Use of aframomum melegueta and method for extracting and separating 6-shogaol from aframomum melegueta
A technology of shogaol and heavenly pepper, which is applied in the field of extraction and separation of 6-shogaol, can solve problems that have not been introduced yet, achieve low cost, high yield, and reduce the cost of raw materials
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Embodiment 1
[0039] 1000 kg of raw materials were crushed to 60 mesh, and subcritical extraction was used to obtain oil extract, and the extraction residue was used for the extraction of 6-zingerol.
[0040] The above-mentioned extract was dissolved in 95% ethanol, and then extracted twice with a mixed solvent of n-hexane and petroleum ether in an equal amount. The volume ratio of n-hexane and petroleum ether was 1:1. The extracts were combined and concentrated to the extract.
[0041] The diameter of the pretreatment column is 10cm, and the height is 50cm. The filler used is aluminum oxide. The conventional column filler is silica gel and reverse phase chromatography silica gel C18, and its ratio is 1:1. The elution solvent is n-hexane:ethyl acetate=8: 1. Collect the eluate containing the active ingredient, concentrate to 1 / 100 of the eluate, and place it for crystallization.
[0042] After dissolving the above-mentioned crystalline sample in acetone with 6 times the crystalline mass, con...
Embodiment 2
[0044] 1000 kg of raw materials were pulverized to 100 mesh, and subcritical extraction was used to obtain oil extract, and the extraction residue was used for the extraction of 6-zingerol.
[0045] The above extract was dissolved with 95% ethanol, then extracted twice with a mixed solvent of petroleum ether and ethyl acetate with 1.5 times the mass of the extract, the volume ratio of petroleum ether and ethyl acetate was 10:1, the extracts were combined and concentrated to the extract.
[0046] The pretreatment column diameter is 20cm, and height is 50cm, and used filler is gac, and conventional column filler is chromatographic filler UniP MM500, and elution solvent is sherwood oil: ethyl acetate=4:1, collects the eluent containing active ingredient, Concentrate to 1 / 10 of the eluate and leave to crystallize.
[0047] The above-mentioned crystalline sample was dissolved in ethyl acetate with 10 times the crystalline mass, concentrated to 0.8 times the mass of the crystalline...
Embodiment 3
[0049] 1000kg of raw materials were pulverized to 80 mesh, and subcritical extraction was used to obtain oil extract, and the extraction residue was used for the extraction of 6-zingerol.
[0050] The above-mentioned extract is dissolved in 95% ethanol, then extracted twice with a mixed solvent of n-hexane, sherwood oil and ethyl acetate equal to the mass of the extract, and the volume ratio of n-hexane, sherwood oil and ethyl acetate is 8:5 : 1, the extracts are combined and concentrated to extract.
[0051] The pretreatment column diameter is 20cm, and height is 50cm, and used filler is Sephadex LH-200, and conventional column filler is chromatographic filler UniP MM500, and elution solvent is n-hexane: sherwood oil: ethanol=91:8:1, collects and contains effective The eluate of the components was concentrated to 5 / 100 of the eluate, and left to crystallize.
[0052]The above-mentioned crystalline sample was dissolved in ethanol with 7 times the crystalline quality, concentr...
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