色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
8期
791-797
,共7页
毛细管电色谱%聚(甲基丙烯酸缩水甘油酯-乙二醇二甲基丙烯酸酯)整体柱%胃蛋白酶亲和手性整体柱%碱性药物%手性分离
毛細管電色譜%聚(甲基丙烯痠縮水甘油酯-乙二醇二甲基丙烯痠酯)整體柱%胃蛋白酶親和手性整體柱%堿性藥物%手性分離
모세관전색보%취(갑기병희산축수감유지-을이순이갑기병희산지)정체주%위단백매친화수성정체주%감성약물%수성분리
capillary electrochromatography ( CEC )%poly ( glycidyl methacrylate-co-
以热引发原位聚合方法制备了聚(甲基丙烯酸缩水甘油酯(glycidyl methacrylate,GMA)-乙二醇二甲基丙烯酸酯(ethyleneglycol dimethacrylate,EDMA))毛细管整体柱,对整体柱的性能进行了表征。结果表明,柱内部结构均匀、渗透性好;整体柱能够实现苯等中性小分子化合物的分离,具有反相色谱特征,重现性和稳定性良好。利用整体柱环氧基团的活性,采用间接法,以戊二醛为连接臂制备胃蛋白酶亲和手性整体柱。在毛细管电色谱模式下进行了柱分离性能研究,并对缓冲液 pH 值和运行电压等分离条件进行了考察。结果表明,亲和整体柱对4种碱性手性药物(奈福泮、氨氯地平、西酞普兰、扑尔敏)有拆分效果,奈福泮、氨氯地平、西酞普兰能达到基线分离。本文为蛋白质亲和毛细管电色谱整体柱的制备和应用提供了新的思路和方法。
以熱引髮原位聚閤方法製備瞭聚(甲基丙烯痠縮水甘油酯(glycidyl methacrylate,GMA)-乙二醇二甲基丙烯痠酯(ethyleneglycol dimethacrylate,EDMA))毛細管整體柱,對整體柱的性能進行瞭錶徵。結果錶明,柱內部結構均勻、滲透性好;整體柱能夠實現苯等中性小分子化閤物的分離,具有反相色譜特徵,重現性和穩定性良好。利用整體柱環氧基糰的活性,採用間接法,以戊二醛為連接臂製備胃蛋白酶親和手性整體柱。在毛細管電色譜模式下進行瞭柱分離性能研究,併對緩遲液 pH 值和運行電壓等分離條件進行瞭攷察。結果錶明,親和整體柱對4種堿性手性藥物(奈福泮、氨氯地平、西酞普蘭、撲爾敏)有拆分效果,奈福泮、氨氯地平、西酞普蘭能達到基線分離。本文為蛋白質親和毛細管電色譜整體柱的製備和應用提供瞭新的思路和方法。
이열인발원위취합방법제비료취(갑기병희산축수감유지(glycidyl methacrylate,GMA)-을이순이갑기병희산지(ethyleneglycol dimethacrylate,EDMA))모세관정체주,대정체주적성능진행료표정。결과표명,주내부결구균균、삼투성호;정체주능구실현분등중성소분자화합물적분리,구유반상색보특정,중현성화은정성량호。이용정체주배양기단적활성,채용간접법,이무이철위련접비제비위단백매친화수성정체주。재모세관전색보모식하진행료주분리성능연구,병대완충액 pH 치화운행전압등분리조건진행료고찰。결과표명,친화정체주대4충감성수성약물(내복반、안록지평、서태보란、복이민)유탁분효과,내복반、안록지평、서태보란능체도기선분리。본문위단백질친화모세관전색보정체주적제비화응용제공료신적사로화방법。
The protein modified monolithic column in affinity capillary electrochromatography (CEC)has attracted considerable attention over the past decades because of its great enanti-oseparation ability. A porous polymethacrylate ester-based capillary monolithic column poly (glycidyl methacrylate-co-ethyleneglycol dimethacrylate )( poly( GMA-co-EDMA )) was pre-pared by in situ co-polymerization. The process was initiated thermally by azobisisobutyronitrile (AIBN). The polymerization mixture contained GMA as the function monomer and EDMA as the crosslinking agent with 1,4-butanediol and 1-propanol as the binary porogen solvent. Under the optimized reaction conditions,including the proportion of monomer and porogens,reaction temperature etc,the column exhibited a uniform structure,sufficient permeability and excel-lent pressure resistance. The separation of alkyl benzenes on the column was mainly based on typical reversed-phase chromatographic retention mechanism. The reproducibility and stability were good with RSDs less than 9. 0% . A pepsin functionalized organic polymer monolith was prepared by covalently bonded pepsin to poly(GMA-co-EDMA)monolith with glutaraldehyde as a spacer based on the activity of epoxide group. The enantioseparation performance of the pep-sin affinity monolith for basic enantiomers has been investigated by CEC. Nefopam,amlodip-ine,citalopram and chlorpheniramine were resolved,and baseline separations of nefopam, amlodipine,citalopram were achieved. The influences of pH,operating voltage,temperature and sample quantity used on the chiral separation were studied. The chiral recognition mecha-nism of enantiomers on the monolithic column in CEC is discussed. This work developed a new method for the preparation and application of protein affinity monolith in CEC.