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KMID : 0861020080230030027
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Korea Journal of Herbology
2008 Volume.23 No. 3 p.27 ~ p.32
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Quantitative Analysis of Quality Control of Natural Medicine by 1H-NMR Spectrometry-Quantitative Analysis of Hesperidin from Citrus unshiu
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Ahn Eun-Mi
Baek Mi-Young
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Abstract
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Objectives : In this paper, we describe that 1H-NMR spectroscopy may be superior to the conventional HPLC for the quantitative analysis of hesperidin from Citrus unshiu.
Methods : 1H-NMR spectra (400 MHz) were recorded in DMSO-d6 using a Varian UNITY Inova AS 400 FT NMR spectrometer. One hundred milligram of powdered Citrus unshiu was weighed out and mixed with 1 ml of DMSO-d6 with sonication for 30 min (room temperature). The extracts were filtrated through a 0.45 μm PVDF filter and 0.5 ml of filtrated extract used for quantitative 1H-NMR measurement (added 1 mg of dimethyl terephthalate as internal standard). The quantity of hesperidin was calculated by the ratio of the intensity of the compound to the known amount of internal standard. For HPLC analysis, the half gram of plant material was extracted with 60 ml of MeOH for 2 hours. The extracts were made 100 ml volume and analyzed by a Waters HPLC system using a YMC ODS column. The total flow rate was 1.0 ml/min with a sample volume 10 μl and UV detection at 280nm.
Results : The contents of hesperidin in Citrus unshiu was determined 5.33±0.06% in the quantitative 1H-NMR method and 5.15±0.12% in HPLC method. Using the quantitative 1H-NMR the contents of hesperidin can be determined in much shorter time than the conventional HPLC measurements.
Conclusions : From those results, the advantages of quantitative 1H-NMR analysis are that can be analyzed to identify and quantify, and no reference compounds required for calibration curve. Besides, it allows rapid and simple quantification for hesperidin with an analysis time for only 10 min without any pre-purification steps.
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KEYWORD
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1H-NMR, HPLC, quantitative analysis, Citrus unshiu, hesperidinttern
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