大管电色谱技术和毛细管电色谱新型固定相研究

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1、天津大学博士学位论文大管电色谱技术和毛细管电色谱新型固定相研究姓名：袁瑞娟申请学位级别：博士专业：应用化学指导教师：包建民20070501体柱上，易于除去磺酸化过程中产生的高浓度无机盐。将其用于手性药物的拆分，得到了较好的分离效果，并且分离速度快，对测定的手性样品20min内均能实现分离，部分样品十分钟之内即可以实现分离。3．有机硅树状化合物填充柱CEC本文首次将有机硅树状化合物固定相用于毛细管电色谱填充柱研究。实验结果表明，树状填料具有典型的反相色谱性质，在低的键合量情况下具有较好的疏水性能，将其用于中性化合物

2、分离时取得了较好的效果，对于硫脲柱效将近90000Nm～。关键词：电色谱：大管；焦耳热；手性拆分；整体柱；有机硅树状化合物；填充柱nABSTRACTCapillaryelectrochromatographyisanewmicro—separationtechniquewithhighperformanceandfastspeed．Muchresearchisfocusedonitstheory,columntechnique，newstationaryphaseandapplication．Themainwor

3、kofthisdissertationiSshownasfollow：1．Wideboreelectrochromatography(WE)techniqueTheseparationchannelofCECisrestrictedtocapillaryscalewithidsmallerthan100gtnduetothelimitofJouleheat，whichresultsinlowloadabilityandpoorconcentrationdetectability．Inordertosolvethi

4、sproblem，anewdevicewassetuptoperformwideboreelectrochromatography．AquartztubewithmillimeteridwasusedastheseparationchannelandapropercoolantwaspumpedthroughtheinnercoolingcapillarywhichiscoaxiallyinsertedintotheseparationchanneltodispeltheJouleheatgenerateddur

5、ingelectrophoresis．TheWEsystemmadeitpossibletoperformelectrochromatographyinawideboretube．PolyacrylamidemonolithiccolumnwaspreparedsuccessfullyOiltheWEsystem．Thecolumnwasevaluatedintheelectrochromatographymodeusingthiourea，naphthaleneandbiphenylasprobecompoun

6、ds．ResultsindicatedthatthissystemcandissipateJouleheatinsituinrealtime，andhashigherloadabilitycomparedwithCEC．AgarosegelcolumnwaspreparedontheWEsystem．Higherelectricfieldstrengthcouldbeappliedacrossthegelcolumnduetotheinnercoolingmechanism，whichmadetheseparat

7、ionfasterthanconventionalagarosegelelectophoresis．Atthesametime，lowerconcentrationdetectablilitywasobtainedduetodirectUVdetectionandlongerlightdistance．2．Sulfatedpoly(IB-cyclodextrin)silica-basedmonolithiccolumnforCECAsulfatedpoly(IB-cyclodextrin)silica-based

8、monolithiccolumnwaspreparedincapillary．ThenitwasevaluatedintheCECmode．Goodenantiomericseparationswereobtainedwhenthecolumnwasappliedinchiralseparation．3．Carbosilanedendrimerpackedcolumnfo