槲皮素是一种植物体中含量丰富、价格较便宜的黄酮类化合物,本研究以γ-[(2,3)-环氧丙氧]丙基三甲氧基硅烷(KH-560)为偶联剂,将其化学键合到硅胶上,得到一种含天然配体的槲皮素键合硅胶固定相(QUSP).采用红外光谱、热重分析、元素分析及固体核磁对其结构进行表征,测得硅胶表面槲皮素的键合量为0.139 mmol/g.采用不同结构的溶质作探针,在评价固定相反相液相色谱疏水作用性能的基础上,侧重研究新固定相对极性芳香族化合物的分离能力,探讨了新固定相的色谱分离机理.研究表明,仅采用甲醇或乙腈-水简单流动相,无需用缓冲液精确控制pH值,QUSP就能分别实现吡啶类、芳胺类、苯酚类、苯甲酸类和黄酮类等极性化合物的快速基线分离.QUSP键合的槲皮素除含疏水性的C6-C3-C6骨架外,黄酮环还能为溶质提供氢键、偶极、π-π、电荷转移等多种作用位点,各种协同作用有利于提高色谱分离选择性,尤其对极性的可离子化的酸性和碱性化合物.
参考文献
[1] | Snyder L R,Kirkland J J,Glajch J L.Practical HPLC Method Development,2nd Edition[M].Chichester,New York:John Wiley & Sons Inc,1997:1-20. |
[2] | Qiu H D,Liang X J,Sun M,et al.Development of Silica-based Stationary Phases for High-performance Liquid Chromatography[J].Anal Bioanal Chem,2011,399(10):3307-3322. |
[3] | Guillarme D,Russo R,Rudaz S,et al.Chromatographic Performance of Silica-Based Stationary Phases in High Temperature Liquid Chromatography:Pharmaceutical Applications[J].Curr Pharm Anal,2007,3 (4):221-229. |
[4] | McCalley D V.The Challenges of the Analysis of Basic Compounds by High Performance Liquid Chromatography:Some Possible Approaches for Improved Separations[J].J Chromatogr A,2010,1217 (6):858-880. |
[5] | Kirkland J J,Henderson J W.Reversed-Phase HPLC Selectivity and Retention Characteristics of Conformationally Different Bonded Alkyl Stationary Phases[J].J Chromatogr Sci,1994,32(11):473-480. |
[6] | Kirkland J J,Adams J B,Straten M A,et al.Bidentate Silane Stationary Phases for Reversed Phase High-performance Liquid Chromatography[J].Anal Chem,1998,70 (20):4344-4352. |
[7] | HUANG Xiaojia,WANG Junde,LIU Xueliang.Synthesis,Characterization and Evaluation of a Novel Double-amine Packing for Reversed-phase High Performance Liquid Chromatography[J].Chinese J Anal Chem,2002,30 (9):1048-1052(in Chinese).黄晓佳,王俊德,刘学良,等.双胺型键合固定相的制备及评价[J].分析化学,2002,30(9):1048-1052. |
[8] | HUANG Xiaojia,LIU Xueliang,WANG Junde,et al.Synthesis,Characterization and Evaluation of a Novel Ester-bonded for Reversed-phase HPLC[J].Chem J Chinese Univ,2002,23 (9):1684-1687 (in Chinese).黄晓佳,刘学良,王俊德,等.新型酯型反相高效液相色谱填料的制备、表征及性能评价[J].高等学校化学校化学学报,2002,23 (9):1684-1687. |
[9] | O'Gara J E,Alden B A,Walter T H.Simple Preparation of a Ca HPLC Stationary Phase with an Intemal Polar Functional Group[J].Anal Chem,1995,67(20):3809-3813. |
[10] | LI Laisheng,CHEN Xiongquan,YANG Hanrong,et al.Preparation and Characterization of a Baicalin-bonded Stationary Phase for High Performance Liquid Chromatography[J].Chinese J Anal Chem,2007,7 (9):1279-1284(in Chinese).李来生,陈雄泉,杨汉荣,等.黄芩苷键合硅胶固定相的制备和表征[J].分析化学,2007,7 (9):1279-1284. |
[11] | CHEN Huiming,LI Laisheng,MA Haiping,et al.Study on the Preparation of Emodin-bonded Silica Stationary Phase and Its Application in Separation of Nucleoside Bases by HPLC[J].Chinese J Anal Lab,2010,29 (3):14-18 (in Chinese).陈会明,李来生,马海萍.等.大黄素键合硅胶固定相的制备及其在核苷碱基药物分离中的研究[J].分析试验室,2010,29(3):14-18. |
[12] | LI Laisheng,YANG Hanrong,LUO Liping,et al.Preparation,Characterization and Bacteriostasis of Diallyl Trisulfidebonded Silica Gel[J].Chinese J Appl Chem,2007,24 (7):782-785 (in Chinese).李来生,杨汉荣,罗丽萍,等.二烯丙基三硫化物键合硅胶的制备、表征及抗菌作用[J].应用化学,2007,24(7):782-785. |
[13] | LIU Yanfang,QIN Li,ZHANG Da,et al.Progress of the Biological Activity of the Quercetin[J].lnt J Ophth,2009,9 (5):941-943 (in Chinese).刘彦芳,秦莉,张达,等.槲皮素的生物学活性研究进展[J].国际眼科杂志,2009,9(5):941-943. |
[14] | Li L S,Fang Y S,Chen H,et al.Preparation and Characterization of a New Quercetin-bonded Stationary Phase for High Performance Liquid Chromatography[J].Chin J Chem,2012,30(5):1144-1154. |
[15] | Marszall M P,Baczek T,Kaliszan R.Reduction of Silanophilic Interactions in Liquid Chromatography with the Use of Ionic Liquids[J].Anal Chim Acta,2005,547 (2):172-178. |
[16] | M erken H M,Beecher G R.Measurement of Food Flavonoids by High-performance Liquid Chromatography:a Riview[J].J Agric Food Chem,2000,48 (3):577-599. |
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