摘要
合成了奎宁衍生物O-9-(叔丁基氨基甲酰基)-11-[(2-甲基丙烯酰氧基)乙硫基]-10,11,-二氢奎宁(MBQN),并通过液质联用、核磁氢谱及红外光谱对其进行了表征。以MBQN为手性功能单体,甲基丙烯酸羟基乙酯(HEMA)为非手性功能单体,乙二醇二甲基丙烯酸酯(EDMA)为交联剂,环己醇、十二醇为二元制孔剂,偶氮二异丁腈(AIBN)为热引发剂,在100μm内径的熔融石英毛细管内采用原位热聚合法制备了Poly(MBQN-co-HEMA-co-EDMA)手性毛细管整体柱。通过元素分析、扫描电镜及压汞仪测试了整体柱固定相的组成、形貌、孔容、孔径及比表面积。采用自组装微流液相色谱对Poly(MBQN-co-HEMA-co-EDMA)整体柱的分离性能进行了评价,基线分离了8种氨基酸衍生物。以N-Bz-DL-Leu为测试对象评测了整体柱的重现性,其各相对标准偏差(RSD)均符合要求。结果表明此整体柱针对氨基酸衍生物分离性能良好,重现性优异。
O-9-（tert-butylcarbamoyl）-11-[（2-methacryloyloxy）ethylthio]-10,11,-dihydroquinine（MBQN） was prepared and characterized by HPLC-MS,NMR and IR. A poly（MBQN-co-HEMA-co-EDMA） chiral monolithic column was prepared via in-situ thermal polymerization in 100 μm inner diameter fused-silica capillary using MBQN as chiral function monomer, hydroxyethyl methacrylate（HEMA） as achiral functional monomer, ethylene glycol dimethacrylate（EDMA） as crosslinking agent, cyclohexanol and dodecanol as binary porogens and azobisisobutyronitrile（AIBN） as thermal initiator. Composition, morphology, pore volume, pore size and specific surface area of the stationary phase of the monolithic column were studied by elemental analysis, scanning electron microscopy and mercury porosimetry. The separation performance of the poly（MBQN-co-HEMA-co-EDMA） monolithic column was evaluated by self assembled microfluidic liquid chromatography to separated 8 amino acid derivatives. The reproducibility of the monolithic column was evaluated with N-Bz-DL-Leu as the test object, and its relative standard deviations（RSD） met the requirements. The results show that the monolithic column has fair separation performance for amino acid derivatives and good reproducibility.
作者
李晨亮
张毅军
赵富强
章亚东
张裕平
LI Chen-liang;ZHANG Yi-jun;ZHAO Fu-qiang;ZHANG Ya-dong;ZHANG Yu-ping(School of Chemical Engineering and Energy,Zhengzhou University,Zhengzhou 450001,China;College of Chemistry and Chemical Engineering,Henan Institute of Science and Technology,Xinxiang 453003,China)
出处
《高校化学工程学报》
EI
CAS
CSCD
北大核心
2018年第5期1210-1216,共7页
Journal of Chemical Engineering of Chinese Universities
基金
NSFC-河南联合基金面上项目(162300410253)
国家自然科学基金青年科学基金项目(21706240)
河南省科技攻关计划(重点)项目(142102210047)
河南省科技计划项目(172102210085)
关键词
奎宁衍生物
手性整体柱
微流液相色谱
氨基酸衍生物
quinine derivatives
chiral monolithic column
microfluidic liquid chromatography
amino acid derivatives
