分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2001年
3期
299-302
,共4页
叶明亮%邹汉法%雷政登%吴仁安%倪坚毅
葉明亮%鄒漢法%雷政登%吳仁安%倪堅毅
협명량%추한법%뢰정등%오인안%예견의
毛细管电色谱%动态改性%吸附固定相%手性分离
毛細管電色譜%動態改性%吸附固定相%手性分離
모세관전색보%동태개성%흡부고정상%수성분리
对动态改性电色谱手性分离进行了研究。电色谱柱填充强阴离子交换固定相(SAX),添加在流动相中的磺化β-环糊精(S-CD)动态地吸附于SAX填料表面,形成一层准手性固定相。色氨酸、阿托品和异博定对映体在本体系获得了很好的分离,它们的分离度分别为2.06,10.1和1.96,对映体峰的柱效介于85,000塔板数/米和412,000塔板数/米之间。连续运行17次,死时间和色氨酸对映体的电色谱保留因子的相对标准偏差分别为0.53%,0.62%和0.69%。此外,以吸附于SAX填料的牛血清白蛋白和S-CD为手性固定相进行了电色谱手性分离的研究。在这两种体系下分离色氨酸对映体的分离度分别为3.86和2.97。吸附S-CD柱电色谱和动态改性电色谱的重现性进行了比较,发现动态改性电色谱有更好的重现性。
對動態改性電色譜手性分離進行瞭研究。電色譜柱填充彊陰離子交換固定相(SAX),添加在流動相中的磺化β-環糊精(S-CD)動態地吸附于SAX填料錶麵,形成一層準手性固定相。色氨痠、阿託品和異博定對映體在本體繫穫得瞭很好的分離,它們的分離度分彆為2.06,10.1和1.96,對映體峰的柱效介于85,000塔闆數/米和412,000塔闆數/米之間。連續運行17次,死時間和色氨痠對映體的電色譜保留因子的相對標準偏差分彆為0.53%,0.62%和0.69%。此外,以吸附于SAX填料的牛血清白蛋白和S-CD為手性固定相進行瞭電色譜手性分離的研究。在這兩種體繫下分離色氨痠對映體的分離度分彆為3.86和2.97。吸附S-CD柱電色譜和動態改性電色譜的重現性進行瞭比較,髮現動態改性電色譜有更好的重現性。
대동태개성전색보수성분리진행료연구。전색보주전충강음리자교환고정상(SAX),첨가재류동상중적광화β-배호정(S-CD)동태지흡부우SAX전료표면,형성일층준수성고정상。색안산、아탁품화이박정대영체재본체계획득료흔호적분리,타문적분리도분별위2.06,10.1화1.96,대영체봉적주효개우85,000탑판수/미화412,000탑판수/미지간。련속운행17차,사시간화색안산대영체적전색보보류인자적상대표준편차분별위0.53%,0.62%화0.69%。차외,이흡부우SAX전료적우혈청백단백화S-CD위수성고정상진행료전색보수성분리적연구。재저량충체계하분리색안산대영체적분리도분별위3.86화2.97。흡부S-CD주전색보화동태개성전색보적중현성진행료비교,발현동태개성전색보유경호적중현성。
A novel mode of chiral separation in electrochromatography (CEC) with dynamically modified stationary phase (DMS-CEC) was presented. The capillary column was packed with strong anionic exchange stationary phase, the sulfated β-cyclodextrin (S-CD), which was added in the mobile phase, dynamically adsorbed to the packing surface and a new layer of chiral stationary phase was formed. The separation of enantiomer was based on their different interaction with the new stationary phase. The enantionmers of tryptophan, atropine and verapamil were successfully separated in this system with resolution of 2.06, 10.1 and 1.96, and the column effeciency for the enantiomers were varied from 85000 plates/m to 412000 plates/m. The relative standard deviation (RSD) of void time and the tryptophan enantiomers′ migration time for 17 consecutive runs were 0.5%, 0.6% and 0.7%, respectively. Enantiomer separation by capillary electrochromatography with adsorbed bovine serum albumin (BSA) and sulfated cyclodextrin (S-CD) as chiral stationary phases were also studied. The resolution for tryptophan enantiomers in the two systems were 3.86 and 2.97, respectively. It was found that the superiority of DMS-CEC over the adsorbed S-CD column CEC was that better repeatability could be obtained in DMS-CEC.