新型直链淀粉手性固定相拆分戊唑醇对映体  被引量:1

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

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作  者: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] 

机构地区:[1]浙江省植物有害生物防控重点实验室一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

出  处:《浙江农业学报》2011年第5期932-936,共5页Acta Agriculturae Zhejiangensis

基  金:国家自然科学基金(20807038);浙江省农业科学院科技创新提升工程资助项目(2007R19Y01E02);浙江省重大项目(2007C02002)

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N/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(☆)与分离因子(OL)随温度升高而降低,分离度(R。)却先升后降,基于线性Van’tHoff曲线的热力学参数证明戊唑醇对映体的分离受焓驱动。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 acetoni- trile ranging from 100% to 40%. The retention factors (k) and selectivity factor (a) decreased when the tempera- ture 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.

关 键 词:戊唑醇对映体 反相色谱 手性拆分 

分 类 号:TQ450.7[化学工程—农药化工]

 

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