色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
8期
798-803
,共6页
高效液相色谱%键合硅胶固定相%大黄素配体%色谱柱%制备%应用
高效液相色譜%鍵閤硅膠固定相%大黃素配體%色譜柱%製備%應用
고효액상색보%건합규효고정상%대황소배체%색보주%제비%응용
high performance liquid chromatography( HPLC)%bonded silica gel stationary phase%emodin ligand%chromatographic column%preparation%application
采用中间体法，先将大黄素配体与γ-[（2，3）-环氧丙氧]丙基三甲氧基硅烷（KH-560）偶联剂反应制备含配体的硅氧烷试剂，然后再与硅胶键合，最终制得大黄素键合硅胶液相色谱固定相（以下简称 ESP）。通过红外光谱、元素分析和热重分析表征固定相的结构。以萘作为溶质探针，甲醇-水（60：40，v / v）为流动相，流速为0.8 mL / min，测得 ESP 柱的柱效。采用传统的反相 C18和苯基柱作参比，将 ESP 应用于系列中性、碱性和酸性芳香族化合物以及实际样品风油精的分离分析，并探讨相关的色谱分离机理。结果表明，配体大黄素被成功地键合到球形硅胶表面，测得配体键合量为0.23 mmol / g，ESP 柱理论塔板数约为19874 N / m。ESP 的偶联剂链和蒽醌环提供了疏水性的结构基础，大黄素配体还能为溶质提供π-π或 p-π、电荷转移、氢键、偶极-偶极等作用点。多位点的协同作用使得 ESP 柱具有独特和优秀的色谱分离选择性，并且无需调节 pH 值，采用简单而廉价的甲醇-水流动相就能实现胺类、酚类等极性样品的基线分离，实验条件简单、方便。
採用中間體法，先將大黃素配體與γ-[（2，3）-環氧丙氧]丙基三甲氧基硅烷（KH-560）偶聯劑反應製備含配體的硅氧烷試劑，然後再與硅膠鍵閤，最終製得大黃素鍵閤硅膠液相色譜固定相（以下簡稱 ESP）。通過紅外光譜、元素分析和熱重分析錶徵固定相的結構。以萘作為溶質探針，甲醇-水（60：40，v / v）為流動相，流速為0.8 mL / min，測得 ESP 柱的柱效。採用傳統的反相 C18和苯基柱作參比，將 ESP 應用于繫列中性、堿性和痠性芳香族化閤物以及實際樣品風油精的分離分析，併探討相關的色譜分離機理。結果錶明，配體大黃素被成功地鍵閤到毬形硅膠錶麵，測得配體鍵閤量為0.23 mmol / g，ESP 柱理論塔闆數約為19874 N / m。ESP 的偶聯劑鏈和蒽醌環提供瞭疏水性的結構基礎，大黃素配體還能為溶質提供π-π或 p-π、電荷轉移、氫鍵、偶極-偶極等作用點。多位點的協同作用使得 ESP 柱具有獨特和優秀的色譜分離選擇性，併且無需調節 pH 值，採用簡單而廉價的甲醇-水流動相就能實現胺類、酚類等極性樣品的基線分離，實驗條件簡單、方便。
채용중간체법，선장대황소배체여γ-[（2，3）-배양병양]병기삼갑양기규완（KH-560）우련제반응제비함배체적규양완시제，연후재여규효건합，최종제득대황소건합규효액상색보고정상（이하간칭 ESP）。통과홍외광보、원소분석화열중분석표정고정상적결구。이내작위용질탐침，갑순-수（60：40，v / v）위류동상，류속위0.8 mL / min，측득 ESP 주적주효。채용전통적반상 C18화분기주작삼비，장 ESP 응용우계렬중성、감성화산성방향족화합물이급실제양품풍유정적분리분석，병탐토상관적색보분리궤리。결과표명，배체대황소피성공지건합도구형규효표면，측득배체건합량위0.23 mmol / g，ESP 주이론탑판수약위19874 N / m。ESP 적우련제련화은곤배제공료소수성적결구기출，대황소배체환능위용질제공π-π혹 p-π、전하전이、경건、우겁-우겁등작용점。다위점적협동작용사득 ESP 주구유독특화우수적색보분리선택성，병차무수조절 pH 치，채용간단이렴개적갑순-수류동상취능실현알류、분류등겁성양품적기선분리，실험조건간단、방편。
An emodin-bonded silica gel stationary phase( ESP)for high performance liquid chromatography has been synthesized by the intermediate method. The preparation process was as follows:γ-glycidoxypropyltrimethoxy silane( KH-560)firstly reacted with emodin ligand;then the intermediate was chemically immobilized to the surface of silica gel. Characterization of ESP was carried out with Fourier transform infrared spectroscopy ( FTIR ), elemental analysis and thermogravimetric analysis. Naphthalene was used as a probe to determine the col-umn efficiency with methanol-water(60 :40,v / v)as binary mobile phase at a flow rate of 0. 8 mL / min. In order to elucidate the related separation mechanism,ESP was used to separate a series of neutral,basic and acidic aromatic compounds,as well as a sample of wind medicated oil. The conventional C 18 column and phenyl column were also tested under the same chromato-graphic conditions for comparison. The results showed that the emodin ligand was successfully bonded to the surface of spherical silica gel with a 0. 23 mmol / g of bonded amount,and the theoretical plate number of ESP column was about 19 874 N / m. The coupling reagent chains and anthraquinone rings in ESP offered a structural basis for hydrophobic interaction. Mean-while,the emodin ligands provided π-π or p-π,charge transfer,hydrogen bonding,dipole-di-pole action sites for different analytes. The synergistic reaction of various action sites endowed ESP column special and excellent chromatographic separation selectivity. And a baseline sepa-ration of polar compounds such as amines and phenols on ESP was easily achieved by using common and cheap methanol-water mobile phases without buffer salts. The experimental condi-tions were simple and convenient.
