Summary of the invention
Technical problem to be solved by this invention is to provide a kind of extraction process of Radix potentillae anserinae total triterpene easy, efficient, with low cost.
For solving the problem, the extraction process of a kind of Radix potentillae anserinae total triterpene of the present invention, comprises the following steps:
(1) Radix potentillae anserinae root is after pulverizing, crossing 10 ~ 60 mesh sieves, obtains Radix potentillae anserinae root powder;
(2) be the alcoholic solution extraction of 50 ~ 95% by described Radix potentillae anserinae root powder mass concentration, obtain extracting solution, this extracting solution obtains filtrate after filtration, and described filtrate obtains extractum through concentrating under reduced pressure; The mass volume ratio of described Radix potentillae anserinae root powder and described alcoholic solution is 1g:10 ~ 30mL;
(3) add water sedimentation 2 ~ 3 times in described extractum, and left at room temperature 1 ~ 3h after stirring, then filters, obtain precipitum;
(4) the dehydrated alcohol adding its quality 2 ~ 5 times in described precipitum dissolves, obtain lysate, in this lysate, add the decolorization and impurity removal by active carbon of its volume 40% ~ 70%, reclaim ethanol, under temperature is 50 ~ 70 DEG C of conditions through drying under reduced pressure to constant weight, obtain crude extract;
(5) by the deionized water dissolving of described crude extract by its quality 2 ~ 10 times, then add ether after concussion extraction, left at room temperature layering, removes ether layer, repeats to merge afterwards for 3 ~ 5 times to be extracted liquid;
(6) in described extract, add the n-butyl alcohol of its volume 2 ~ 5 times, after concussion extraction, left at room temperature layering, get butanol solution part, re-extract 4 ~ 7 times, merge and obtain butanol solution, this butanol solution to constant weight, obtains Radix potentillae anserinae total-triterpene extract through drying under reduced pressure.
Described step (2) in extraction conditions refer to that temperature is 60 ~ 80 DEG C, extraction time 3 ~ 4 times, each 0.5 ~ 2.5 h.
Described step (2) in concentrating under reduced pressure condition refer to that temperature is 50 ~ 70 DEG C.
Described step is replaced (4) to prepare crude extract by following preparation method: the dehydrated alcohol adding its quality 2 ~ 5 times in described precipitum dissolves, obtain lysate, this lysate is adsorbed to the inspection of effluent maloic acid with the macroporous adsorptive resins AB-8 of its quality 2/3 times and is positive; Then use the washing post bed of lysate quality 5 ~ 6 times closely colourless to effluent, then use lysate quality 5 ~ 6 times and the ethanol elution that mass concentration is 95% is negative to ethanol elution, collect eluent, reclaim ethanol, obtain crude extract.
Described step (6) in drying under reduced pressure condition refer to that temperature is 60 ~ 80 DEG C.
The present invention compared with prior art has the following advantages:
1, because the present invention carries out sedimentation by after extract water dissolution, most starch and polysaccharide can be removed fast, therefore, for the purification in later stage reduces difficulty.
2, the present invention adopts macroporous resin to carry out purification process, just can obtain the higher Radix potentillae anserinae total triterpene of purity through water and ethanol two-step pretreatment.
3, the inventive method is simple to operate, and production cost is low, and gained Radix potentillae anserinae total triterpene composition has anticancer function, can be used for preparing the active drug that acceptable carrier can be made into multiple dosage form.
Detailed description of the invention
embodiment 1an extraction process for Radix potentillae anserinae total triterpene, comprises the following steps:
(1) 0.5kg Radix potentillae anserinae root is after pulverizing, crossing 10 mesh sieves, obtains Radix potentillae anserinae root powder.
(2) by Radix potentillae anserinae root powder mass concentration be 50% alcoholic solution be extract under the condition of 60 DEG C in temperature, extraction time 3 times, each 0.5 h, merges and obtains extracting solution, this extracting solution obtains filtrate after filtration, and filtrate obtains extractum through concentrating under reduced pressure under temperature is 50 DEG C of conditions.
Wherein: the mass volume ratio of Radix potentillae anserinae root powder and alcoholic solution is 1g:10mL.
(3) add water sedimentation 2 times in extractum, and left at room temperature 1 h after stirring, then filters, obtain precipitum.
(4) the dehydrated alcohol adding its quality 2 times in precipitum dissolves, and obtains lysate, adds the decolorization and impurity removal by active carbon of its volume 50% in this lysate, reclaim ethanol, under temperature is 50 DEG C of conditions through drying under reduced pressure to constant weight, obtain crude extract.
(5) by the deionized water dissolving of crude extract by its quality 2 times, then add ether after concussion extraction, left at room temperature layering, removes ether layer, repeats to merge afterwards for 4 times to be extracted liquid.
(6) in extract, add the n-butyl alcohol of its volume 2 times, after concussion extraction, left at room temperature layering, get butanol solution part, re-extract 4 times, merge obtain butanol solution, this butanol solution under temperature is 60 DEG C of conditions through drying under reduced pressure to constant weight, obtain Radix potentillae anserinae total-triterpene extract 9.6g.
embodiment 2an extraction process for Radix potentillae anserinae total triterpene, comprises the following steps:
(1) 1kg Radix potentillae anserinae root is after pulverizing, crossing 40 mesh sieves, obtains Radix potentillae anserinae root powder.
(2) by Radix potentillae anserinae root powder mass concentration be 60% alcoholic solution be extract under the condition of 70 DEG C in temperature, extraction time 4 times, each 1 h, merges and obtains extracting solution, this extracting solution obtains filtrate after filtration, and filtrate obtains extractum through concentrating under reduced pressure under temperature is 70 DEG C of conditions.
Wherein: the mass volume ratio of Radix potentillae anserinae root powder and alcoholic solution is 1g:20mL.
(3) add water sedimentation 3 times in extractum, and left at room temperature 2h after stirring, then filters, obtain precipitum.
(4) the dehydrated alcohol adding its quality 5 times in precipitum dissolves, and obtains lysate, adds the decolorization and impurity removal by active carbon of its volume 40% in this lysate, reclaim ethanol, under temperature is 70 DEG C of conditions through drying under reduced pressure to constant weight, obtain crude extract.
(5) by the deionized water dissolving of crude extract by its quality 5 times, then add ether after concussion extraction, left at room temperature layering, removes ether layer, repeats to merge afterwards for 3 times to be extracted liquid.
(6) in extract, add the n-butyl alcohol of its volume 5 times, after concussion extraction, left at room temperature layering, get butanol solution part, re-extract 5 times, merge obtain butanol solution, this butanol solution under temperature is 80 DEG C of conditions through drying under reduced pressure to constant weight, obtain Radix potentillae anserinae total-triterpene extract 13.5g.
embodiment 3an extraction process for Radix potentillae anserinae total triterpene, comprises the following steps:
(1) 10kg Radix potentillae anserinae root is after pulverizing, crossing 60 mesh sieves, obtains Radix potentillae anserinae root powder.
(2) by Radix potentillae anserinae root powder mass concentration be 95% alcoholic solution be extract under the condition of 80 DEG C in temperature, extraction time 3 times, each 2.5 h, merge and obtain extracting solution, this extracting solution obtains filtrate after filtration, and filtrate obtains extractum through concentrating under reduced pressure under temperature is 60 DEG C of conditions.
Wherein: the mass volume ratio of Radix potentillae anserinae root powder and alcoholic solution is 1g:30mL.
(3) add water sedimentation 2 times in extractum, and left at room temperature 3h after stirring, then filters, obtain precipitum.
(4) the dehydrated alcohol adding its quality 3 times in precipitum dissolves, and obtains lysate, adds the decolorization and impurity removal by active carbon of its volume 70% in this lysate, reclaim ethanol, under temperature is 60 DEG C of conditions through drying under reduced pressure to constant weight, obtain crude extract.
(5) by the deionized water dissolving of crude extract by its quality 10 times, then add ether after concussion extraction, left at room temperature layering, removes ether layer, repeats to merge afterwards for 5 times to be extracted liquid.
(6) in extract, add the n-butyl alcohol of its volume 3 times, after concussion extraction, left at room temperature layering, get butanol solution part, re-extract 7 times, merge obtain butanol solution, this butanol solution under temperature is 70 DEG C of conditions through drying under reduced pressure to constant weight, obtain Radix potentillae anserinae total-triterpene extract 120g.
embodiment 4an extraction process for Radix potentillae anserinae total triterpene, comprises the following steps:
(1) 0.5kg Radix potentillae anserinae root is after pulverizing, crossing 40 mesh sieves, obtains Radix potentillae anserinae root powder.
(2) by Radix potentillae anserinae root powder mass concentration be 70% alcoholic solution be extract under the condition of 70 DEG C in temperature, extraction time 3 times, each 1h, merge obtain extracting solution, this extracting solution obtains filtrate after filtration, and filtrate obtains extractum through concentrating under reduced pressure under temperature is 50 DEG C of conditions.
Wherein: the mass volume ratio of Radix potentillae anserinae root powder and alcoholic solution is 1g:20mL.
(3) add water sedimentation 3 times in extractum, and left at room temperature 1h after stirring, then filters, obtain precipitum.
(4) the dehydrated alcohol adding its quality 2 times in precipitum dissolves, and obtains lysate, and this lysate is adsorbed to the inspection of effluent maloic acid with the macroporous adsorptive resins AB-8 of its quality 2/3 times and is positive; Then use the washing post bed of lysate quality 5 times closely colourless to effluent, then by lysate quality 5 times and the ethanol elution that mass concentration is 95% be negative to ethanol elution, collect eluent, reclaim ethanol, obtain crude extract.
(5) by the deionized water dissolving of crude extract by its quality 2 times, then add ether after concussion extraction, left at room temperature layering, removes ether layer, repeats to merge afterwards for 3 times to be extracted liquid.
(6) in extract, add the n-butyl alcohol of its volume 2 times, after concussion extraction, left at room temperature layering, get butanol solution part, re-extract 5 times, merge obtain butanol solution, this butanol solution under temperature is 60 DEG C of conditions through drying under reduced pressure to constant weight, obtain Radix potentillae anserinae total-triterpene extract 10.8g.
embodiment 5an extraction process for Radix potentillae anserinae total triterpene, comprises the following steps:
(1) 1kg Radix potentillae anserinae root is after pulverizing, crossing 30 mesh sieves, obtains Radix potentillae anserinae root powder.
(2) by Radix potentillae anserinae root powder mass concentration be 80% alcoholic solution be extract under the condition of 80 DEG C in temperature, extraction time 3 times, each 2 h, merge and obtain extracting solution, this extracting solution obtains filtrate after filtration, and filtrate obtains extractum through concentrating under reduced pressure under temperature is 60 DEG C of conditions.
Wherein: the mass volume ratio of Radix potentillae anserinae root powder and alcoholic solution is 1g:30mL.
(3) add water sedimentation 3 times in extractum, and left at room temperature 3h after stirring, then filters, obtain precipitum.
(4) the dehydrated alcohol adding its quality 5 times in precipitum dissolves, and obtains lysate, and this lysate is adsorbed to the inspection of effluent maloic acid with the macroporous adsorptive resins AB-8 of its quality 2/3 times and is positive; Then use the washing post bed of lysate quality 6 times closely colourless to effluent, then by lysate quality 6 times and the ethanol elution that mass concentration is 95% be negative to ethanol elution, collect eluent, reclaim ethanol, obtain crude extract.
(5) by the deionized water dissolving of crude extract by its quality 6 times, then add ether after concussion extraction, left at room temperature layering, removes ether layer, repeats to merge afterwards for 5 times to be extracted liquid.
(6) in extract, add the n-butyl alcohol of its volume 5 times, after concussion extraction, left at room temperature layering, get butanol solution part, re-extract 7 times, merge obtain butanol solution, this butanol solution under temperature is 80 DEG C of conditions through drying under reduced pressure to constant weight, obtain Radix potentillae anserinae total-triterpene extract 14.7g.
embodiment 6an extraction process for Radix potentillae anserinae total triterpene, comprises the following steps:
(1) 10kg Radix potentillae anserinae root is after pulverizing, crossing 60 mesh sieves, obtains Radix potentillae anserinae root powder.
(2) by Radix potentillae anserinae root powder mass concentration be 95% alcoholic solution be extract under the condition of 80 DEG C in temperature, extraction time 4 times, each 2 h, merge and obtain extracting solution, this extracting solution obtains filtrate after filtration, and filtrate obtains extractum through concentrating under reduced pressure under temperature is 70 DEG C of conditions.
Wherein: the mass volume ratio of Radix potentillae anserinae root powder and alcoholic solution is 1g:30mL.
(3) add water sedimentation 3 times in extractum, and left at room temperature 2h after stirring, then filters, obtain precipitum.
(4) the dehydrated alcohol adding its quality 4 times in precipitum dissolves, and obtains lysate, and this lysate is adsorbed to the inspection of effluent maloic acid with the macroporous adsorptive resins AB-8 of its quality 2/3 times and is positive; Then use the washing post bed of lysate quality 5.5 times closely colourless to effluent, then by lysate quality 5.5 times and the ethanol elution that mass concentration is 95% be negative to ethanol elution, collect eluent, reclaim ethanol, obtain crude extract.
(5) by the deionized water dissolving of crude extract by its quality 8 times, then add ether after concussion extraction, left at room temperature layering, removes ether layer, repeats to merge afterwards for 5 times to be extracted liquid.
(6) in extract, add the n-butyl alcohol of its volume 4 times, after concussion extraction, left at room temperature layering, get butanol solution part, re-extract 7 times, merge obtain butanol solution, this butanol solution under temperature is 70 DEG C of conditions through drying under reduced pressure to constant weight, obtain Radix potentillae anserinae total-triterpene extract 126g.