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蒋孟虹, 于小波, 毛黎顺, 沈文斌, 狄斌. 核磁共振法测定10-O-(N,N-二甲氨基乙基)-银杏内酯B甲磺酸盐标准物质的含量[J]. 中国药科大学学报, 2013, 44(4): 339-342. DOI: 10.11665/j.issn.1000-5048.20130410
引用本文: 蒋孟虹, 于小波, 毛黎顺, 沈文斌, 狄斌. 核磁共振法测定10-O-(N,N-二甲氨基乙基)-银杏内酯B甲磺酸盐标准物质的含量[J]. 中国药科大学学报, 2013, 44(4): 339-342. DOI: 10.11665/j.issn.1000-5048.20130410
JIANG Menghong, YU Xiaobo, MAO Lishun, SHEN Wenbin, DI Bin. Quantitative determination of 10-O-(N, N-dimethylaminoethyl)-ginkgolide B methanesulfonate by nuclear magnetic resonance[J]. Journal of China Pharmaceutical University, 2013, 44(4): 339-342. DOI: 10.11665/j.issn.1000-5048.20130410
Citation: JIANG Menghong, YU Xiaobo, MAO Lishun, SHEN Wenbin, DI Bin. Quantitative determination of 10-O-(N, N-dimethylaminoethyl)-ginkgolide B methanesulfonate by nuclear magnetic resonance[J]. Journal of China Pharmaceutical University, 2013, 44(4): 339-342. DOI: 10.11665/j.issn.1000-5048.20130410

核磁共振法测定10-O-(N,N-二甲氨基乙基)-银杏内酯B甲磺酸盐标准物质的含量

Quantitative determination of 10-O-(N, N-dimethylaminoethyl)-ginkgolide B methanesulfonate by nuclear magnetic resonance

  • 摘要: 建立核磁共振氢谱法测定10-O-(N,N-二甲氨基乙基)-银杏内酯B甲磺酸盐(XQ-1H)标准物质的含量。以齐多夫定为内标,DMSO-d6-D2O(5∶1)为溶剂,氢谱测定条件为:脉冲宽度30°,延迟时间20 s,采样次数32次,窗函数0.3 Hz。在此条件下,样品与内标的定量峰分离良好,线性范围宽,含量测定结果为99.12%,RSD为0.16%。该方法专属、准确,简便、快速,适用于对药物基准物质绝对含量的测定。

     

    Abstract: A new method was established to determine the content of 10-O-(N, N-dimethylaminoethyl)-ginkgolide B methanesulfonate by 1H NMR using DMSO-d6-D2O(5 ∶1)as the solvent and zidovudine as the internal standard. Experimental parameters of NMR were extensively investigated. Under the optimal condition, the sample and internal standard showed good separation and linearity. The content of 10-O-(N, N-dimethylaminoethyl)-ginkgolide B methanesulfonate was 99. 12% and its RSD was 0. 16%. This method is specificity, accurate, simple and rapid, and is suitable for the quantitative determination of the content of the reference substance content.

     

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