| 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 |
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| 引用本文： | 黄桂兰,李重九,黄修柱.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[J].分析化学,2006,34(3):407-410. |
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| 作者姓名： | 黄桂兰 李重九 黄修柱 |
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| 作者单位： | 中国农业大学理学院应用化学系,北京,100094;防化研究院第六研究所,北京,102205;中国农业大学理学院应用化学系,北京,100094;农业部农药检定所,北京,100026 |
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| 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。
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| 关 键 词： | 核磁共振 芳氧丙酸酯类除草剂 对映体纯度 手性镧系位移试剂 化学位移不等价 |
| 收稿时间： | 05 18 2005 12:00AM |
| 修稿时间： | 2005-05-182005-09-29 |
Chiral Lanthanide Shift Reagent-Nuclear Magnetic Resonance Method for Determination of Enantiomeric Purity of Arylphenoxypropionate Herbicides |
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| Huang Guilan,Li Chongjiu,Huang Xiuzhu.Chiral Lanthanide Shift Reagent-Nuclear Magnetic Resonance Method for Determination of Enantiomeric Purity of Arylphenoxypropionate Herbicides[J].Chinese Journal of Analytical Chemistry,2006,34(3):407-410. |
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| Authors: | Huang Guilan Li Chongjiu Huang Xiuzhu |
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| Institution: | 1.Department of Applied Chemistry, College of Applied Chemistry, China Agriculture University, Beijing 100094;2.The Sixth Research Center, Institnte of Chemical Defence, Beijing 102205;3.Institute for the Control Agrochemicals, Ministry of Agriculture, Beijing 100026 |
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| 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. |
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| Keywords: | Nuclear magnetic resonance arylphenoxypropionate herbicides enantiomeric purity chiral lanthanide shift reagent chemical shift non-equivalence |
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