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药物对映体含量测定的核磁共振法研究Ⅰ.非洛地平

Study of NMR Methods for Stereoisomeric Determination of PharmaceuticalsⅠ. Felodipine

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【作者】 沈文斌王庆锋廖海平

【Author】 Shen Wenbin; Wang Qingfeng and Liao Haiping (Physical & Chemical Test Center of Jiangsu Province 210002)

【机构】 江苏省理化测试中心

【摘要】 本文报道了在位移试剂Eu(FOD)3、Eu(TFC)3和Eu(HFC)3存在下非洛地平质子信号的镧诱导位移(LIS)值,非洛地平的芳氢质子信号得到简化并解析;在手性位移试剂Eu(HFC)3存在下,观察到甲酯的甲基明显的对映体位移差值(△△δ),据此,可对非洛地平直接进行对映体的含量分析。当Eu(HFC)3:非洛地平为0.620(摩尔比)时,甲酯甲基的R和S对映体两峰的峰谷高度为峰高的3.8%,即当对映体之一的含量不低于3.8%时,可对非洛地平的对映体含量进行精确的直接测定。

【Abstract】 The 90MHz 1H NMR spectra of racemic felodipine [4-(2, 3-dichlorophenyl)-1, 4-dihydro-2, 6-dimethyl-3, 5-pyridinedicarboxylic acid, ethyl methyl ester), have been studied with the achiral shift reagent, Eu (FOD)3, Ⅰ, and the chiral shift reagent, Eu (TFC)3, Ⅱ, and Eu (HFC)3, Ⅲ. Substantial Lanthanide-Induced Shifts (LIS) were seen for the proton signals of FLDP withⅠ andⅢ, and the aromatic proton signals were simplified. Appreciable enantiomeric shift differences (△△δ) were seen for methyl signal of -COOCH3 usingⅢ that should permit direct determination of enantiomeric excess for samples of FLDP. As little as 3. 8% of a minor enantiomer should be readily detectable.

  • 【文献出处】 药物分析杂志 ,CHINESE JOURNAL OF PHARMACEUTICAL ANALYSIS , 编辑部邮箱 ,1996年04期
  • 【分类号】R917
  • 【被引频次】10
  • 【下载频次】200
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