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拟除虫菊酯类农药在超临界流体色谱中的对映体分离 被引量:6

Enantiomer Separation of Synthetic Pyrethroids by Supercritical Fluid Chromatography
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摘要 [目的]获得单一对映体对于低毒高效的农药生产和环境安全具有重要意义。[方法]使用超临界CO2色谱,对6种拟除虫菊酯类农药在Sino-Chiral OJ柱上进行对映体分离研究,考察了改性剂种类(甲醇、乙醇和异丙醇)及体积分数(1%、3%、5%)对其分离的影响。[结果]高效氯氟氰菊酯在3种改性剂条件下都得到了基线分离;氯菊酯只在甲醇作为改性剂时得到分离;氰戊菊酯只在3%乙醇改性条件下实现部分分离;氯氰菊酯在乙醇作为改性剂时取得了最优分离,得到8个异构体中的7个出峰;联苯菊酯和溴氰菊酯均只得到2个对映体出峰。[结论]在手性分离过程中,对映体与手性固定相之间的偶极-偶极和π-π作用对菊酯类农药的分离起较大作用,同时卤素取代基的电负性大小对分离也有较大影响。 To obtain the pure-enantiomer of chiral pesticides is meaningful for researching their stereoselectivity of pesticidal activity and toxicity to environmental fate.[Methods] The enantiomer separation of synthetic pyrethroids was conducted on Sino-Chiral OJ by supercritical fluid chromatography(SFC).The influence of the type and concentration of organic modifier in mobile phase was studied.[Results] Lambda-cyhalothrin could be separated with 1-5% methanol,ethanol or isopropanol in supercritical CO2.Permethrin could be separated only when methanol was added in mobile phase,while fenvalerate achieved partially resolution as the mobile phase containing 3% ethanol.7 chromatographic peaks of cypermethrin were obtained by adding ethanol as modifier.2 chromatographic peaks of bifenthrin and deltamethrin were obtained.[Conclusions] The dipolar-dipolar interaction and π-π interaction between chiral stationary phase and pesticides could be in favour of the enantioseparation of pyrethroids.Meanwhile,the electronegativity of halogen substituent has an effect on separation.
出处 《农药》 CAS 北大核心 2011年第7期492-494,497,共4页 Agrochemicals
基金 浙江省自然科学基金项目(Y506264)
关键词 拟除虫菊酯 超临界色谱 对映体分离 Sino-ChiralOJ柱 synthetic pyrethroids supercritical fluid chromatography enantiomeric separation Sino-Chiral OJ
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