摘要
合成了氟铃脲农药粗品,通过活性炭吸附、重结晶进行初步纯化;然后采用柱层析分离技术,以硅胶为填料,乙酸乙酯/石油醚(30～60℃)(1:3,V/V)为展开剂(Rf≈0.5)进行提纯.用紫外光谱(UV)、红外光谱(IR)、核磁共振(1H NMR,13C NMR)及质谱(MS)进行了结构表征;以高效液相色谱法测得该试样纯度在99%以上.
Hexailumumron as the starting material was synthesized, and then was preliminarily purified by adsorption with active carbon, and re-crystallation in sequence. The further purification was carried out by passing through a chromatographic column with silica gel as the fixed phase and ethyl acetate/ petroleum ether（boiling point 30～60℃） at a ratio of one to three as the mobile phase （Rf≈0.5）. The purified hexaflumumron was characterized by MDS, EAS, UV, IR, ^1H NMR, ^13 CNMR and MS. The purity of the pesticide as CRM was determined to be over 99 % by HPLC.
出处
《分析科学学报》
CAS
CSCD
2005年第6期630-632,共3页
Journal of Analytical Science
基金
制
修订国家标准计划项目(B094-98)
关键词
氟铃脲
标准样品
合成
纯化
表征
Hexaflumumron
Certified reference material（CRM）
Synthesis
Purification
Characterization
