色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
5期
447-451
,共5页
窦阿波%邹存杰%单圆鸿%石先哲%许国旺
竇阿波%鄒存傑%單圓鴻%石先哲%許國旺
두아파%추존걸%단원홍%석선철%허국왕
毛细管高效液相色谱%毛细管整体柱%制备%混合模式
毛細管高效液相色譜%毛細管整體柱%製備%混閤模式
모세관고효액상색보%모세관정체주%제비%혼합모식
capillary high performance liquid chromatography%capillary monolithic column%preparation%mixed-mode
混合模式毛细管整体色谱柱由于保留机理多样,具有很好的应用前景。本文以[2-(甲基丙烯酰基氧基)乙基]二甲基-(3-磺酸丙基)氢氧化铵( SPE )为单体,乙二醇二甲基丙烯酸酯( EDMA )为交联剂,偶氮二异丁腈( AIBN)为引发剂,正丙醇/1,4-丁二醇/水三元体系为致孔剂,制备了聚合物基质 SPE-co-EDMA 毛细管液相色谱整体柱。通过系统优化致孔剂和反应物种类和配比、引发剂的用量、反应时间和反应温度等因素,提高了整体柱的柱效、机械强度、渗透性和重复性。结果表明该毛细管整体柱在10 MPa 内具有良好的机械强度,渗透性为2.17×10-14 m2,而且批次内和批次间峰面积的重现性(RSD)分别为1.0%和4.6%。以极性和非极性的多种化合物评价了该毛细管整体柱的色谱性能,结果表明该柱在高有机相中具有亲水相互作用机理,在低有机相中具有反相作用机理,显示出混合模式分离特性。
混閤模式毛細管整體色譜柱由于保留機理多樣,具有很好的應用前景。本文以[2-(甲基丙烯酰基氧基)乙基]二甲基-(3-磺痠丙基)氫氧化銨( SPE )為單體,乙二醇二甲基丙烯痠酯( EDMA )為交聯劑,偶氮二異丁腈( AIBN)為引髮劑,正丙醇/1,4-丁二醇/水三元體繫為緻孔劑,製備瞭聚閤物基質 SPE-co-EDMA 毛細管液相色譜整體柱。通過繫統優化緻孔劑和反應物種類和配比、引髮劑的用量、反應時間和反應溫度等因素,提高瞭整體柱的柱效、機械彊度、滲透性和重複性。結果錶明該毛細管整體柱在10 MPa 內具有良好的機械彊度,滲透性為2.17×10-14 m2,而且批次內和批次間峰麵積的重現性(RSD)分彆為1.0%和4.6%。以極性和非極性的多種化閤物評價瞭該毛細管整體柱的色譜性能,結果錶明該柱在高有機相中具有親水相互作用機理,在低有機相中具有反相作用機理,顯示齣混閤模式分離特性。
혼합모식모세관정체색보주유우보류궤리다양,구유흔호적응용전경。본문이[2-(갑기병희선기양기)을기]이갑기-(3-광산병기)경양화안( SPE )위단체,을이순이갑기병희산지( EDMA )위교련제,우담이이정정( AIBN)위인발제,정병순/1,4-정이순/수삼원체계위치공제,제비료취합물기질 SPE-co-EDMA 모세관액상색보정체주。통과계통우화치공제화반응물충류화배비、인발제적용량、반응시간화반응온도등인소,제고료정체주적주효、궤계강도、삼투성화중복성。결과표명해모세관정체주재10 MPa 내구유량호적궤계강도,삼투성위2.17×10-14 m2,이차비차내화비차간봉면적적중현성(RSD)분별위1.0%화4.6%。이겁성화비겁성적다충화합물평개료해모세관정체주적색보성능,결과표명해주재고유궤상중구유친수상호작용궤리,재저유궤상중구유반상작용궤리,현시출혼합모식분리특성。
Based on the diversity of the retention mechanism ,mixed-mode capillary monolithic columns have broad application prospect. In this work,a novel capillary polymer monolithic column was prepared with [ 2-( methacryloyloxy )ethyl ]dimethyl-( 3-sulfopropyl )ammonium hydroxide( SPE)as monomer,ethylene dimethacrylate( EDMA)as crosslinking agent,azobi-sisobutyronitrile( AIBN ) as initiator and butylalcohol/1,4-butanediol/water as ternary poro-gens. Under the optimized reaction conditions including the proportion of monomer and poro-gens,amount of initiator,reaction temperature and polymerization time,the monolithic col-umn showed good mechanical strength up to 10 MPa,high permeability of 2. 17 × 10-14 m 2 and good repeatability. The peak area RSDs of column-to-column and batch-to-batch reproducibility were 1. 0% and 4. 6%,respectively. Finally,the capillary monolithic column was evaluated with polar and non-polar test mixtures. It showed hydrophilic interaction under high organic phase while hydrophobic interaction under low organic phase,indicating it a mixed-mode monolithic column.