CN103421126A - Method for extracting laminarin - Google Patents
Method for extracting laminarin Download PDFInfo
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- CN103421126A CN103421126A CN2013100849269A CN201310084926A CN103421126A CN 103421126 A CN103421126 A CN 103421126A CN 2013100849269 A CN2013100849269 A CN 2013100849269A CN 201310084926 A CN201310084926 A CN 201310084926A CN 103421126 A CN103421126 A CN 103421126A
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- laminarin
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- tangle
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Abstract
The invention discloses a method for extracting laminarin, which especially comprises the following steps: drying, crushing, filtering and then soaking into water after washing kelp, performing water extraction and ultrasonic extraction and then ethanol precipitation to obtain laminarin precipitates, and finally drying the precipitates to obtain coarse laminarin. The method has the benefits that the method for ultrasonic-assisted extraction of the laminarin improves the extraction rate of the laminarin, reduces the extraction time, and is simple, convenient and environmental-friendly; researches show that the biological activity of the laminarin extracted by the method is not reduced.
Description
Technical field
The present invention relates to a kind of method of extracting laminarin.
Background technology
Laminarin claims again seaweed gel, have antitumor, antiviral, antibiotic, eliminate free radical, antioxygenation.Can be widely used in daily-use sanitary articles for use, makeup and healthcare products and field of medicaments.
At present, the technical process of extracting Crude polysaccharides in sea-tangle mainly contains: fragmentation → lixiviate → precipitation → centrifugal → drying → crude product, wherein, lixiviate and precipitation are the committed steps that affects product yield, quality and economic benefit.The extracting method of traditional laminarin comprises: hot water extraction method, enzyme extraction method, alkali extraction method, and all there is certain defect in these extracting method.As: the temperature of water extraction will be controlled at 100 ℃, needs a large amount of energy expenditures and longer extraction time, is not suitable for industrial production; There is very large pollution in the method for acid extraction, need a large amount of acid while digesting sea-tangle simultaneously, thereby this extracting method just is applicable to else extraction research of laboratory-scale: alkali extraction method is the main method of present industrial abstract laminarin, the benefit of the method is simple to operate, digestion thoroughly, the sea-tangle of equal in quality can be extracted and be obtained more laminarin, but there is very large pollution in this extracting method, thereby industrial production is subject to certain restrictions, and the extraction difficulty in the sea-tangle later stage of this disposal methods is larger.
Summary of the invention
Given this, the object of the present invention is to provide a kind of method of extracting laminarin, with existing seriously polluted, the problem that extraction time is long of the extracting method that solves laminarin in prior art.
To achieve these goals, the invention provides a kind of method of extracting laminarin, comprise the steps:
A, sea-tangle is cleaned and to dry after, be ground into Kelp Powder, sieving for standby;
B, the Kelp Powder of preparing in the A step is immersed in water, at 60 ~ 80 ℃ of lower ultrasonic-leaching 15 ~ 60min;
After C, the ultrasonic-leaching in the B step finish, heat water to 85 ~ 95 ℃, lixiviate 3 ~ 5h, obtain vat liquor;
D, the vat liquor in the C step is carried out to centrifugation, by the centrifugal waste residue gone out recentrifuge after washing, merge the resulting supernatant liquor of two times centrifugal, add the ethanol that massfraction is 95% in described supernatant liquor, standing 8 ~ 12h, obtain being insoluble to the laminarin precipitation of ethanol;
E, the laminarin that obtains in D step precipitation is carried out to drying, obtain the laminarin product.
Further, in described A step, be that Kelp Powder is crossed to 30 ~ 50 mesh sieves.
Further, is controlling solid-to-liquid ratio the ratio that this solid-to-liquid ratio of 25 ~ 50(is solid masses and liquid volume in described B step?), controlling ultrasonic power is 600 ~ 1000W, and ultrasonic time is 50 ~ 70min, and the water extraction temperature is 85 ~ 95 ℃, and the time is 3 ~ 5h.
Further, in described D step, the dosage of described ethanol is 2 ~ 4 times of supernatant liquor volume.
Further, in described D step, the rotating speed of controlling whizzer is 3500 ~ 4500 r/min, and centrifugation time is 10 ~ 20min.
Further, in described E step, dry mode be warm air drying and vacuum lyophilization in a kind of.
Further, the temperature of described warm air drying is 60 ℃, and the temperature of described vacuum lyophilization is-40 ℃.
The invention has the advantages that: the method for ultrasonic-assisted extraction laminarin has improved the extraction yield of laminarin, saved extraction time, simple and convenient extraction, environmental protection, and studies show that the biological activity of the laminarin that this method is extracted does not reduce.
Embodiment
Following examples are described in detail technical scheme of the present invention, but the present invention is not restricted to this embodiment.In order to make the public have thoroughly and understand the present invention, in the following preferred embodiment of the present invention, describe concrete details in detail.
Embodiment 1
A kind of method of extracting laminarin, comprise the steps:
A, sea-tangle is cleaned and to dry after, be ground into Kelp Powder, cross 40 mesh sieves standby;
B, take the Kelp Powder 20g prepared in the A step, be immersed in water, at 70 ℃ of lower ultrasonic-leaching 30min;
After C, the ultrasonic-leaching in the B step finish, heat water to 90 ℃, lixiviate 4h, obtain vat liquor;
D, the vat liquor in the C step is carried out to centrifugation 15min, the centrifugal waste residue gone out recentrifuge after washing is separated to 15min, centrifuge speed while controlling the two times centrifugal separation is 4000r/m, merge two times centrifugal resulting separation supernatant liquor, add the ethanol that 3 times of massfractions to the supernatant liquor volume are 95% in described supernatant liquor, standing 8h, obtain being insoluble to the laminarin precipitation of ethanol;
E, the laminarin that obtains in D step precipitation is placed in to air dry oven, carries out drying under 60 ℃, obtain the laminarin product.
Embodiment 2
A kind of method of extracting laminarin, comprise the steps:
A, sea-tangle is cleaned and to dry after, be ground into Kelp Powder, cross 30 mesh sieves standby;
B, take the Kelp Powder 10g prepared in the A step, be immersed in water, at 60 ℃ of lower ultrasonic-leaching 60min;
After C, the ultrasonic-leaching in the B step finish, heat water to 85 ℃, lixiviate 5h, obtain vat liquor;
D, the vat liquor in the C step is carried out to centrifugation 20min, the centrifugal waste residue gone out recentrifuge after washing is separated to 20min, centrifuge speed while controlling the two times centrifugal separation is 3500r/m, merge two times centrifugal resulting separation supernatant liquor, add the ethanol that 2 times of massfractions to the supernatant liquor volume are 95% in described supernatant liquor, standing 10h, obtain being insoluble to the laminarin precipitation of ethanol;
E, the laminarin that obtains in D step precipitation is placed in to lyophilizer, carries out vacuum lyophilization under-40 ℃, obtain the laminarin product.
Embodiment 3
A kind of method of extracting laminarin, comprise the steps:
A, sea-tangle is cleaned and to dry after, be ground into Kelp Powder, cross 50 mesh sieves standby;
B, take the Kelp Powder 30g prepared in the A step, be immersed in water, at 80 ℃ of lower ultrasonic-leaching 15min;
After C, the ultrasonic-leaching in the B step finish, heat water to 95 ℃, lixiviate 3h, obtain vat liquor;
D, the vat liquor in the C step is carried out to centrifugation 10min, the centrifugal waste residue gone out recentrifuge after washing is separated to 10min, centrifuge speed while controlling the two times centrifugal separation is 4500r/m, merge two times centrifugal resulting separation supernatant liquor, add the ethanol that 4 times of massfractions to the supernatant liquor volume are 95% in described supernatant liquor, standing 12h, obtain being insoluble to the laminarin precipitation of ethanol;
E, the laminarin that obtains in D step precipitation is placed in to air dry oven, carries out drying under 60 ℃, obtain the laminarin product.
Embodiment 4
A kind of method of extracting laminarin, comprise the steps:
A, sea-tangle is cleaned and to dry after, be ground into Kelp Powder, cross 40 mesh sieves standby;
B, take the Kelp Powder 25g prepared in the A step, be immersed in water, at 65 ℃ of lower ultrasonic-leaching 30min;
After C, the ultrasonic-leaching in the B step finish, heat water to 90 ℃, lixiviate 4h, obtain vat liquor;
D, the vat liquor in the C step is carried out to centrifugation 15min, the centrifugal waste residue gone out recentrifuge after washing is separated to 15min, centrifuge speed while controlling the two times centrifugal separation is 4000r/m, merge two times centrifugal resulting separation supernatant liquor, add the ethanol that 2.5 times of massfractions to the supernatant liquor volume are 95% in described supernatant liquor, standing 9h, obtain being insoluble to the laminarin precipitation of ethanol;
E, the laminarin that obtains in D step precipitation is placed in to air dry oven, carries out drying under 60 ℃, obtain the laminarin product.
Embodiment 5
A kind of method of extracting laminarin, comprise the steps:
A, sea-tangle is cleaned and to dry after, be ground into Kelp Powder, cross 40 mesh sieves standby;
B, take the Kelp Powder 40g prepared in the A step, be immersed in water, at 70 ℃ of lower ultrasonic-leaching 30min;
After C, the ultrasonic-leaching in the B step finish, heat water to 90 ℃, lixiviate 4h, obtain vat liquor;
D, the vat liquor in the C step is carried out to centrifugation 20min, the centrifugal waste residue gone out recentrifuge after washing is separated to 20min, centrifuge speed while controlling the two times centrifugal separation is 4000r/m, merge two times centrifugal resulting separation supernatant liquor, add the ethanol that 3 times of massfractions to the supernatant liquor volume are 95% in described supernatant liquor, standing 8h, obtain being insoluble to the laminarin precipitation of ethanol;
E, the laminarin that obtains in D step precipitation is placed in to lyophilizer, carries out drying under-40 ℃, obtain the laminarin product.
Embodiment 6
The method of ultrasonic-assisted extraction fucoidin, its step is as follows:
Get 10 g brown alga powder with 1: 50 soaked overnight of solid-liquid ratio, carry out respectively colloidal mill and the ultrasonic-assisted extraction of colloidal mill not, to do contrast, extracting solution is centrifugal, go supernatant liquid to add appropriate massfraction 2% calcium chloride solution, 37 ℃ of constant temperature 24 h, centrifugation goes out supernatant liquid, adds ethanol to 20% of total solution, centrifugal, in the clear liquid of upper strata, add ethanol to 60% of total solution, centrifugal, will be deposited in-40 ℃ of lyophilizes and obtain fucoidin.
In sum, it is only preferred embodiment of the present invention, not be used for limiting scope of the invention process, all equalizations of doing according to the described shape of the claims in the present invention scope, structure, feature and spirit change and modify, and all should be included in claim scope of the present invention.
Claims (6)
1. a method of extracting laminarin, is characterized in that, comprises the steps:
A, sea-tangle is cleaned and to dry after, be ground into Kelp Powder, cross after 30 ~ 50 mesh sieves standby;
B, the Kelp Powder of preparing in the A step is immersed in water, at 60 ~ 80 ℃ of lower ultrasonic-leaching 15 ~ 60min;
After C, the ultrasonic-leaching in the B step finish, heat water to 85 ~ 95 ℃, lixiviate 3 ~ 5h, obtain vat liquor;
D, the vat liquor in the C step is carried out to centrifugation, by the centrifugal waste residue gone out recentrifuge after washing, merge the resulting supernatant liquor of two times centrifugal, add the ethanol that massfraction is 95% in described supernatant liquor, standing 8 ~ 12h, obtain being insoluble to the laminarin precipitation of ethanol;
E, the laminarin that obtains in D step precipitation is carried out to drying, obtain the laminarin product.
2. the method for polysaccharide in extraction according to claim 1 sea-tangle, it is characterized in that, in described B step, is controlling solid-to-liquid ratio the ratio that this solid-to-liquid ratio of 25 ~ 50(is solid masses and liquid volume?), controlling ultrasonic power is 600 ~ 1000W, ultrasonic time is 50 ~ 70min, and the water extraction temperature is 85 ~ 95 ℃, and the time is 3 ~ 5h.
3. the method for polysaccharide in extraction sea-tangle according to claim 1, is characterized in that, in described D step, the dosage of described ethanol is 2 ~ 4 times of supernatant liquor volume.
4. the method for polysaccharide in extraction sea-tangle according to claim 1, is characterized in that, in described D step, the rotating speed of controlling whizzer is 3500 ~ 4500 r/min, and centrifugation time is 10 ~ 20min.
5. the method for polysaccharide in extraction according to claim 1 sea-tangle, is characterized in that, in described E step, dry mode be warm air drying and vacuum lyophilization in a kind of.
6. the method for polysaccharide in extraction sea-tangle according to claim 6, is characterized in that, the temperature of described warm air drying is 60 ℃, and the temperature of described vacuum lyophilization is-40 ℃.
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Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103755831A (en) * | 2014-01-22 | 2014-04-30 | 山东大学(威海) | Method for coproducing fucoidan and seaweed fertilizer |
CN103936875A (en) * | 2014-04-18 | 2014-07-23 | 广西还珠海洋生物科技有限公司 | Method for extracting laminarin from kelp |
CN104403022A (en) * | 2014-12-19 | 2015-03-11 | 桂林市和胤祥新型材料有限公司 | Preparation method of laminarin |
CN104710541A (en) * | 2015-03-31 | 2015-06-17 | 广西还珠海洋生物科技有限公司 | Method for preparing laminarin from kelp |
CN105294873A (en) * | 2015-10-24 | 2016-02-03 | 山东好当家海洋发展股份有限公司 | Extraction method for laminarin |
CN106072086A (en) * | 2016-06-22 | 2016-11-09 | 福州大学 | A kind of seaweed polyose product of similar sago and preparation method thereof |
CN106387733A (en) * | 2016-09-06 | 2017-02-15 | 苏州大学 | Fucoidan effervescent tablets and preparation method thereof |
CN107135829A (en) * | 2017-05-05 | 2017-09-08 | 宁波大学 | A kind of brown alga extract for reducing fruit and vegetable residual pesticide and its application |
CN108703182A (en) * | 2018-04-25 | 2018-10-26 | 福建亿达食品有限公司 | A kind of EGG YOLK SHORTCAKE formula and preparation method thereof with laminarin |
CN109776691A (en) * | 2018-12-28 | 2019-05-21 | 福建大昌生物科技实业有限公司 | A kind of novel processing technique for kelp |
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US20070087996A1 (en) * | 2005-10-18 | 2007-04-19 | Hideaki Hagiwara | Method of extracting fucoidan |
CN101074246A (en) * | 2006-09-21 | 2007-11-21 | 寻山集团有限公司 | Production and use for algin oligose |
CN101134783A (en) * | 2007-10-19 | 2008-03-05 | 大连工业大学 | Method for preparing sea-tangle polysaccharide |
CN102274247A (en) * | 2011-07-19 | 2011-12-14 | 南通大学 | Laminaria polysaccharide japonica capsules and preparation method and application thereof |
CN102690367A (en) * | 2012-06-28 | 2012-09-26 | 合肥工业大学 | Preparation method of anti-atherosclerosis active laminarins |
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2013
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Patent Citations (5)
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US20070087996A1 (en) * | 2005-10-18 | 2007-04-19 | Hideaki Hagiwara | Method of extracting fucoidan |
CN101074246A (en) * | 2006-09-21 | 2007-11-21 | 寻山集团有限公司 | Production and use for algin oligose |
CN101134783A (en) * | 2007-10-19 | 2008-03-05 | 大连工业大学 | Method for preparing sea-tangle polysaccharide |
CN102274247A (en) * | 2011-07-19 | 2011-12-14 | 南通大学 | Laminaria polysaccharide japonica capsules and preparation method and application thereof |
CN102690367A (en) * | 2012-06-28 | 2012-09-26 | 合肥工业大学 | Preparation method of anti-atherosclerosis active laminarins |
Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103755831A (en) * | 2014-01-22 | 2014-04-30 | 山东大学(威海) | Method for coproducing fucoidan and seaweed fertilizer |
CN103755831B (en) * | 2014-01-22 | 2015-10-21 | 山东大学(威海) | The method of coproduction fucoidan and seaweed fertilizer |
CN103936875A (en) * | 2014-04-18 | 2014-07-23 | 广西还珠海洋生物科技有限公司 | Method for extracting laminarin from kelp |
CN104403022A (en) * | 2014-12-19 | 2015-03-11 | 桂林市和胤祥新型材料有限公司 | Preparation method of laminarin |
CN104710541A (en) * | 2015-03-31 | 2015-06-17 | 广西还珠海洋生物科技有限公司 | Method for preparing laminarin from kelp |
CN105294873A (en) * | 2015-10-24 | 2016-02-03 | 山东好当家海洋发展股份有限公司 | Extraction method for laminarin |
CN106072086A (en) * | 2016-06-22 | 2016-11-09 | 福州大学 | A kind of seaweed polyose product of similar sago and preparation method thereof |
CN106387733A (en) * | 2016-09-06 | 2017-02-15 | 苏州大学 | Fucoidan effervescent tablets and preparation method thereof |
CN107135829A (en) * | 2017-05-05 | 2017-09-08 | 宁波大学 | A kind of brown alga extract for reducing fruit and vegetable residual pesticide and its application |
CN107135829B (en) * | 2017-05-05 | 2020-12-04 | 宁波大学 | Brown algae extract for reducing fruit and vegetable pesticide residues and application thereof |
CN108703182A (en) * | 2018-04-25 | 2018-10-26 | 福建亿达食品有限公司 | A kind of EGG YOLK SHORTCAKE formula and preparation method thereof with laminarin |
CN109776691A (en) * | 2018-12-28 | 2019-05-21 | 福建大昌生物科技实业有限公司 | A kind of novel processing technique for kelp |
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Application publication date: 20131204 |