色谱
色譜
색보
Chinese Journal of Chromatography
2015年
9期
910-916
,共7页
用天%吴凡%肖红斌%万伯顺
用天%吳凡%肖紅斌%萬伯順
용천%오범%초홍빈%만백순
亲水作用色谱%固定相%糖醇%糖基%选择性
親水作用色譜%固定相%糖醇%糖基%選擇性
친수작용색보%고정상%당순%당기%선택성
hydrophilic interaction liquid chromatography ( HILIC )%stationary phases%sugar alcohol%glycosyl group%selectivity
利用-NCO和-OH的加成反应,通过简单的两步反应将木糖醇和麦芽糖醇成功地键合于硅胶表面,制备了两种新型糖醇类亲水作用色谱固定相。流动相中乙腈含量对保留的影响曲线表明,这两种糖醇固定相具有典型的亲水作用色谱固定相性质,对极性和亲水性化合物有很强的保留作用。利用这两种固定相成功分离了水溶性维生素、水杨酸及其类似物、碱基及其相应的核苷和淫羊藿苷类似物等模型混合物,同时糖醇固定相展现了新颖的选择性,特别是相对于线形的木糖醇键合固定相,非线形的麦芽糖醇键合固定相表现出了对糖基的独特保留能力。此外,缓冲盐的pH和浓度对保留的影响表明静电作用在这两种糖醇固定相的保留机理中也发挥着一定的作用。本文所发展的糖醇类固定相具有良好的分离性能,有望在亲水作用色谱分离领域发挥潜在的应用价值。
利用-NCO和-OH的加成反應,通過簡單的兩步反應將木糖醇和麥芽糖醇成功地鍵閤于硅膠錶麵,製備瞭兩種新型糖醇類親水作用色譜固定相。流動相中乙腈含量對保留的影響麯線錶明,這兩種糖醇固定相具有典型的親水作用色譜固定相性質,對極性和親水性化閤物有很彊的保留作用。利用這兩種固定相成功分離瞭水溶性維生素、水楊痠及其類似物、堿基及其相應的覈苷和淫羊藿苷類似物等模型混閤物,同時糖醇固定相展現瞭新穎的選擇性,特彆是相對于線形的木糖醇鍵閤固定相,非線形的麥芽糖醇鍵閤固定相錶現齣瞭對糖基的獨特保留能力。此外,緩遲鹽的pH和濃度對保留的影響錶明靜電作用在這兩種糖醇固定相的保留機理中也髮揮著一定的作用。本文所髮展的糖醇類固定相具有良好的分離性能,有望在親水作用色譜分離領域髮揮潛在的應用價值。
이용-NCO화-OH적가성반응,통과간단적량보반응장목당순화맥아당순성공지건합우규효표면,제비료량충신형당순류친수작용색보고정상。류동상중을정함량대보류적영향곡선표명,저량충당순고정상구유전형적친수작용색보고정상성질,대겁성화친수성화합물유흔강적보류작용。이용저량충고정상성공분리료수용성유생소、수양산급기유사물、감기급기상응적핵감화음양곽감유사물등모형혼합물,동시당순고정상전현료신영적선택성,특별시상대우선형적목당순건합고정상,비선형적맥아당순건합고정상표현출료대당기적독특보류능력。차외,완충염적pH화농도대보류적영향표명정전작용재저량충당순고정상적보류궤리중야발휘착일정적작용。본문소발전적당순류고정상구유량호적분리성능,유망재친수작용색보분리영역발휘잠재적응용개치。
New types of stationary phases for hydrophilic interaction liquid chromatography ( HILIC ) with unique selectivity are very important for the separation of various polar and hydrophilic analytes. Two novel HILIC stationary phases based on sugar alcohol modified silica were synthesized by a simple two?step reaction in which xylitol and maltitol were bonded onto the surface of silica particles via the addition reaction between -NCO and -OH. The effect of acetonitrile content on the retention indicated that the two stationary phases were of typical HILIC character and exhibited strong retention for polar and hydrophilic analytes. They succee?ded in the separation of a wide range of polar and hydrophilic analytes including water soluble vitamins, salicylic acid and its analogues, nucleic acid bases and nucleosides, and icariin and its analogues with unique selectivity. Especially, the maltitol stationary phase showed unique selectivity on glycosyl group, compared to xylitol stationary phase. Furthermore, the effects of buffer pH as well as salt concentration on the retention indicated that electrostatic interaction played an important role in the separation mechanism of the two stationary phases. For sure, the efficient stationary phases are of great potential applications in HILIC.