CN1313479C - Method for preparing holothurin from waste solution of sea cucumber processing - Google Patents
Method for preparing holothurin from waste solution of sea cucumber processing Download PDFInfo
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- CN1313479C CN1313479C CNB2005100441221A CN200510044122A CN1313479C CN 1313479 C CN1313479 C CN 1313479C CN B2005100441221 A CNB2005100441221 A CN B2005100441221A CN 200510044122 A CN200510044122 A CN 200510044122A CN 1313479 C CN1313479 C CN 1313479C
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Abstract
The present invention relates to a method for preparing the saponin of sea cucumbers by using a processing waste solution for sea cucumbers, which comprises the steps that firstly, the waste solution of the sea cucumbers is filtered; then, the filtering solution is precipitated, held and centrifuged with ethanol; centrifugal supernatant solutions are decompressed and concentrated to remove ethanol ingredients so as to obtain concentrated solutions; the solutions pass through a large hole adsorption resin column at the flowing speed of 1.5 to 2.0 BV/h, and then, water is used for washing through the same flowing speed so as to remove impurity ingredients, such as salinity, saccharide, pigment, etc.; then, 60 to 70% of the ethanol is used for eluting the saponin ingredients of the sea cucumbers adsorbed on the large hole adsorption resin column, eluting solutions are collected and concentrated to form a paste shape, and the eluting solutions are frozen and dried to prepare saponin dried products of the sea cucumbers. The process is mainly characterized in that the processing waste solution generated for the sea cucumbers can be used fully, and the waste solution is changed into valuable products, so that the saponin which is separated preserves perfect structures and effective bioactivity. The present invention has the advantages of simple operation, short production periods, low production cost, no pollution and high utility value of the products.
Description
Technical field
The present invention relates to a kind of processing method of utilizing the sea cucumber processing-waste to prepare the sea cucumber saponin.
Background technology
Since ancient times, sea cucumber is exactly one of precious eight product in sea, and it is under the jurisdiction of the Echinodermata Holothuroidea.In Ming Dynasty's " food book on Chinese herbal medicine ", point out that already sea cucumber has main invigorating premordial QI, grows the beneficial vital organs of the human body. and the many health-preserving functions such as deficient of dispelling.Along with the raising of living standards of the people and the enhancing of health care consciousness, the medical care effect of sea cucumber has obtained approval and application more and more widely, having formed with countries and regions such as China, Singapore, Hong Kong, Japan, Korea S, the U.S., Indonesia, Philippines simultaneously is the trade and the consumption market at center, some are the product consequentiality that starting material are developed with the sea cucumber, as holothurian oral liquid, sea cucumber peptide nourishing capsule, sea cucumber wine, freeze-drying sea cucumber etc.
Recent study finds that the main active ingredient in the sea cucumber is its secondary metabolite---the sea cucumber saponin, the sea cucumber saponin all has distribution in sea cucumber body wall corium reticular tissue, body cavity, interior glandular tube and internal organ, has multiple pharmacologically active activity, as antitumor action, raising immunizing power, anti-neovascularization, anticoagulation, promotion fibrinolysis, the formation of inhibition embolism, anti-inflammatory action (as sacroiliitis) and anti-radioactivity, and suppress hiv virus, hepatitis B virus, simple scar exanthema virus etc.; In addition, research finds that also the sea cucumber saponin has the antifungal efficacy of wide spectrum.At present, the scientific research institution of existing a lot of countries is devoted to the research and development based on the product of sea cucumber saponin.Japan has been walked in the prostatitis in the world in this field, and Japanese Bei Chuanshi utilizes the stichopus japonicus saponin to develop the product of treatment beriberi and tinea alba fungi resisting infection.Usually the method for extracting the sea cucumber saponin from sea cucumber is to adopt traditional organic solvent extractionprocess, these class methods are produced not only complex operation of sea cucumber saponin, to the equipment requirements height, use a large amount of organic solvents (as methyl alcohol) in the production process, contaminate environment, and the sea cucumber overall utilization rate is not high, after having extracted the sea cucumber saponin, other nutritional activities composition can not effectively utilize, and the sea cucumber resource has been caused serious waste.Because the restriction of above various reasons, at present, China is relatively backward in the research in this field, institute's development product only is confined to the processing of the thick product of sea cucumber, and saponin component residues in the processing-waste more in the course of processing, waste liquid can not get effective utilization, has caused the significant wastage of resource.
Summary of the invention
The present invention seeks to make full use of the waste liquid in the sea cucumber course of processing, a kind of processing method for preparing the sea cucumber saponin with the sea cucumber waste liquid is provided.
Present method is to utilize sea cucumber to send out the system waste liquid as extracting material, at first, the sea cucumber waste liquid is filtered, remove insoluble composition, then, filtrate is used ethanol sedimentation, leave standstill, centrifugal to remove the albumen in the filtrate, compositions such as mucopolysaccharide, again with centrifuged supernatant with common concentrating under reduced pressure technology concentrating under reduced pressure to remove alcohol component wherein, the gained concentrated solution, with the flow velocity of 1.5～2.0 times of column volumes (BV)/h by macroporous adsorptive resins, then water with same flow velocity wash-out to remove salinity wherein, carbohydrate, impurity components such as pigment are that 60～70% ethanol elutions are attracted to the sea cucumber saponin component on the macroporous adsorbent resin with concentration then, collect elutriant and be evaporated to the medicinal extract shape, lyophilize becomes sea cucumber saponin dry product.
The present invention makes full use of sea cucumber and sends out the waste liquid that is produced in the system process, utilize macroporous adsorbent resin to send out the system waste liquid and extract the sea cucumber saponin from sea cucumber, can make in the sea cucumber waste liquid 95% saponin obtain enrichment, make intact structure of isolating saponin and effective biological activity, experiment shows, separates the saponin component that obtains and have good biological effect from the sea cucumber waste liquid.The principal feature of this technology is the discarded liquid that can make full use of after sea cucumber sends out system, and simple to operate, with short production cycle, with high content of technology, production cost is low, and environmentally safe, product have high utility value.
Embodiment
1, sea cucumber sends out discarded liquid after the system and filters (perhaps centrifugal) and remove insoluble composition;
2, ethanol is added in the filtrate, and to make alcohol concn wherein be 20～25%, leave standstill more than 10 hours; If the alcohol concn in the filtrate surpasses 25%, will influence sea cucumber saponin extraction yield; If concentration is lower than 20%, albumen, mucopolysaccharide composition are removed not exclusively in the filtrate, stop up macroporous adsorptive resins easily.
3, ethanol sedimentation liquid is centrifugal, and 2500～3000r/min more than the 30min, collects supernatant liquor;
4, with the supernatant liquor concentrating under reduced pressure, temperature is controlled at 45～50 ℃ (in case saponin pyrohydrolysises), and the alcohol component of removing in the supernatant liquor gets concentrated solution; The strong and weak length that is connected the sugar chain on the main chain backbone with it of biological activity of discovering the sea cucumber saponin has confidential relation, during concentrating under reduced pressure such as temperature too high, can make part sugar chain hydrolytic cleavage, and the biologic activity of influence extraction gained saponin; Therefore, temperature remains on 45～50 ℃ of concentrating under reduced pressure the saponin structure in the supernatant liquor is remained intact.
5, the concentrated solution behind the concentrating under reduced pressure, by macroporous adsorptive resins, the sea cucumber saponin is adsorbed on the macroporous adsorbent resin with the flow velocity of 1.5～2.0BV/h; Flow velocity is too high, and sea cucumber saponin adsorption rate will be reduced; Flow velocity is low excessively, will increase extraction time.
6, then wash above-mentioned macroporous adsorptive resins with same flow velocity, to remove impurity components such as salinity residual in the macroporous adsorbent resin, carbohydrate, pigment with 4～6BV water;
7, then be 60～70% ethanol, the sea cucumber saponin component that is adsorbed on the macroporous resin eluted that collection elutriant concentrating under reduced pressure (temperature is controlled at 45～50 ℃) promptly gets medicinal extract shape sea cucumber saponin with concentration;
8, above-mentioned medicinal extract lyophilize is got sea cucumber saponin dry product.
Embodiment 1
The discarded liquid 5L centrifugal (rotating speed is at 2500r/min) that sea cucumber sends out after the system removes insolubles, supernatant liquor is with ethanol sedimentation and to make alcohol concn wherein be 25%, left standstill 10 hours, centrifugal above-mentioned precipitated liquid, rotating speed is at 2500r/min, centrifugal 45min, collect supernatant liquor, the supernatant liquor concentrating under reduced pressure is removed alcohol component, temperature is controlled at 45 ℃ during concentrating under reduced pressure, liquid 2L behind the concentrating under reduced pressure, with the flow velocity of 2BV/h by AB-8 type macroporous adsorptive resins (R35mm * H90mm), then wash above-mentioned macroporous adsorptive resins with the flow velocity of 2BV/h with 6BV water, then, the sea cucumber saponin component that is adsorbed on the macroporous adsorbent resin is eluted, collect elutriant concentrating under reduced pressure (temperature is controlled at 45 ℃) to the medicinal extract shape with 70% ethanol of 5BV, with medicinal extract-20 ℃ freezing, get sea cucumber saponin dry product with freeze drier-54 ℃ of following lyophilizes then.
Embodiment 2
Sea cucumber sends out the discarded liquid 5L multilayer filtered through gauze after the system, filtrate is with ethanol sedimentation and to make alcohol concn wherein be 25%, left standstill 12 hours, centrifugal above-mentioned precipitated liquid, rotating speed is at 3000r/min, centrifugal 30min, collect supernatant liquor, the supernatant liquor concentrating under reduced pressure is removed alcohol component, temperature is controlled at 50 ℃ during concentrating under reduced pressure, the liquid 1.5L behind the concentrating under reduced pressure, with the flow velocity of 1.5BV/h by D101 type macroporous adsorptive resins (R30mm * H100mm), then wash above-mentioned macroporous adsorptive resins with same flow velocity with 6BV water, then, the sea cucumber saponin component that is adsorbed on the macroporous adsorbent resin is eluted, collect elutriant concentrating under reduced pressure (temperature is controlled at 50 ℃) to the medicinal extract shape with 60% ethanol of 6BV, with medicinal extract-20 ℃ freezing, get sea cucumber saponin dry product with freeze drier-54 ℃ of following lyophilizes then.
Claims (5)
1, a kind of processing method of utilizing the sea cucumber processing-waste to prepare the sea cucumber saponin, at first the sea cucumber waste liquid is filtered, filtrate is used ethanol sedimentation then, leave standstill, centrifugal, again the centrifuged supernatant concentrating under reduced pressure is removed alcohol component, get concentrated solution, flow velocity with 1.5～2.0 times of column volume/h passes through macroporous adsorptive resins, then water is with same flow velocity wash-out, then be attracted to the sea cucumber saponin component on the macroporous adsorbent resin and collect elutriant with ethanol elution and be evaporated to the medicinal extract shape, last lyophilize is a sea cucumber saponin dry product.
2, processing method as claimed in claim 1, when it is characterized in that above-mentioned filtrate is used ethanol sedimentation, should make alcohol concn wherein is 20～25%.
3, processing method as claimed in claim 1 is characterized in that the alcohol concn that above-mentioned wash-out is used is 60～70%.
4, processing method as claimed in claim 1 is characterized in that the temperature in the above-mentioned concentrating under reduced pressure is controlled at 45～50 ℃.
5, processing method as claimed in claim 1 is characterized in that above-mentioned macroporous adsorbent resin is D101 type or AB-8 type.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100441221A CN1313479C (en) | 2005-07-17 | 2005-07-17 | Method for preparing holothurin from waste solution of sea cucumber processing |
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| CNB2005100441221A CN1313479C (en) | 2005-07-17 | 2005-07-17 | Method for preparing holothurin from waste solution of sea cucumber processing |
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| CN1313479C true CN1313479C (en) | 2007-05-02 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101585873B (en) * | 2009-07-09 | 2012-10-03 | 大连水产学院 | Method for reclaiming protein and crude polysaccharide from waste sea cucumber processing liquid |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101375863B (en) * | 2008-09-17 | 2013-07-31 | 青岛佳日隆海洋食品有限公司 | Method for extracting polysaccharide and other multiple active components in boiling juice of trepang |
| CN102060905B (en) * | 2010-11-12 | 2012-10-10 | 山东省科学院生物研究所 | Technology method for preparing sea cucumber saponin Holotoxin A1 comparison product by utilizing fresh sea cucumber processing waste liquid |
| CN102512452B (en) * | 2011-11-29 | 2013-08-28 | 山东好当家海洋发展股份有限公司 | Process method for preparing sea cucumber glycosides by using sea cucumber coelomic fluid |
| CN102406048B (en) * | 2011-11-29 | 2013-04-17 | 山东好当家海洋发展股份有限公司 | Method for preparing sea cucumber glycoprotein by using sea cucumber blanching solution |
| CN104262451B (en) * | 2014-10-24 | 2016-04-13 | 威海芝恩药业股份有限公司 | A kind of method extracting selenka from Holothurian machining waste liquid |
| CN104739868A (en) * | 2015-02-15 | 2015-07-01 | 大连工业大学 | Comprehensive utilization method for sea cucumber processing waste liquid |
| CN110590967A (en) * | 2019-08-27 | 2019-12-20 | 中国海洋大学 | Method for recovering organic matters rich in sea cucumber polysaccharide from sea cucumber blanching liquid |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2005063789A1 (en) * | 2003-12-31 | 2005-07-14 | Council Of Scientific & Industrial Research | Isolation of bivittoside d from sea cucumber and activity thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005063789A1 (en) * | 2003-12-31 | 2005-07-14 | Council Of Scientific & Industrial Research | Isolation of bivittoside d from sea cucumber and activity thereof |
Non-Patent Citations (3)
| Title |
|---|
| 海参皂苷研究进展 邹峥嵘等，中国海洋药物，第1期 2004 * |
| 海参的药理作用及临床研究进展 聂卫等，天津药学，第14卷第1期 2002 * |
| 海参的药理作用及临床研究进展 聂卫等，天津药学，第14卷第1期 2002;海参皂苷研究进展 邹峥嵘等，中国海洋药物，第1期 2004 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101585873B (en) * | 2009-07-09 | 2012-10-03 | 大连水产学院 | Method for reclaiming protein and crude polysaccharide from waste sea cucumber processing liquid |
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