interaction between amino functional groups and silica particles. The thickness of the coating could be tuned from 130 to 600 nm by increasing the coating cycles from one to three. Both the retention factor and the resolution were greatly increased with increasing coating cycles. The loading capacity determined by naphthalene in the column with three coating cycles is 152.1 pmol. The effects of buffer concentration and pH value on the stability of the coating were evaluated. The retention reproducibility of the separation of toluene was 0.8, 1.2, 2.3, and 4.5%, respectively, for run-to-run, day-to-day, column-to-column, and batch-to-batch, respectively. The chromatographic performance of these columns was evaluated by both capillary liquid chromatography and open-tubular capillary electrochromatography (OT-CEC). Separation of aromatic hydrocarbons in the column with three coating cycles provided high theoretical plate numbers (up to 269,280 plates m(-1) for toluene) and short separation time (<15 min) by using OT-CEC mode. The method was also used to separate egg white proteins. Both acidic and basic proteins as well as four glycoisoforms were separated in a single run.
建立了一种采用多层叠加工艺，用二氧化硅纳米颗粒修饰裸露熔融石英毛细管内表面的简单涂层方法。通过氨基官能团与二氧化硅颗粒之间的强静电相互作用，二氧化硅纳米颗粒吸附在毛细管壁上。通过将涂层循环次数从1次增加到3次，涂层厚度可在130至600nm之间调节。随着涂层循环次数的增加，保留因子和分离度均显著提高。在具有三次涂层循环的柱中，萘测定的负载量为152.1pmol。评估了缓冲液浓度和pH值对涂层稳定性的影响。甲苯分离的保留重现性在批内、批间、柱间和批次间分别为0.8%、1.2%、2.3%和4.5%。通过毛细管液相色谱和开管毛细管电色谱（OT-CEC）对这些柱的色谱性能进行了评估。在具有三次涂层循环的柱中，采用OT-CEC模式分离芳烃，提供了高理论塔板数（甲苯高达269280块/m）和短分离时间（<15分钟）。该方法还用于分离蛋清蛋白。一次进样即可分离酸性和碱性蛋白质以及四种糖异构体。
