A kind of preparation method of effective part of Yemachai
An effective part, wild horse technology, applied in the field of traditional Chinese medicine and natural medicine, can solve the problems of composition defects, lack of large-scale equipment, high production cost of reversed-phase silica gel chromatography technology, etc., and achieve low production cost and green production process.
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Embodiment 1
[0109] Example 1 Preparation of the effective fraction of Yemazhui (1)
[0110] (1) extract
[0111] Take 5kg of Yemachai medicinal material, add 50% ethanol to extract twice, filter, recover the filtrate under reduced pressure, add water to make the medicinal solution contain 0.5g of crude drug per ml, and set aside; HPLC detection chart is attached figure 1 .
[0112] (2) Macroporous resin refining
[0113] Pass the above medicinal solution through AB-8 macroporous resin chromatographic column (5L), first elute with 2 times the column volume of water, then 2 times the column volume of 85% ethanol, collect the ethanol eluate, and recover ethanol under reduced pressure , concentrated to a relative density of 1.30 (50°C) thick paste 280g;
[0114] (3) Supercritical extraction and refining
[0115] Take 280g of thick paste, add 10 times the weight of adsorbent, mix well, dry, pulverize, put into supercritical extraction axe, with extraction pressure of 30MPa, extraction temp...
Embodiment 2
[0116] Example 2 Preparation of the effective fraction of Yemazhui (2)
[0117] (1) extract
[0118] Take 3kg of Ye Ma Zhui medicinal material, add water to decoct and extract with alcohol twice, filter, recover the filtrate under reduced pressure to 1g of crude drug per ml, and set aside;
[0119] (2) Macroporous resin refining
[0120] Pass the above medicinal solution through HPD-400 macroporous resin chromatographic column (4L), first elute with 2 times the column volume of water, then 2 times the column volume of 60% ethanol, collect the ethanol eluate, and recover ethanol under reduced pressure , concentrated to a relative density of 1.28 (50°C) thick paste 215g;
[0121] (3) Supercritical extraction and refining
[0122] Take 215g of thick paste, add 5 times the weight of adsorbent, mix well, dry, pulverize, put into supercritical extraction axe, with extraction pressure of 35MPa, extraction temperature of 50°C, entrainer (ethanol) dosage of 20%, separation pressure ...
Embodiment 3
[0123] Example 3 Preparation of the effective fraction of Yemazhui (3)
[0124] (1) extract
[0125] Take 5 kg of Ye Ma Zhui medicinal material, add 30% ethanol to extract twice, filter, recover the filtrate under reduced pressure to 0.5 g of crude drug per ml, and set aside;
[0126] (2) Macroporous resin refining
[0127] Pass the above medicinal solution through a D101 macroporous resin chromatographic column (8L), first elute with 2 times the column volume of water, then 3 times the column volume of 70% ethanol, collect the ethanol eluate, recover ethanol under reduced pressure, concentrate To a relative density of 1.31 (50 ℃) thick paste 283g;
[0128] (3) Supercritical extraction and refining
[0129] Take 283g of thick paste, add 15 times the weight of adsorbent, mix well, dry, pulverize, put into supercritical extraction axe, with extraction pressure of 40MPa, extraction temperature of 40°C, entrainer (80% ethanol) dosage of 10%, The separation pressure is 7MPa, th...
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