手性整体柱毛细管电色谱法拆分溴氰菊酯对映体
Resolution of Enantiomers of Deltamethrin by Capillary Electrochromatography Using Chiral Monolithic Column
摘 要
采用一步键合法制备了烯丙基-β-环糊精手性整体柱,将其作为毛细管分离柱,用毛细管电色谱法对溴氰菊酯的对映体进行手性拆分。在优化的试验条件下,乙腈与pH 6.5的5 mmol·L-1磷酸二氢钠溶液以体积比40比60组成的混合溶液作为流动相,运行电压为10 kV,毛细管柱温为20 ℃,溴氰菊酯的4对对映体在10 min内成功分离。
手性整体柱
对映体拆分
溴氰菊酯
Capillary electrochromatography
Chiral monolithic column
Resolution of enantiomers
Deltamethrin
Abstract
A method of capillary electrochromatography was proposed for the resolution of enantiomers of deltamethrin using allyl-β-cyclodextrin chiral monolithic capillary column as separation column, which was prepared by in-situ polymerization. A mixed solution of acetonitrile and 5 mmol·L-1 NaH2PO4 (of pH 6.5) solution (40+60 by vol.) was used as mobile phase. Separation voltage of 10 kV and capillary column temperature of 20℃ were chosen. Under the optimized conditions, 4 pairs of enantiomers of deltamethrin were successfully separated within 10 min.
中图分类号 O657.8
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收稿日期 2010/3/19
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备注李英杰(1961-),男,齐齐哈尔人,教授,主要从事色谱分析和光谱分析研究。
引用该论文: LI Ying-jie,LIANG Hui,ZHANG Chun-yu,HAO Xiu-ju,SONG Chun-hui. Resolution of Enantiomers of Deltamethrin by Capillary Electrochromatography Using Chiral Monolithic Column[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2011, 47(5): 547～549
李英杰,梁辉,张春雨,郝秀菊,宋春晖. 手性整体柱毛细管电色谱法拆分溴氰菊酯对映体[J]. 理化检验－化学分册, 2011, 47(5): 547～549
被引情况:
【1】卢亚玲,祝文君,艾明艳,刘文杰, "固相萃取-气相色谱-质谱法测定水果中9种菊酯农药残留量",理化检验－化学分册 51, 970-973(2015)
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参考文献
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【3】GUERROUACHE M, MAILLOT M C, CARBI-NEER B. Functionalization of macroporous organic polymer monolith based on succinimide ester reactivity for chiral capillary chromatography: a cyclodextrin click approach［J］. Macromolecular Rapid Communications, 2009,30(2):109-113.
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【5】YUN Tian, CHENG Zhong, FU En-qin, et al. Novel β-cyclodextrin derivative functionalized polymethacrylate-based monolithic columns for enantioselective separation of ibuprofen and naproxen enantiomers in capillary electrochromatography［J］. J Chromatogr A, 2009,1216(6):1000-1007.
【6】WANG Peng, JIANG Shu-ren, LIU Dong-hui, et al. Enantiomeric resolution of chiral pesticides by high-performance liquid chromatography［J］. Journal of Agriculture and Food Chemistry, 2006,54(5):1577-1583.
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【8】ARMSTRONG D W, TANG Y B, WARD T, et al. Derivatized cyclodextrins immobilized on fused-silica capillaries for enantiomeric separations via capillary electrophoresis, gas chromatography, or supercritical fluid chromatography［J］. Anal Chem, 1993,65:1114-1117.
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【11】CHAO Yan, SCHAUFELBERGER D, ERNI F. Electrochromatography and micro high-performance liquid chromatography with 320 μm I.D. packed columns［J］. J Chromatogr A, 1994,670:15-23.
【2】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.
【3】GUERROUACHE M, MAILLOT M C, CARBI-NEER B. Functionalization of macroporous organic polymer monolith based on succinimide ester reactivity for chiral capillary chromatography: a cyclodextrin click approach［J］. Macromolecular Rapid Communications, 2009,30(2):109-113.
【4】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, 2009,09,039.
【5】YUN Tian, CHENG Zhong, FU En-qin, et al. Novel β-cyclodextrin derivative functionalized polymethacrylate-based monolithic columns for enantioselective separation of ibuprofen and naproxen enantiomers in capillary electrochromatography［J］. J Chromatogr A, 2009,1216(6):1000-1007.
【6】WANG Peng, JIANG Shu-ren, LIU Dong-hui, et al. Enantiomeric resolution of chiral pesticides by high-performance liquid chromatography［J］. Journal of Agriculture and Food Chemistry, 2006,54(5):1577-1583.
【7】MAGUIRE R J. J. Agri. Chemical and photochemical isomerization of deltamethrin［J］. Food Chem, 1990,38(7):1613-1617.
【8】ARMSTRONG D W, TANG Y B, WARD T, et al. Derivatized cyclodextrins immobilized on fused-silica capillaries for enantiomeric separations via capillary electrophoresis, gas chromatography, or supercritical fluid chromatography［J］. Anal Chem, 1993,65:1114-1117.
【9】邹汉法,刘震,叶明亮,等.毛细管电色谱及其应用［M］.北京:科学出版社, 2001:133-137.
【10】BOUGHTFLOWER R J, UNDERWOOD T, PATERSON C. Several authors have also described the difficulties associated with reproducibly fabricating frits for retaining packing material in conventional capillaries［J］. J Chromatographia, 1995,40:329-335.
【11】CHAO Yan, SCHAUFELBERGER D, ERNI F. Electrochromatography and micro high-performance liquid chromatography with 320 μm I.D. packed columns［J］. J Chromatogr A, 1994,670:15-23.
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