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手性镧系位移试剂核磁共振法测定芳氧丙酸酯类除草剂对映体纯度

Chiral Lanthanide Shift Reagent-Nuclear Magnetic Resonance Method for Determination of Enantiomeric Purity of Arylphenoxypropionate Herbicides

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【作者】 黄桂兰李重九黄修柱

【Author】 Huang Guilan~ 1,2 , Li Chongjiu~ *1 , Huang Xiuzhu~3 ~1(Department of Applied Chemistry, College of Applied Chemistry, China Agriculture University, Beijing 100094) ~2(The Sixth Research Center, Institute of Chemical Defence, Beijing 102205) ~3(Institute for the Control Agrochemicals, Ministry of Agriculture, Beijing 100026)

【机构】 中国农业大学理学院应用化学系农业部农药检定所 北京100094防化研究院第六研究所北京102205北京100094北京100026

【摘要】 以Eu(hfc)3和Pr(hfc)3为手性镧系位移试剂(CLSR),比较了两种CLSR对2,4-滴丙酸甲酯的1HNMR和13C NMR谱手性分离效果,结果表明:Pr(hfc)3比Eu(hfc)3对手性中心相连的甲基具有更好的手性分离效果。首次应用Pr(hfc)3测定了盖草能、稳杀得和喹禾灵3种手性芳氧丙酸酯类除草剂的1HNMR和13CNMR谱,其1HNMR谱分离度R约为1,盖草能和喹禾灵的13C NMR谱分离度R大于1.5,说明1H NMR和13CNMR谱手性分离效果适用于对映体纯度测定。与手性色谱法相比,CLSR-NMR法测定对映体纯度具有操作简便、分析速度快的显著优势。

【Abstract】 The chemical shift non-equivalence in 1H and 13 C nuclear magnetic resonance (NMR) of dichlorprop-methyl were compared by using Eu-heptafluorohydroxy-methylene-d-camphorato (hfc)3 and Pr(hfc)3 as chiral lanthanide shift reagents (CLSR), it showed that Pr(hfc)3 was more effective than Eu(hfc)3. Pr(hfc)3 was used as firstly in detecting the chemical shift non-equivalence of 1H and 13 C NMR of three arylphenoxypropionate herbicides, quizalofop-ethyl, halxoyfop-etotyl and fluazifop-butyl. The result showed that the chiral resolutions of 1H NMR of three herbicides were about 1, and the chiral resolutions of 13 C NMR of quizalofop-ethyl and halxoyfop-etotyl were more than 1.5. That means the chiral resolutions of 1H NMR and 13 C NMR are fit for determining the enantiomeric purity. CLSR-NMR method is simpler and faster than chiral chromatographic method in the determination of the enantiomeric purity.

  • 【文献出处】 分析化学 ,Chinese Journal of Analytical Chemistry , 编辑部邮箱 ,2006年03期
  • 【分类号】TQ450.2
  • 【被引频次】2
  • 【下载频次】246
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