Institute of Pharmaceutical Analysis, College of Pharmacy, Jinan University, Guangzhou 510632, China; Department of Pharmacy and Guangdong Province Key Laboratory of Pharmacodynamic Constituents of Traditional Chinese Medicine & New Drug Research, Jinan University, Guangzhou 510632, China; Departamento de Química Analítica, Química Física e Ingeniería Química, Universidad de Alcalá, Ctra. Madrid-Barcelona Km. 33.600, 28871 Alcalá de Henares, Madrid, Spain.
Institute of Pharmaceutical Analysis, College of Pharmacy, Jinan University, Guangzhou 510632, China; Department of Pharmacy and Guangdong Province Key Laboratory of Pharmacodynamic Constituents of Traditional Chinese Medicine & New Drug Research, Jinan University, Guangzhou 510632, China.
J Chromatogr A. 2019 May 24;1593:63-72. doi: 10.1016/j.chroma.2019.01.065. Epub 2019 Jan 24.
An O-[2-(methacryloyloxy)-ethylcarbamoyl]-10,11-dihydroquinidine (MQD)-silica hybrid monolithic column was prepared by a facile "one-step" strategy within a 100 μm I.D. capillary. The influence of the methanol, ethylene glycol and water volume ratio, reaction temperature and time, cetyltrimethylammonium bromide and MQD monomers content and volume ratio of tetramethoxysilane and vinyltrimethoxysilane was investigated to obtain a satisfactory morphology of monolithic columns. The optimized MQD-silica hybrid monolithic column was evaluated in terms of permeability, stability, efficiency, reproducibility, and was characterized by scanning electron microscopy and nano-liquid chromatography. Among the 52 N-derivatized protein and non-protein amino acids, a total of 44 analytes could be baseline enantioseparated using the optimized conditions in either reversed phase mode (RPM) or polar organic phase mode (POM). The results showed that POM (ACN/MeOH/HAc/TEA (60/40/0.055/0.005, v/v/v/v)) offered better performance than RPM (10 mM ammonium acetate/ACN (30/70, v/v) (apparent pH=5.3)) in terms of enantioresolution and efficiency with shorter analysis times.
一种 O-[2-(甲基丙烯酰氧基)乙基氨基甲酰基]-10,11-二氢奎宁（MQD）-硅胶杂化整体柱是通过在 100μm ID 毛细管内的简便“一步”策略制备的。考察了甲醇、乙二醇和水的体积比、反应温度和时间、十六烷基三甲基溴化铵和 MQD 单体含量以及四甲氧基硅烷和乙烯基三甲氧基硅烷的体积比对整体柱形态的影响，以获得满意的整体柱形态。优化后的 MQD-硅胶杂化整体柱的渗透性、稳定性、效率、重现性进行了评价，并通过扫描电子显微镜和纳米液相色谱进行了表征。在 52 种 N-衍生化蛋白和非蛋白氨基酸中，使用优化条件，在反相模式（RPM）或极性有机相模式（POM）下，可基线分离出 44 种分析物。结果表明，与 RPM（10mM 乙酸铵/ACN（30/70，v/v）（表观 pH=5.3）相比，POM（ACN/MeOH/HAc/TEA（60/40/0.055/0.005，v/v/v/v））在分离度和效率方面具有更好的性能，同时分析时间更短。
