New method for purifying nettle extract 3,4-divanilyltetrahydrofuran
A technology of tetrahydrofuran and two vanilla, applied in 3 fields, can solve problems such as low extraction purity and low extraction rate
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Embodiment 1
[0012] Example 1: A method for significantly improving the purity of 3,4-divanillyltetrahydrofuran in nettle using ultra-high pressure extraction and column chromatography coupling technology. The steps are as follows:
[0013] (1) Put the cut sections of dried nettle into a pressure-resistant bag, add 6 times the volume of ethanol with a concentration of 70%, treat it under ultra-high pressure 200MPA, 10min, 20℃, recover the ethanol, and dry it under vacuum at 60℃. Crude:
[0014] (2) Dissolve the obtained crude powder of 3,4 divanillyl tetrahydrofuran in ethyl acetate, add an appropriate amount of pre-activated silica gel, stir, dry the ethyl acetate, pass through a 60 mesh sieve, and apply 200 mesh silica gel column chromatography to an industrial-grade column ;
[0015] (3) At a flow rate of 2BV / h, gradient elution was carried out with ethyl acetate-methanol under 3:1, 4:1, 5:1 conditions, followed by thin layer chromatography, and collected 3,4 divanillyltetrahydrofuran Ingr...
Embodiment example 2
[0019] Implementation case 2: A method for enriching and purifying 3,4 divanillyl tetrahydrofuran in nettle using macroporous adsorption resin, the steps are as follows:
[0020] (1) Put the cut sections of dried nettle into a pressure-resistant bag, add 7 times the volume of ethanol with a concentration of 75%, treat it under ultra-high pressure 300MPA, 15min, 20℃, recover the ethanol, and dry it under vacuum at 60℃. Crude;
[0021] (2) Dissolve the obtained 3,4 divanillyl tetrahydrofuran coarse crystalline powder in ethyl acetate, add an appropriate amount of pre-activated silica gel, stir, dry the ethyl acetate, pass through a 60-mesh sieve, and apply a 300-mesh silica gel column to an industrial-grade column Analyze
[0022] (3) Perform gradient elution with ethyl acetate-methanol under the conditions of 3-5:1 at a flow rate of 3BV / h, followed by thin-layer chromatography, and collect the fraction containing 3,4-divanillyltetrahydrofuran;
[0023] (4) Use a thin layer to determi...
Embodiment example 3
[0026] Implementation case 3: A method for enriching and purifying 3,4 divanillyl tetrahydrofuran in nettle using macroporous adsorption resin, the steps are as follows:
[0027] (1) Put the cut sections of dried nettle into a pressure-resistant bag, add 8 times the volume of ethanol with a concentration of 80%, treat it under ultra-high pressure 400MPA, 12min, 20℃, recover the ethanol, and dry it under vacuum at 60℃. Crude;
[0028] (2) Dissolve the obtained crude powder of 3,4 divanillyl tetrahydrofuran in ethyl acetate, add an appropriate amount of pre-activated silica gel, stir, dry the ethyl acetate, pass through a 60 mesh sieve, and apply 200 mesh silica gel column chromatography to an industrial-grade column ;
[0029] (3) At a flow rate of 3BV / h, use petroleum ether-ethanol to perform gradient elution under the conditions of 3-5:1, followed by thin-layer chromatography, and collect the 3,4-divanillyltetrahydrofuran fraction;
[0030] (4) Use a thin layer to determine the 3,4...
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