羧基丁二酰-β-环糊精微球毛细管柱的制备及其应用于气相色谱
Preparation of Carboxy-Succinyl-β-Cyclodextrin Microspheres Capillary Column and Its Application to GC
摘 要
以采用文献方法合成的化合物羧基丁二酰-β-环糊精微球为固定相,通过溶胶-凝胶技术制备了毛细管气相色谱柱。用此毛细管柱分离了难以分开的2种氨基酸和3种手性药物对映体。对此分离柱的色谱参数进行了测定,5对对映体的分离因子在1.22~3.21之间,分离度在7.05~22.74之间。分离DL-甲硫氨酸的试验中,测得其分离因子的相对标准偏差(n=7)小于0.65%。所有数据表明,该色谱柱分离效果良好,适宜用于气相色谱分析。
毛细管色谱柱
氨基酸
手性药物
溶胶-凝胶
气相色谱法
对映体
Carboxy-succinyl-β-cyclodextrin microspheres
Capillary column
Amino acids
Chiral drugs
Sol-gel
GC
Enantiomer
Abstract
A capillary chromatographic column was prepared by using carboxy-succinyl-β-cyclodextrin microspheres as stationary phase and applying the sol-gel technique. This novel column was used in the separation of 2 amino acids and enantiomers of 3 chiral drugs which were very hard to separate. Several main parameters of this chromatographic column were determined and the following results were obtained: ① values of separation factor for 5 pairs of enantiomers were found in the range of 1.22-3.21, with resolution in the range of 7.05-22.74; ② relative standard deviation (n=7) of separation factor (β) of DL-methionine was found to be less than 0.65%. As a whole, this new column showed high efficiency in separation and was favorable to be used in GC analysis.
中图分类号 O657.7
所属栏目 工作简报
基金项目 黑龙江省自然科学基金资助项目(B201218)
收稿日期 2012/11/25
修改稿日期
网络出版日期
作者单位点击查看
联系人作者李英杰(lyj310@163.com)
备注李英杰(1961-),男,黑龙江齐齐哈尔人,教授,博士,研究方向为电色谱分析。
引用该论文: LI Ying-jie,DING Li,Lv Ren-jiang,ZHANG Fu-xiang,XU Ting-ting,WU Jing. Preparation of Carboxy-Succinyl-β-Cyclodextrin Microspheres Capillary Column and Its Application to GC[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2013, 49(12): 1458～1461
李英杰,丁莉,吕仁江,张福祥,徐婷婷,吴婧. 羧基丁二酰-β-环糊精微球毛细管柱的制备及其应用于气相色谱[J]. 理化检验－化学分册, 2013, 49(12): 1458～1461
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【2】ZHANG B, EDMUND T B, DAVID M G, et al. Singal-particle fritting technology for capillary electrochromatography［J］. Anal Chem, 2007,79:9229-9233．
【3】ANURAG S R, EMILY W, CSABA H. Electrosmotic mobility and conductivity in columns for capillary electrochromatography［J］. Anal Chem, 1999,71:2633-2641．
【4】VRATISLAV K, JOSEPH K, EDGAR A A. Capillary electrophoresis in bioanalysis［J］. Anal Chem, 2008,80:4533-4550．
【5】YUN Tian, CHENG Zhong, FU En-qin, et al. Novel-cyclodextrin derivative functionalized polymethacrylate-based monolithic columns for enantioselective separation of ibuprofen and naproxen enantiomers in capillary electrochromatography［J］. J Chromatography A, 2009(1216):1000-1007．
【6】CHEN Z, BILL B, CHANG H C. Open-tubular capillary electrochromatography-mass spectrometry with sheathless nanoflow electrosprayionization for analysis of amino acids and peptides［J］. Mass Spectrom, 2007,42:244-253．
【7】玛尔江·巴哈提别克,薛云云,王彦,等.应用加压毛细管电色谱技术检测鸡蛋中四环素类农兽药残留的研究［J］.中国抗生素杂志, 2011,7(36):536-539．
【8】曾玉香,王超,王炳强.手性固定相毛细管电色谱在手性药物分离中的应用研究进展［J］.理化检验-化学分册, 2009,45(4):485-490．
【9】LI Ying-jie, SONG Chun-hui, ZHANG Ling-yi, et al. Fabrication and evaluation of chiral monolithic column modified by β-cyclodextrin derivatives［J］. Talanta, 2010,80:1378-1384．
【10】ARAKI J, KATAOKAa T. New solvent for polyrotaxane.Dissolution of a poly(ethylene glycol)yclodextrin olyrotaxane in a calcium thiocyanate aqueous solution or N-methylmorpholine·Nde monohydrate［J］. J Appl Po Sci, 2007,105:2265-2270．
【11】MOHAMMED A G, SAFAA M E, KHALED F E. Preparation and utilization of ionic exchange resin via graft coplymerization of β-CD itaconate with chitosan［J］. Care Poly, 2004,56:387-396．
【12】GHEORGHE F, MARIETA C. Preparation and characterization of pH and temperature-sensitive pullulan microspheres for controlledrelease of drugs［J］. Biomaterials, 2008,29:2767-2775．
【13】刘林涛,张光华,黄怡,等.pH敏感性β-环糊精微球的制备及其吸附性能［J］.化工环保, 2009,29(6):559-562．
【14】施治国,冯钰铸,达世禄.溶胶-凝胶技术制备毛细管硅胶整体柱及其应用［J］.分析科学学报, 2003,19(6):503-506．
【15】ASIAIE R, HUANG X, FAMAN D, et al. Sintered octadecylsilica as monolithic column packing in capillary electrochromatography and micro high-performance liquid chromatogrphy［J］. J Chromatography A, 1998,806(2):251-263．
【16】李仲谨,杨威,王培霖.β-环糊精聚合物微球的合成与表征［J］.精细化工, 2010,27(7):692-695．
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