分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2010年
2期
192-196
,共5页
叶芳贵%韩燕燕%王顺%黄保军%赵书林
葉芳貴%韓燕燕%王順%黃保軍%趙書林
협방귀%한연연%왕순%황보군%조서림
毛细管电色谱%硅胶整体柱%溶胶-凝胶%混合模式
毛細管電色譜%硅膠整體柱%溶膠-凝膠%混閤模式
모세관전색보%규효정체주%용효-응효%혼합모식
Capillary electrochromatography%Silica monolithic column%Sol-gel%Mixed mode
采用溶胶-凝胶技术制备了丁基胺丙基硅胶毛细管整体柱, 此整体固定相表面同时含有能产生阳极的电渗流的仲胺官能团和产生疏水作用的正丁基和丙基官能团.对所制备的整体柱电色谱性能进行了详细的表征和分析.考察了流动相pH值对电渗流的影响;对烷基苯同系物、有机酸酸性化合物和苯胺类碱性化合物保留行为进行了研究,并对其可能的保留机理进行了探讨.实验结果表明, 对于中性化合物的保留机理主要基于反相作用;而对于酸性化合物的保留行为则是基于混合模式作用机理,即除了电泳作用外,还包括阴离子交换和疏水作用.碱性化合物在丁基胺丙基硅胶毛细管整体柱上的峰形较好,没有明显的峰拖尾现象.
採用溶膠-凝膠技術製備瞭丁基胺丙基硅膠毛細管整體柱, 此整體固定相錶麵同時含有能產生暘極的電滲流的仲胺官能糰和產生疏水作用的正丁基和丙基官能糰.對所製備的整體柱電色譜性能進行瞭詳細的錶徵和分析.攷察瞭流動相pH值對電滲流的影響;對烷基苯同繫物、有機痠痠性化閤物和苯胺類堿性化閤物保留行為進行瞭研究,併對其可能的保留機理進行瞭探討.實驗結果錶明, 對于中性化閤物的保留機理主要基于反相作用;而對于痠性化閤物的保留行為則是基于混閤模式作用機理,即除瞭電泳作用外,還包括陰離子交換和疏水作用.堿性化閤物在丁基胺丙基硅膠毛細管整體柱上的峰形較好,沒有明顯的峰拖尾現象.
채용용효-응효기술제비료정기알병기규효모세관정체주, 차정체고정상표면동시함유능산생양겁적전삼류적중알관능단화산생소수작용적정정기화병기관능단.대소제비적정체주전색보성능진행료상세적표정화분석.고찰료류동상pH치대전삼류적영향;대완기분동계물、유궤산산성화합물화분알류감성화합물보류행위진행료연구,병대기가능적보류궤리진행료탐토.실험결과표명, 대우중성화합물적보류궤리주요기우반상작용;이대우산성화합물적보류행위칙시기우혼합모식작용궤리,즉제료전영작용외,환포괄음리자교환화소수작용.감성화합물재정기알병기규효모세관정체주상적봉형교호,몰유명현적봉타미현상.
A novel silica monolithic stationary phase functionalized with butylaminopropyl ligands for capillary electrochromatography(CEC) has been presented. The monolithic capillary columns were prepared by a sol-gel) process and subsequent a chemical modification. The amino groups on the surface of the stationary phase are meant to generate a substantial anodic electroosmotic flow (EOF). The butyl and propyl groups provide) hydrophobic properties. To evaluate the column performance, effects of buffer pH and organic modifier content on the EOF and electrochromatographic retention behavior of alkylbenzenes, organic acids and anilines were investigated. The monolithic stationary phase exhibited reversed phase (RP) chromatographic behavior toward neutral solutes. The model organic acid anion solutes were separated by the mixed mode mechanism, which comprised RP interaction, weak anion-exchange, and electrophoresis. Basic compounds such as anilines) were well separated on the butylaminopropyl silica monolithic column without peak tailing.