A kind of bergamot flavone extract and its separation and purification method
A technology of bergamot flavonoids and extracts, which is applied in the field of separation and purification, can solve the problems of low extraction rate, many impurities, and generate a large amount of acid-base solution, and achieves the effects of large extraction amount and high extraction efficiency.
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Embodiment 1
[0043] Embodiment 1 A kind of method for separating and purifying flavone extract from Guangfo hands
[0044] 1. Purification method
[0045] (1) Preparation of the crude extract of bergamot flavonoids: 400g of bergamot flavonoids was extracted by continuous phase change extraction. The extraction conditions were: ethanol concentration 85%, extraction temperature 90°C, extraction time 120min, flow rate 20L / h;
[0046] (2) Polyamide resin pretreatment: Take an appropriate amount of polyamide resin and soak it in 95% ethanol for 24 hours, stir continuously, remove air bubbles, and put it into the column. Elute with 3 column volumes of 95% ethanol until the eluate is transparent and there is no residue (or very little residue) after evaporation to dryness. Then sequentially elute with 2.5 times column volume of 5% NaOH aqueous solution, 1 times column volume of distilled water, and 2.5 times column volume of 10% acetic acid aqueous solution, and finally elute with distilled wat...
Embodiment 2
[0059] Example 2 Influence of sample loading flow rate on polyamide adsorption effect
[0060] Pretreated polyamide resin 5g (on a dry basis) is packed into a glass chromatography column (26×400 mm) by a wet method, the column volume is 20mL, and the sample loading is 2.087mg / mL (flavonoid concentration) prepared in Example 1 The crude extract of flavonoids was loaded at 1.0mL / min, 1.5mL / min, and 2.0mL / min respectively for dynamic adsorption, and the effluent was collected according to the column bed volume (BV) (BV is the volume multiple of the resin), and each The concentration of total flavonoids in bergamot in part of the effluent was detected, and the concentration of flavonoids was detected, and the flow rate was plotted against the concentration of the effluent to investigate the effect of sample loading flow rate on the adsorption effect. result Figure 4 shown. Depend on Figure 4 It can be seen that when the sample loading flow rate is 1 mL / min, the time to reach ...
Embodiment 3
[0061] Example 3 The influence of sample loading volume on polyamide adsorption effect
[0062] Pretreated polyamide resin 5g (on a dry basis) is packed into a glass chromatography column (26×400 mm) by a wet method, the column volume is 20mL, and the sample loading is 2.087mg / mL (flavonoid concentration) prepared in Example 1 The crude extract of flavonoids, the loading flow rate is 1mL / min, the direction flows through the resin bed from top to bottom, the effluent is collected according to the column bed volume (BV) (BV is the resin volume multiple), and the total amount of bergamot in each effluent is measured. Concentration of flavonoids, taking the concentration of total flavonoids in the effluent as one-tenth of the concentration of the sample solution as the leak point, taking the volume of the effluent (BV) as the abscissa, the percentage of the total flavonoids in the effluent and the total flavonoids in the sample solution Values (C / C0 x 100%) were used to plot the...
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