CN104403020A - Semi-bionic lentinan extraction method - Google Patents
Semi-bionic lentinan extraction method Download PDFInfo
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- CN104403020A CN104403020A CN201410700171.5A CN201410700171A CN104403020A CN 104403020 A CN104403020 A CN 104403020A CN 201410700171 A CN201410700171 A CN 201410700171A CN 104403020 A CN104403020 A CN 104403020A
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Abstract
The invention discloses a semi-bionic lentinan extraction method which mainly comprises the following steps: (1) raw material pretreatment; (2) weakly acidic water extraction; (3) weakly alkaline water extraction; (4) neutral water extraction; (5) eluent preparation; (6) trapped fluid preparation; (7) concentration under reduced pressure; (8) centrifugal removal of precipitates; (9) vacuum drying of the precipitates; (10) crushing and packaging. According to the semi-bionic lentinan extraction method, pure water extraction is replaced by semi-bionic extraction, an HD-3 resin column is adopted for decolorization and deproteinization, and an ultrafiltration membrane is adopted for ultrafiltration fractionation, so that high lentinan extraction yield and high lentinan purity are achieved.
Description
Technical field
the present invention relates to a kind of extraction method of polysaccharides, particularly a kind of method of semi-bionic extraction lentinan.
Background technology
mushroom has another name called mushroom, is famous edible medicinal fungi of holding concurrently, before more than 1,000 years, just starts collection and utilization.Have in Compendium of Material Medica: mushroom " sweet, flat, nontoxic "; " medical center bun will " be recorded: mushroom " sweet, cold ", " can hold in the palm acne poison "; " life book on Chinese herbal medicine " thinks mushroom " beneficial gas, not hungry, control wind and break blood "; " herbal classic is met former " think mushroom " for compensate vitamins D want agent, prevention rickets, and eliminate-poverty blood ".Mushroom contains multiple effective medicinal ingredients, after contained ergosterol (provitamin D, its content is higher than general food) is absorbed by the body, vitamins D can be changed under light illumination, the resistibility of human body can be strengthened, and the growth of children's bone and tooth can be promoted, prevention rickets.
lentinan is topmost effective active composition in mushroom fruiting body, activeconstituents in lentinan is β-(1-3)-D-dextran with branch, main chain is made up of the glucosyl group of β-(1-3)-connection, the glucosyl group connected by β-(1-6), in pectination along main chain stochastic distribution.Research show active polysaccharide composition β-(1-3)-D-dextran of mushroom to suppress allos, homology or even genetic tumour all effective.Lentinan can stimulate the immunity system of body, immunologic function is restored and improves, thus plays anti-cancer, antitumous effect.
the original extracting method of lentinan mainly takes over each method of tradition system of fungus polysaccharide, after hot water extraction, direct united extraction liquid concentrates, then uses alcohol precipitation, after sediment fraction centrifugation being gone out, obtain Crude polysaccharides goods by spraying dry after vacuum-drying or water dissolution.With the water-soluble polysaccharide that single water extraction can only propose wherein, the polysaccharide in a lot of cell wall is also had to be difficult to extract.Mushroom to be utilized further, prepare its deep processed product, only have and improve extraction process on the original basis, the hedgehogt fungus crude polysaccharose extract of high density could be prepared.The deficiency of tradition water extract-alcohol precipitation method mainly contains: the Crude polysaccharides yield 1, extracted is low, not high to the utilization ratio of former section; 2, there are many pectin substance class viscous substances in mushroom, add polysaccharide content in the extract obtained of extracting solution during extraction not high, affect the performance of its efficacy effect.
Summary of the invention
the object of this invention is to provide a kind of method of semi-bionic extraction lentinan, replace simple water extraction with semi-bionic extraction, finally adopt HD-3 resin column decolouring deproteinated and ultra-filtration membrane ultrafiltration classification, make that Polyose extraction yield is high, purity good.
object of the present invention is achieved through the following technical solutions: a kind of method of semi-bionic extraction lentinan, and the method for described semi-bionic extraction lentinan follows these steps to order and carries out:
(1) raw materials pretreatment: get dry mushroom, pulverizes, and crosses 50 ~ 120 mesh sieves, obtains mushroom dried powder;
(2) weakly acidic water extracts: regulate between extraction water to pH4.0-5.5 with weak acid, take the mushroom dried powder of appropriate (1) step, the proportion being 1:5-1:25 by solid-liquid ratio adds weakly acidic water, heat and control temperature at 50-60 DEG C, atmospheric pressure state extracts l-2 hour, centrifugation, obtains filtrate 1 and filter residue;
(3) alkalescent water extracts: regulate between extraction water to pH7-8 with weak base, be that the filter residue that the proportion of 1:5-1:25 obtains to (2) step adds alkalescent water by solid-liquid ratio, heat and control temperature at 50-60 DEG C, atmospheric pressure state extracts 1-2 hour, centrifugation, obtains filtrate 2 and filter residue;
(4) neutral water extracts: regulate extraction use water pH neutral with acid, be that the filter residue that 1:5-1:25 obtains to (3) step adds neutral water by solid-liquid ratio, heat and control temperature at 95-100 DEG C, atmospheric pressure state extracts 1 hour, filter press, filtrate puts into storage tank, centrifugation, obtain filtrate 3 and filter residue, residue discards;
(5) prepare elutriant: merging filtrate 1, filtrate 2, filtrate 3, regulate filtrate pH to be 4.0 ~ 4.5 with dilute hydrochloric acid, upper chromatography column, in post, filled media is HD-3 resin, chromatographic decolorization deproteinated under 4 ~ 5BV/h flow velocity, collects 6 ~ 7BV elutriant;
(6) trapped fluid is prepared: regulate elutriant pH to be 6.5 ~ 7.5, under 0.1 ~ 0.25Mpa pressure, carry out ultrafiltration with the ceramic membrane that ultra-filtration membrane is 50KD and 10KD, trapped fluid in the middle of collecting;
(7) concentrating under reduced pressure: the trapped fluid of (6) step is carried out concentrating under reduced pressure, thickening temperature 65-70 DEG C, pressure is less than 0.lMPa, when concentrating as 500 DEG C of heat surveys, proportion is 1.050-1.080;
(8) centrifugal segregation sediment: 4000rmp high speed centrifugation, disgorging, supernatant liquor is cooked alcohol precipitation further and uses;
(9) precipitate vacuum-drying: throw out is loaded high plate equably, expect that high to be no more than dish high by 1/3, be first placed in 60-65 DEG C of baking oven inner drying 4 hours, then vacuumize drying, temperature controls 65 DEG C, negative pressure 0.lMPa, vacuum-drying 8 hours;
(10) pulverize: take out dry thing, the pulverizer be cooled with circulating water, by crushing material, is crossed 80 mesh sieves, is namely obtained lentinan.
beneficial effect of the present invention: the present invention's semi-bionic extraction replaces simple water extraction, finally adopts HD-3 resin column decolouring deproteinated and ultra-filtration membrane ultrafiltration classification, makes that Polyose extraction yield is high, purity good.
1. half bionical be from biopharmacy angle, simulation oral administration and medicine are through the principle of gastrointestinal transit, and be a kind of new extraction process designed through the Chinese medicine preparation of digestive tube administration, its feature retains more effective constituent.
2. apply resin chromatography post and carry out decolouring deproteinated, eliminate protein equimolecular impurity, make the polysaccharide content of extraction higher, purer.
Embodiment
embodiment 1
(1): get dry mushroom (can be obtained through natural air drying by new fresh mushroom), pulverize, 80 mesh sieves, obtain mushroom dried powder;
(2) weakly acidic water extracts: regulate extraction water to pH4.0 with weak acid, and taking the powder of appropriate (1) step, is that 1:8 adds weakly acidic water by solid-liquid ratio, heat and control temperature at 50-60 DEG C, atmospheric pressure state extracts l hour, and centrifugation, obtains filtrate 1 and filter residue;
(3) alkalescent water extracts: regulate extraction water to pH8.0 with alkali, and being 1:8 by solid-liquid ratio adds week-base water to the filter residue of (1) step, heat and control temperature at 50-60 DEG C, atmospheric pressure state extracts 1 hour, centrifugation, obtains filtrate 2 and filter residue;
(4) neutral water extracts: neutral with acid for adjusting pH, and being 1:8 by solid-liquid ratio adds neutral water to the filter residue of (3) step, heat and control temperature at 95-100 DEG C, atmospheric pressure state extracts 1 hour, filter press, and filtrate 15 puts into storage tank.Centrifugation, obtain filtrate 3 and filter residue, residue discards;
(5) merge No. three extracting solutions, regulate filtrate pH to be 4.0 ~ 4.5 with dilute hydrochloric acid, upper chromatography column, in post, filled media is HD-3 resin, chromatographic decolorization deproteinated under 4 ~ 5BV/h flow velocity, collects 6 ~ 7BV elutriant;
(6) regulate elutriant pH to be 6.5 ~ 7.5, under 0.1 ~ 0.25Mpa pressure, carry out ultrafiltration with the ceramic membrane that ultra-filtration membrane is 50KD and 10KD, trapped fluid in the middle of collecting;
(7) concentrating under reduced pressure: the trapped fluid of (6) step is carried out concentrating under reduced pressure, thickening temperature 65-70 DEG C, pressure is less than 0.lMPa, is concentrated to proportion 1.050-1.080 (500 DEG C of heat are surveyed);
(8) centrifugal segregation sediment: 4000rmp high speed centrifugation, disgorging, supernatant liquor is cooked alcohol precipitation further and uses;
(9) precipitate vacuum-drying: throw out is loaded high plate equably, expect that high to be no more than dish high by 1/3, be first placed in 60-65 DEG C of baking oven inner drying 4 hours, then vacuumize drying, temperature controls 65 DEG C, negative pressure 0.lMPa, vacuum-drying 8 hours;
(10) pulverize: take out dry thing, the pulverizer be cooled with circulating water, by crushing material, is crossed 80 mesh sieves, is namely obtained lentinan.
the lentinan yield extracted is 21.32%.
embodiment 2
(1) get dry mushroom (can be obtained through natural air drying by new fresh mushroom), pulverize, cross 80 mesh sieves, obtain mushroom dried powder;
(2) weakly acidic water extracts: regulate extraction water to pH4.0 with weak acid, and taking the powder of appropriate (1) step, is that 1:8 adds weakly acidic water by solid-liquid ratio, heat and control temperature at 50-60 DEG C, atmospheric pressure state extracts 2 hours, centrifugation, obtains filtrate 1 and filter residue;
(3) alkalescent water extracts: regulate extraction water to pH8.0 with alkali, and being 1:8 by solid-liquid ratio adds week-base water to the filter residue of (1) step, heat and control temperature at 50-60 DEG C, atmospheric pressure state extracts 2 hours, centrifugation, obtains filtrate 2 and filter residue;
(4) neutral water extracts: neutral with acid for adjusting pH, and being 1:8 by solid-liquid ratio adds neutral water to the filter residue of (3) step, heat and control temperature at 95-100 DEG C, atmospheric pressure state extracts 1 hour, filter press, and filtrate 15 puts into storage tank, centrifugation, obtain filtrate 3 and filter residue, residue discards;
(5) merge No. three extracting solutions, regulate filtrate pH to be 4.0 ~ 4.5 with dilute hydrochloric acid, upper chromatography column, in post, filled media is HD-3 resin, chromatographic decolorization deproteinated under 4 ~ 5BV/h flow velocity, collects 6 ~ 7BV elutriant;
(6) regulate elutriant pH to be 6.5 ~ 7.5, under 0.1 ~ 0.25Mpa pressure, carry out ultrafiltration with the ceramic membrane that ultra-filtration membrane is 50KD and 10KD, trapped fluid in the middle of collecting;
(7) concentrating under reduced pressure: the trapped fluid of (6) step is carried out concentrating under reduced pressure, thickening temperature 65-70 DEG C, pressure is less than 0.lMPa, is concentrated to proportion 1.050-1.080 (500 DEG C of heat are surveyed);
(8) centrifugal segregation sediment: 4000rmp high speed centrifugation, disgorging, supernatant liquor is cooked alcohol precipitation further and uses;
(9) precipitate vacuum-drying: throw out is loaded high plate equably, expect that high to be no more than dish high by 1/3, be first placed in 60-65 DEG C of baking oven inner drying 4 hours.Vacuumize drying again, temperature controls 65 DEG C, negative pressure 0.lMPa, vacuum-drying 8 hours;
(10) pulverize: take out dry thing, the pulverizer be cooled with circulating water, by crushing material, is crossed 80 mesh sieves, is namely obtained lentinan;
the lentinan yield extracted is 24.21%.
Claims (1)
1. a method for semi-bionic extraction lentinan, is characterized in that: the method for described semi-bionic extraction lentinan follows these steps to order and carries out:
(1) raw materials pretreatment: get dry mushroom, pulverizes, and crosses 50 ~ 120 mesh sieves, obtains mushroom dried powder;
(2) weakly acidic water extracts: regulate between extraction water to pH4.0-5.5 with weak acid, take the mushroom dried powder of appropriate (1) step, the proportion being 1:5-1:25 by solid-liquid ratio adds weakly acidic water, heat and control temperature at 50-60 DEG C, atmospheric pressure state extracts l-2 hour, centrifugation, obtains filtrate 1 and filter residue;
(3) alkalescent water extracts: regulate between extraction water to pH7-8 with weak base, be that the filter residue that the proportion of 1:5-1:25 obtains to (2) step adds alkalescent water by solid-liquid ratio, heat and control temperature at 50-60 DEG C, atmospheric pressure state extracts 1-2 hour, centrifugation, obtains filtrate 2 and filter residue;
(4) neutral water extracts: regulate extraction use water pH neutral with acid, be that the filter residue that 1:5-1:25 obtains to (3) step adds neutral water by solid-liquid ratio, heat and control temperature at 95-100 DEG C, atmospheric pressure state extracts 1 hour, filter press, filtrate puts into storage tank, centrifugation, obtain filtrate 3 and filter residue, residue discards;
(5) prepare elutriant: merging filtrate 1, filtrate 2, filtrate 3, regulate filtrate pH to be 4.0 ~ 4.5 with dilute hydrochloric acid, upper chromatography column, in post, filled media is HD-3 resin, chromatographic decolorization deproteinated under 4 ~ 5BV/h flow velocity, collects 6 ~ 7BV elutriant;
(6) trapped fluid is prepared: regulate elutriant pH to be 6.5 ~ 7.5, under 0.1 ~ 0.25Mpa pressure, carry out ultrafiltration with the ceramic membrane that ultra-filtration membrane is 50KD and 10KD, trapped fluid in the middle of collecting;
(7) concentrating under reduced pressure: the trapped fluid of (6) step is carried out concentrating under reduced pressure, thickening temperature 65-70 DEG C, pressure is less than 0.lMPa, when concentrating as 500 DEG C of heat surveys, proportion is 1.050-1.080;
(8) centrifugal segregation sediment: 4000rmp high speed centrifugation, disgorging, supernatant liquor is cooked alcohol precipitation further and uses;
(9) precipitate vacuum-drying: throw out is loaded high plate equably, expect that high to be no more than dish high by 1/3, be first placed in 60-65 DEG C of baking oven inner drying 4 hours, then vacuumize drying, temperature controls 65 DEG C, negative pressure 0.lMPa, vacuum-drying 8 hours;
(10) pulverize: take out dry thing, the pulverizer be cooled with circulating water, by crushing material, is crossed 80 mesh sieves, is namely obtained lentinan.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111484567A (en) * | 2020-06-01 | 2020-08-04 | 枣庄学院 | Extraction and preparation method of polysaccharide in long red dates, polysaccharide and application |
| CN111743816A (en) * | 2019-03-29 | 2020-10-09 | 北京东方淼森生物科技有限公司 | Skin care product additive with anti-haze effect and industrial preparation method thereof |
| CN113876895A (en) * | 2021-11-11 | 2022-01-04 | 劲牌持正堂药业有限公司 | Preparation method and application of composite extract with hypoglycemic activity |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1861636A (en) * | 2005-05-10 | 2006-11-15 | 上海市农业科学院 | Process for half bionic extracting preparing hedgehogt fungus crude polysaccharose |
| CN102786606A (en) * | 2012-09-05 | 2012-11-21 | 龙海市颖欣农业科技有限公司 | Processing method of lentinan |
-
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- 2014-11-28 CN CN201410700171.5A patent/CN104403020A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1861636A (en) * | 2005-05-10 | 2006-11-15 | 上海市农业科学院 | Process for half bionic extracting preparing hedgehogt fungus crude polysaccharose |
| CN102786606A (en) * | 2012-09-05 | 2012-11-21 | 龙海市颖欣农业科技有限公司 | Processing method of lentinan |
Non-Patent Citations (3)
| Title |
|---|
| 于洪涛: "三种食用菌多糖分离纯化的研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》, no. 04, 15 April 2013 (2013-04-15) * |
| 李珺 等: "超滤膜技术在香菇多糖提取中的应用", 《北方园艺》, 31 December 2009 (2009-12-31) * |
| 田洪芸 等: "陶瓷膜超滤纯化香菇多糖及其相对分子质量的测定", 《山东农业科学》, vol. 45, no. 11, 31 December 2013 (2013-12-31) * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111743816A (en) * | 2019-03-29 | 2020-10-09 | 北京东方淼森生物科技有限公司 | Skin care product additive with anti-haze effect and industrial preparation method thereof |
| CN111484567A (en) * | 2020-06-01 | 2020-08-04 | 枣庄学院 | Extraction and preparation method of polysaccharide in long red dates, polysaccharide and application |
| CN113876895A (en) * | 2021-11-11 | 2022-01-04 | 劲牌持正堂药业有限公司 | Preparation method and application of composite extract with hypoglycemic activity |
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Application publication date: 20150311 |