Quantitative analysis of bilobalide and ginkgolides from Ginkgo biloba leaves and ginkgo products using 1H-NMR
Quantitative analysis of bilobalide and ginkgolides from Ginkgo biloba leaves and ginkgo products using 1H-NMR
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DOI：
10.1248/cpb.51.158
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发表时间：
2003-02-01
影响因子：
1.7
通讯作者：
Verpoorte, R
中科院分区：
文献类型：
--
作者：
Choi, YH;Choi, HK;Verpoorte, R
采用1H-1-NMR光谱法对银杏叶及6种商品银杏产品中的银杏内酯、银杏内酯A、B、C进行了定量分析。通过分析每个单重态H-12进行实验，其在H-1-NMR谱中在36.0 -7.0范围内分离良好。然而，白果内酯和银杏内酯的H-12质子可能与银杏黄酮的H-6或H-8质子重叠。因此，通过评价溶剂对化合物中这些信号的分辨率的影响，选择了用于化合物分析的最佳H-1-NMR溶剂。丙酮-d（6）-苯-d（6）（50：50）是最好的溶剂。通过每种化合物的强度与已知量的内标物（25 μ g/ml）间苯三酚的相对比率计算化合物的量。该方法可以在5分钟内快速简单地定量未衍生化的白果内酯和银杏内酯，无需任何预纯化步骤。
H-1-NMR spectrometry was applied to the quantitative analysis of the bilobalide, ginkgolides A, B, and C in Ginkgo biloba leaves and six kinds of commercial Ginkgo products without any chromatographic purification. The experiment was performed by the analysis of each singlet H-12, which were well separated in the range of 3 6.0-7.0 in the H-1-NMR spectrum. However, the H-12 protons of bilobalide and ginkgolides may have overlapped with H-6 or H-8 protons of the Ginkgo flavonoids. Therefore, the optimum H-1-NMR solvent for the analysis of the compound was selected through the evaluation of solvent effects on the resolution of these signals from the compounds. Acetone-d(6)-benzene-d(6) (50: 50) was found to be the best one among the solvents evaluated. The quantity of the compounds was calculated by the relative ratio of the intensity of each compound to the known amount of internal standard (25 mug/ml), phloroglucinol. This method allows rapid and simple quantitation of underivatized bilobalide and ginkgolides in 5 min without any pre-purification steps.