欢迎登录材料期刊网

材料期刊网

高级检索

采用固液相表面连续反应法,先将偶联剂γ-[(2,3)-环氧丙氧]丙基三甲氧基硅烷(KH-560)键合到球形硅胶表面,然后再将植物有效成分丁香酚与硅胶上的 KH-560活性基团反应,合成了丁香酚键合硅胶液相色谱固定相( EGSP)。采用元素分析、热重分析和红外光谱对该固定相的结构进行了表征。以萘作为溶质探针,乙腈-水(35:65,v/v)为流动相,流速为0.8 mL/min,测得 EGSP柱的柱效。以一系列的中性、碱性和酸性化合物为溶质探针, C18柱和苯基柱作参比,对该固定相的色谱性能及保留机理进行了研究。结果表明,硅胶表面成功键合上了丁香酚配体,键合量为0.28 mmol/g,EGSP柱理论塔板数约为24707 N/m。该固定相不仅具有良好的反相色谱性能,同时由于配体结构中含有芳环、烯基和甲氧基,还能与溶质发生π-π电荷转移、偶极-偶极和氢键作用。与传统的反相 C18柱和苯基柱相比,EGSP在极性芳香族化合物的快速、简便分离中占优势。

A eugenol-bonded silica gel stationary phase( EGSP ) for high performance liquid chromatography( HPLC)has been synthesized by the solid-liquid successive reaction method. The preparation process included two steps:firstly,γ-glycidoxypropyltrimethoxy-silane( KH-560)was covalently attached to the surface of spherical silica gel. Then the bonded silica gel continued to react with eugenol ligand,which was a plant active component,and obtained EGSP. The structure of EGSP was characterized by elemental analysis,thermogravimetric anal-ysis and Fourier transform infrared spectroscopy. Using naphthalene as a probe,the column efficiency was tested under the mobile phase of acetonitrile-water(35:65,v/v)at a flow rate of 0. 8 mL/min. The chromatographic properties and the retention mechanism of EGSP were evaluated by using neutral,basic and acidic analytes as solute probes. Meanwhile,the compar-ative study with C18 column and phenyl column was also carried out under the same chromato-graphic conditions. The result showed that the eugenol ligand was successfully bonded to the surface of silica gel with a 0. 28 mmol/g of bonded amount,and the theoretical plate number of EGSP column was about 24 707 N/m. The EGSP appeared to be a kind of excellent reversed-phase stationary phase with suitable hydrophobicity and various synergistic sites. The eugenol ligand bonded on silica gel could first provide π-π interaction sites for different analytes because of its benzene ring and alkenyl. In addition,the methoxy groups of eugenol were re-sponsible for dipole-dipole and hydrogen-bonding interactions between the ligand and solutes in the effective separation process. Comparing with traditional C 18 column and phenyl column,EGSP has an advantage in the fast separation of polar compounds under simple experimental conditions.

参考文献

[1] 于世林.高效液相色谱方法及应用[M].北京:化学工业出版社,2000:8.
[2] Mullangi,R.;Sharma,K.;Srinivas,N.R..Review of HPLC methods and HPLC methods with mass spectrometric detection for direct determination of aspirin with its metabolite(s) in various biological matrices[J].Biomedical Chromatography: An International Journal Devoted to Research in Chromatographic Methodologies and Their Applications in the Biosciences,20128(8):906-941.
[3] Jardim, I.C.S.F.;Maldaner, L.;Lourenco, J.;Fioravanti, L.M.A.;Collins, C.H..Some new selective stationary phases for RP-HPLC[J].Journal of separation science,201019(19):2917-2929.
[4] Qiu H D;Liang X J;Sun M.[J].Anal Bioanal Chem,2011399(10):3307.
[5] Beesley T E.[J].LC GC Eur,201124(5):270.
[6] Ward T J;Ward K D.[J].Anal Chem,201284(2):626.
[7] Xiao, Y.;Ng, S.-C.;Tan, T.T.Y.;Wang, Y..Recent development of cyclodextrin chiral stationary phases and their applications in chromatography[J].Journal of chromatography. A,2012:52-68.
[8] 朱元棋;徐晓冬;冯四伟;常秀娟;邱蕾蕾.大分子键合型手性固定相的研究进展[J].高分子通报,2012(6):92-97.
[9] 雷雯;张凌怡;朱亚仙;杜一平;张维冰.以戊二醛为间隔臂的万古霉素键合手性固定相制备[J].分析化学,2010(11):1544-1549.
[10] 沈爱金;郭志谋;梁鑫淼.亲水作用色谱固定相的发展及应用[J].化学进展,2014(1):10-18.
[11] Kotoni, D.;D'Acquarica, I.;Ciogli, A.;Villani, C.;Capitani, D.;Gasparrini, F..Design and evaluation of hydrolytically stable bidentate urea-type stationary phases for hydrophilic interaction chromatography[J].Journal of chromatography, A: Including electrophoresis and other separation methods,2012:196-211.
[12] 刘士佳;乔晓强;杨艳军;闫宏远.新型咪唑嵌合氨基亲水作用色谱固定相的制备及其色谱性能[J].色谱,2014(10):1079-1083.
[13] Shen A J;Guo Z M;Yu L.[J].Chem Commun,201147(15):4550.
[14] Shen A J;Li X L;Dong X F.[J].J Chromatogr A,20131314:63.
[15] 方奕珊;李来生;陈红;张杨.高效液相色谱槲皮素键合硅胶固定相分离极性化合物[J].应用化学,2013(1):79-87.
[16] 张杨;刘妙芬;方奕姗;李来生.靛红键合固定相分离黄酮类化合物[J].南昌大学学报(理科版),2012(3):228-232.
[17] 宋小妹;唐志书.中药化学成分提取分离与制备[M].北京:人民卫生出版社,2009:62.
[18] 彭宅彪;张琼光;代虹健;丁英平.丁香酚的药理学研究进展[J].时珍国医国药,2006(10):2079-2081.
[19] Marszall M P;Baczek T;Kaliszan R.[J].Anal Chim Acta,2005547(2):172.
上一张 下一张
上一张 下一张
计量
  • 下载量()
  • 访问量()
文章评分
  • 您的评分:
  • 1
    0%
  • 2
    0%
  • 3
    0%
  • 4
    0%
  • 5
    0%