C18反相色谱固定相的制备及性能评价
Preparation and Performance Evaluation of C18 Stationary Phase for Reversed-Phase Chromatography
摘 要
以粒径10 μm硅胶为基质,与1,6-六亚甲基二异氰酸酯和十二醇反应制得新型C18反相色谱固定相。热失重结果表明,所制得的固定相在200 ℃以内热稳定性良好。扫描电镜结果表明:硅胶在改性前后没有损坏,颗粒完整,适合于色谱柱的填装。该固定相对联苯的静态吸附在4 h时达到平衡,吸附行为符合Langmuir吸附等温式。用芳香烃和极性化合物对固定相的分离性能进行评价,结果表明所合成的固定相具有良好的色谱性能。
硅胶
Langmuir吸附
C18 stationary phase for reversed-phase chromatography
Silica gel
Langmuir adsorption
Abstract
Novel C18 stationary phase for reversed-phase chromatography was prepared through the reaction of 1,6-diisocyanatocyclohexane and dodecanol with silica gel ( 10 μm) as matrix. It was shown by the result of thermogravimetry, the stationary phase behaved to have good thermal stability below 200 ℃. As shown by the result of SEM, the silica gel was kept undamaged before and after denaturing and was suitable for packing into the chromatographic column. It was found that the static adsorption of biphenyl on the stationary phase attained to equilibrium after 4 h. The adsorption behavior of the stationary phase was found to conform with the Langmuir isotherm. The separation capability of the stationary phase was evaluated by using aromatic and polar compounds as sample. It was shown that the stationary phase displayed good chromatographic properties.
中图分类号 O65 DOI 10.11973/lhjy-hx201604001
所属栏目 试验与研究
基金项目 江苏省自然科学基金(BK20141163);烟草行业卷烟 烟气重点实验室开放研究基金(SZBCW201300555)
收稿日期 2015/4/1
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备注张培培(1987-),女,江苏徐州人,硕士研究生,主要 从事新型色谱分离材料的研究。
引用该论文: ZHANG Pei-pei,ZHUANG Wei,CHEN Qiang,WU Shun,HAO Wei-qiang. Preparation and Performance Evaluation of C18 Stationary Phase for Reversed-Phase Chromatography[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2016, 52(4): 373～377
张培培,庄 韦,陈 强,吴 顺,郝卫强. C18反相色谱固定相的制备及性能评价[J]. 理化检验－化学分册, 2016, 52(4): 373～377
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参考文献
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【15】李来生,陈红,马海萍,等.厚朴酚键合硅胶液相色谱固定相的制备、表征与性能评价［J］.高等学校化学学报, 2012,33(4):707-713.
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【2】蒋生祥,刘霞.硅胶基质高效液相色谱固定相［J］.色谱, 2007,25(2):163-173.
【3】ZHAI C, LU Q, CHEN X, et al. Molecularly imprinted layer coated silica nanoparticles toward highly selective separation of active diosgenin from dioscorea nipponica makino［J］. J Chromatogr A, 2009,1216(12):2254-2262.
【4】雷毅,黄艳婷,罗卓雅.高效液相色谱法测定壮阳保健品中4种硫代西地那非类药物［J］.理化检验-化学分册, 2014,50(5):530-535.
【5】张剑,罗进,耿萌辉,等.反相高效液相色谱法同时测定壮阳类保健品中达泊西汀和4种PDE5抑制剂［J］.理化检验-化学分册, 2014,50(3):323-326.
【6】夏海涛,刘玉芬,李咏梅.高效液相色谱法分析红景天根中红景天甙［J］.理化检验-化学分册, 2006,42(6):490-491.
【7】HEMSTROM P, IRGUM K. Hydrophilic interaction chromatography［J］. J Sep Sci, 2006,29(12):1784-1821.
【8】杨新立,王俊德,熊博晖.高效液相色谱用硅质填料的进展［J］.色谱, 2000,18(4):308-312.
【9】王利娟,杨更亮,李煦,等.酯型十八烷基键合硅胶整体柱的制备、表征及性能评价［J］.色谱, 2005,23(5):504-507.
【10】KIRKLAND J J, ADAMS J B, VAN STRATEN M A, et al. Bidentate silane stationary phases for reversed-phase high-performance liquid chromatography［J］. Anal Chem, 1998,70(2):4344-4352.
【11】WIRTH M J, FATUNMBI H O. Horizontal polymerization of mixed trifunctional silanes on silica: a potential chromatographic stationary phase［J］. Anal Chem, 1992,64(22):2783-2786.
【12】WIRTH M J, FATUNMBI H O. Horizontal polymerization of mixed trifunctional silanes on silica. 2. Application to chromatographic silica gel［J］. Anal Chem, 1993,65(6):822-826.
【13】FAIRBANK R W P, XIANG Y, WIRTH M J. Use of methyl spacers in a mixed horizontally polymerized stationary phase［J］. Anal Chem, 1995,67(21):3879-3885.
【14】黄晓佳,刘莺,丛润滋,等.用于碱性物质分离的酰胺型反相色谱键合相的制备及评价［J］.色谱, 2001,19(4):293-296.
【15】李来生,陈红,马海萍,等.厚朴酚键合硅胶液相色谱固定相的制备、表征与性能评价［J］.高等学校化学学报, 2012,33(4):707-713.
【16】NEUE U D, ALDEN B A, WALTER T H. Universal procedure for the assessment of the reproducibility and the classification of silica-based reversed-phase packings-II. Classification of reversed-phase packings［J］. J Chromatogr A, 1999,849(1):101-116.
【17】LANGMUIR I. The constitution and fundamental properties of solids and liquids. Part I. Solids［J］. J Am Chem Soc, 1916,38(11):2221-2295.
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