›› 2011, Vol. 23 ›› Issue (5): 0-936.

• 植物保护 •    

新型直链淀粉手性固定相拆分戊唑醇对映体

王雪松1,2, 赵长山2, 章虎1, 何付丽2, 王祥云1, 徐浩1, 王新全1,*
  

  1. 1浙江省植物有害生物防控重点实验室—省部共建国家重点实验室培育基地,浙江省农业科学院 农产品质量标准研究所,浙江 杭州 310021;2东北农业大学 农学院,黑龙江 哈尔滨 150030
  • 收稿日期:1900-01-01 修回日期:1900-01-01 出版日期:2011-09-25 发布日期:2011-09-25

Enantiomeric separation of tebuconazole by new type of amylose chiral stationary phase

WANG Xue-song;ZHAO Chang-shan;ZHANG Hu;HE Fu-li;WANG Xiang-yun;XU Hao;WANG Xin-quan;*   

  1. 1State Key Laboratory Breeding Base for Zhejiang Sustainable Pest and Disease Control, Institute of Quality and Standard on Agricultural Products, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China;2College of Agriculture, Northeast Agricultural University, Harbin 150030, China
  • Received:1900-01-01 Revised:1900-01-01 Online:2011-09-25 Published:2011-09-25

摘要: 采用新型直链淀粉-三(5-氯-2-甲基苯基氨基甲酸酯)涂敷型手性固定相在反相色谱条件下拆分戊唑醇对映体,评价了流动相组成(甲醇/水,乙腈/水)及柱温(5~45℃)对对映体分离的影响。结果表明:以甲醇/水为流动相时,在甲醇含量100%至40%范围内,戊唑醇对映体均无分离趋势;而用乙腈/水为流动相时,在乙腈含量100%至40%范围内,戊唑醇对映体均可实现基线分离;在5~45℃,V(乙腈)∶V(水)=1∶1,对映体的保留因子(k)与分离因子(α)随温度升高而降低,分离度(RS)却先升后降,基于线性Van't Hoff曲线的热力学参数证明戊唑醇对映体的分离受焓驱动。

关键词: 戊唑醇对映体, 反相色谱, 手性拆分

Abstract: The separation of tebuconazole enantiomers was performed by high-performance liquid chromatography (HPLC) on the amylose-tris (5-chlorine-dimethy-phenylcarbamate) chiral stationary phase using reverse phase mode. The effects of different mobile phase compositions (methanol/water, acetonitrile/water) and column temperature (5-45℃) on the chiral separation were investigated. The results showed that tebuconazole enantiomers did not separate using methanol/water as mobile phase with the content of methanol ranging from 100% to 40%. In contrast, baseline separation of enantiomers was achieved using acetonitrile/water as mobile phase with the content of acetonitrile ranging from 100% to 40%. The retention factors (k) and selectivity factor (α) decreased when the temperature increased from 5℃ to 45℃, while the resolution (RS) of enantiomers first increased and then decreased within the same range of temperature (acetonitrile/water,50/50, V/V). Thermodynamical parameters illustrated that separation of tebuconazole enantiomers was driven by enthalpy.

Key words: tebuconazole enantiomers, reverse phase chromatography, chiral separation