CN104672344A - Enteromorpha functional oligosaccharide zinc and preparation method thereof - Google Patents
Enteromorpha functional oligosaccharide zinc and preparation method thereof Download PDFInfo
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Abstract
The invention discloses enteromorpha functional oligosaccharide zinc and a preparation method thereof. The principle that an oligosaccharide compound can form a stable complex with metal salt is adopted, after the enteromorpha functional oligosaccharide is extracted by adopting the enteromorpha as raw materials, deproteinization and polysaccharide removal are carried out, and then the enteromorpha functional oligosaccharide is compounded with Zn<2+> to prepare novel organic zinc salt which has biological activity and is easily absorbed by a human body. The prepared enteromorpha functional oligosaccharide zinc integrates the healthcare functions of the functional oligosaccharide and trace element zinc and has the characteristics of non-toxicity, no pollution, good water solubility, good biological effectiveness and high conversion rate in a biological pH range; the equipment is simple, the cost is low, the operation is easy, a novel resource can be developed for supplementing zinc to the human body, and the economical additional value of the enteromorpha resource can be greatly increased by virtue of the high-value development and application.
Description
Technical field
The invention belongs to medicine, field of health care products, be specifically related to a kind of Enteromorpha functional oligosaccharide zinc and preparation method thereof.
Background technology
Enteromorpha is Chlorophyta Ulvaceae Enteromorpha, and being commonly called as " Ulva lactuca L. ", " green laver ", is important economical alga, mostly is wild algae kind, is distributed widely in the Shi Zhaozhong of river mouth and middle tide band.China's wild Enteromorpha resource is very abundant, and all there is distribution in such as the marine sites such as Shandong, Jiangsu, Zhejiang, Fujian, coastland.Record in Compendium of Material Medica, Enteromorpha " burn last nasal insufflation and stop bleeding from five sense organs or subcutaneous tissue, soup leaching is smash deposited the back of the hand and swollen and ache ".Correlative study finds, Enteromorpha contains the nutritive ingredient of multiple needed by human, and the feature of its high protein, high dietary-fiber, lower fat, low in calories, rich in mineral substances and VITAMIN, becomes the desirable feedstock of natural nutrient food.
Enteromorpha growth and breeding is very competent, and according to incompletely statistics, the output of the annual Enteromorpha of current ALONG COASTAL FUJIAN can reach more than 100,000 tons.Meanwhile, due to seawater eutrophication, global warming in recent years, make Enteromorpha be break out formula growth, even cause the generation of " green tide ", have a strong impact on the development of marine ecology and coastal tourism.The Enteromorpha of cleaned disembarkation, is used as garbage loading embeading or burning more, and this not only causes the waste of large number of biological resource, also pollutes ecotope.Therefore, carry out the high-valued development and utilization research of Enteromorpha resource, solve sudden green damp disaster in time, have important practical significance.
Oligosaccharides, also known as " oligose ", is the carbohydrate general name that 2-10 monose is combined into.Research finds, many oligosaccharides have the superperformances such as low in calories, stable, nontoxic, and can improving immunity of organisms, the diabetes-alleviating state of an illness, promote bifidus bacillus propagation, suppress the growth of enteron aisle spoilage organism, improve enteric microorganism environment etc. in play important function.Zinc is that human body and animal body are survived one of required important trace element, it is the important composition composition of more than 100 kind of enzyme in human body, it also plays very important effect in regulate gene expression, adjustment immunity of organism, cell proliferation and differentiation, body growth and metabolism etc., but because human body is not easy to absorb inorganic zinc salt, and the four generations zinc supplementation product existed in the market is owing to there being the side effect of stimulating intestine and stomach, or digestibility is low or high cost is difficult to reasons such as popularizing, be not well positioned to meet the demand of human body zinc supplementation.
For the above-mentioned weak point of zinc supplementation product, the present invention take Enteromorpha as raw material, novel organic zinc salt---the functional oligosaccharide zinc of a kind of functional oligosaccharide and zinc formation is prepared based on metal complex principle, it not only has the double health function of functional oligosaccharide and trace element zinc, and the bioavailability of human body to zinc can be improved, have potential health care, medical treatment and pharmaceutical use, market application foreground is wide; Simultaneously, the present invention rationally can effectively fully utilize Enteromorpha resource, develop high-valued deep processed product, improve its commodity value and economic value added, walk out the predicament that Enteromorpha is undersold as raw material or is directly used as offal treatment, for the minimizing wasting of resources and environmental pollution, improve the economic benefit of oceanic resources, social benefit and ecological benefits and have important practical significance.
Summary of the invention
The object of the present invention is to provide a kind of Enteromorpha functional oligosaccharide zinc and preparation method thereof, it is on the basis of comprehensive utilization Enteromorpha Resource Access Enteromorpha functional oligosaccharide, Enteromorpha functional oligosaccharide zinc is prepared by metal complex principle, this product is compared with inorganic zinc, biological effectiveness is high, not only can be used as the reinforcer of zinc element in food and animal-feed, can also provide the Enteromorpha functional oligosaccharide with physiological regulation activity simultaneously, make it can play respective physiologically active, have again a synergistic effect.
For achieving the above object, the present invention adopts following technical scheme:
A kind of Enteromorpha functional oligosaccharide zinc is by the Enteromorpha functional oligosaccharide extracted in Enteromorpha and Zn
2+the organic zinc salt that complexing is formed.
The preparation method of described Enteromorpha functional oligosaccharide zinc comprises the extraction of Enteromorpha functional oligosaccharide, deproteinated, Polysaccharide removing, metal complex legal system for the step of Enteromorpha functional oligosaccharide zinc; Its concrete steps are as follows:
1) extraction of Enteromorpha functional oligosaccharide: the Enteromorpha powder getting drying, pulverizing, excessively 60-80 mesh sieve, volume ratio 1:15-40 adds the ethanolic soln infiltration 30-60min that mass concentration is 30%-80% by weight, then in 30-60 DEG C, supersound extraction 2 times under 100-500 W, each 30-90min, united extraction liquid, suction filtration, filtrate reduced in volume is to 5% of original volume;
2) deproteinated: adopt sevage method, by propyl carbinol and chloroform by volume 1:4 mix, join in step 1) gained extracting solution, centrifugal after violent jolting 20min, remove the denatured protein of water layer and solution layer intersection; Repeat this operation until denatured protein removes completely;
3) Polysaccharide removing: adopt alcohol deposition method, by the extracting solution concentrated by rotary evaporation after deproteinated to 5% of original volume, then 1:3-9 adds the ethanol that mass concentration is 95% by volume, the refrigerator putting into 0-10 DEG C after stirring leaves standstill 24 h, gets supernatant liquor concentrating under reduced pressure, pressed powder that lyophilize obtains Enteromorpha functional oligosaccharide extract;
4) metal complex legal system is for Enteromorpha functional oligosaccharide zinc: in the pressed powder of step 3) gained Enteromorpha functional oligosaccharide extract, volume ratio 1:8-15 adds the ethanolic soln that mass concentration is 10%-50% by weight, make it be mixed with Enteromorpha functional oligosaccharide sample liquid that concentration is 0.5-5.0 mg/mL, then the citric acid of food grade or sodium carbonate are joined in Enteromorpha functional oligosaccharide sample liquid, its pH is regulated to be 6.0-11.0, and slowly add the acetic acid zinc solution or solution of zinc sulfate that concentration is 5.0-15.0mg/mL under agitation, complex reaction 30-60 min, reaction terminate after under 3500 × g centrifugal 30 min, collect the throw out obtained, washing is extremely without Free Zinc, described Enteromorpha functional oligosaccharide zinc finished product is obtained again through lyophilize.
remarkable advantage of the present invention is:the present invention take Enteromorpha as raw material, adopts ultrasonic-assisted extraction method to extract Enteromorpha functional oligosaccharide, and the feature utilizing oligosaccharides can form stable comple with metal-salt prepares the Enteromorpha functional oligosaccharide zinc with physiologically active.Present device is simple, cost is low, easy to operate, and obtained enteromorpha oligosaccharide zinc is compared with inorganic zinc, and bioavailability is high, not only can be used as the zinc source in food and animal-feed, can also provide and there is bioactive oligosaccharides, make it can play respective physiologically active, again there is synergistic effect
Simultaneously, the comprehensive utilization Enteromorpha resource that the present invention's energy is effective and reasonable, improve its commodity value and economic value added, break through Enteromorpha raw material price cheap or be directly taken as the limitation of offal treatment, for the minimizing wasting of resources and environmental pollution, improve the economic benefit of oceanic resources, social benefit and ecological benefits and have important practical significance.
Embodiment
A preparation method for Enteromorpha functional oligosaccharide zinc, its concrete steps are as follows:
1) extraction of Enteromorpha functional oligosaccharide: the Enteromorpha powder getting drying, pulverizing, excessively 60-80 mesh sieve, volume ratio 1:15-40 adds the ethanolic soln infiltration 30-60min that mass concentration is 30%-80% by weight, then in 30-60 DEG C, supersound extraction 2 times under 100-500 W, each 30-90min, united extraction liquid, suction filtration, filtrate reduced in volume is to 5% of original volume;
2) deproteinated: by propyl carbinol and chloroform by volume 1:4 mix, join in step 1) gained extracting solution, centrifugal after violent jolting 20min, the denatured protein of removing water layer and solution layer intersection; Repeat this operation until denatured protein is removed completely;
3) Polysaccharide removing: by the extracting solution concentrated by rotary evaporation after deproteinated to 5% of original volume, then 1:3-9 adds the ethanol that mass concentration is 95% by volume, the refrigerator putting into 0-10 DEG C after stirring leaves standstill 24 h, gets supernatant liquor concentrating under reduced pressure, pressed powder that lyophilize obtains Enteromorpha functional oligosaccharide extract;
4) metal complex legal system is for Enteromorpha functional oligosaccharide zinc: in the pressed powder of step 3) gained Enteromorpha functional oligosaccharide extract, volume ratio 1:8-15 adds the ethanolic soln that mass concentration is 10%-50% by weight, make it be mixed with Enteromorpha functional oligosaccharide sample liquid that concentration is 0.5-5.0 mg/mL, then the citric acid of food grade or sodium carbonate are joined in Enteromorpha functional oligosaccharide sample liquid, its pH is regulated to be 6.0-11.0, and slowly add the acetic acid zinc solution or solution of zinc sulfate that concentration is 5.0-15.0mg/mL under agitation, complex reaction 30-60 min, reaction terminate after under 3500 × g centrifugal 30 min, collect the throw out obtained, washing is extremely without Free Zinc, the powder of described Enteromorpha functional oligosaccharide zinc is obtained again through lyophilize.
More being convenient to make content of the present invention understand, below in conjunction with embodiment, technical solutions according to the invention are described further, but the present invention being not limited only to this.
Embodiment 1
1) extraction of Enteromorpha functional oligosaccharide: Enteromorpha powder 10 kg getting drying, pulverizing, excessively 80 mesh sieves, volume ratio 1:15 adds the ethanolic soln infiltration 30min that mass concentration is 80% by weight, then in 30 DEG C, supersound extraction 2 times under 500 W, each 30min, united extraction liquid, suction filtration, filtrate reduced in volume is to 5% of original volume;
2) deproteinated: by propyl carbinol and chloroform by volume 1:4 mix, join in step 1) gained extracting solution, centrifugal after violent jolting 20min, the denatured protein of removing water layer and solution layer intersection; Repeat this operation until denatured protein is removed completely;
3) Polysaccharide removing: by the extracting solution concentrated by rotary evaporation after deproteinated to 5% of original volume, then 1:3 adds the ethanol that mass concentration is 95% by volume, the refrigerator putting into 10 DEG C after stirring leaves standstill 24 h, gets supernatant liquor concentrating under reduced pressure, pressed powder that lyophilize obtains Enteromorpha functional oligosaccharide extract;
4) metal complex legal system is for Enteromorpha functional oligosaccharide zinc: the pressed powder 100g getting step 3) gained Enteromorpha functional oligosaccharide extract, volume ratio 1:8 adds the ethanolic soln that mass concentration is 50% by weight, make it be mixed with Enteromorpha functional oligosaccharide sample liquid that concentration is 5.0 mg/mL, then the citric acid of food grade is joined in Enteromorpha functional oligosaccharide sample liquid, its pH is regulated to be 11.0, and slowly add the acetic acid zinc solution that concentration is 15.0mg/mL under agitation, complex reaction 60 min, reaction terminate after under 3500 × g centrifugal 30 min, collect the throw out obtained, washing is extremely without Free Zinc, the powder of described Enteromorpha functional oligosaccharide zinc is obtained again through lyophilize.
Embodiment 2
1) extraction of Enteromorpha functional oligosaccharide: Enteromorpha powder 30 kg getting drying, pulverizing, excessively 60 mesh sieves, volume ratio 1:40 adds the ethanolic soln infiltration 60min that mass concentration is 30% by weight, then in 60 DEG C, supersound extraction 2 times under 100W, each 60min, united extraction liquid, suction filtration, filtrate reduced in volume is to 5% of original volume;
2) deproteinated: by propyl carbinol and chloroform by volume 1:4 mix, join in step 1) gained extracting solution, centrifugal after violent jolting 20min, the denatured protein of removing water layer and solution layer intersection; Repeat this operation until denatured protein is removed completely;
3) Polysaccharide removing: by the extracting solution concentrated by rotary evaporation after deproteinated to 5% of original volume, then 1:9 adds the ethanol that mass concentration is 95% by volume, the refrigerator putting into 3 DEG C after stirring leaves standstill 24 h, gets supernatant liquor concentrating under reduced pressure, pressed powder that lyophilize obtains Enteromorpha functional oligosaccharide extract;
4) metal complex legal system is for Enteromorpha functional oligosaccharide zinc: the pressed powder 500g getting step 3) gained Enteromorpha functional oligosaccharide extract, volume ratio 1:15 adds the ethanolic soln that mass concentration is 10%-50% by weight, make it be mixed with Enteromorpha functional oligosaccharide sample liquid that concentration is 0.5 mg/mL, then the citric acid of food grade is joined in Enteromorpha functional oligosaccharide sample liquid, its pH is regulated to be 7.0, and slowly add the acetic acid zinc solution that concentration is 5.0mg/mL under agitation, complex reaction 60 min, reaction terminate after under 3500 × g centrifugal 30 min, collect the throw out obtained, washing is extremely without Free Zinc, the powder of described Enteromorpha functional oligosaccharide zinc is obtained again through lyophilize.
Embodiment 3
1) extraction of Enteromorpha functional oligosaccharide: Enteromorpha powder 20 kg getting drying, pulverizing, excessively 80 mesh sieves, volume ratio 1:20 adds the ethanolic soln infiltration 50min that mass concentration is 60% by weight, then in 40 DEG C, supersound extraction 2 times under 250 W, each 90min, united extraction liquid, suction filtration, filtrate reduced in volume is to 5% of original volume;
2) deproteinated: by propyl carbinol and chloroform by volume 1:4 mix, join in step 1) gained extracting solution, centrifugal after violent jolting 20min, the denatured protein of removing water layer and solution layer intersection; Repeat this operation until denatured protein is removed completely;
3) Polysaccharide removing: by the extracting solution concentrated by rotary evaporation after deproteinated to 5% of original volume, then 1:6 adds the ethanol that mass concentration is 95% by volume, the refrigerator putting into 6 DEG C after stirring leaves standstill 24 h, gets supernatant liquor concentrating under reduced pressure, pressed powder that lyophilize obtains Enteromorpha functional oligosaccharide extract;
4) metal complex legal system is for Enteromorpha functional oligosaccharide zinc: the pressed powder 200g getting step 3) gained Enteromorpha functional oligosaccharide extract, volume ratio 1:10 adds the ethanolic soln that mass concentration is 30% by weight, make it be mixed with Enteromorpha functional oligosaccharide sample liquid that concentration is 1.0 mg/mL, then the sodium carbonate of food grade is joined in Enteromorpha functional oligosaccharide sample liquid, its pH is regulated to be 8.0, and slowly add the solution of zinc sulfate that concentration is 10.0mg/mL under agitation, complex reaction 50 min, reaction terminate after under 3500 × g centrifugal 30 min, collect the throw out obtained, washing is extremely without Free Zinc, the powder of described Enteromorpha functional oligosaccharide zinc is obtained again through lyophilize.
The present invention take Enteromorpha as raw material, ultrasonic-assisted extraction method is adopted to extract Enteromorpha functional oligosaccharide, and the feature utilizing oligosaccharides can form stable comple with metal-salt prepares the Enteromorpha functional oligosaccharide zinc with physiologically active, gained Enteromorpha functional oligosaccharide zinc integrates the nourishing function of functional oligosaccharide and trace element zinc, have in physiological pH range nontoxic, pollution-free, water-soluble good with biological effectiveness, the feature that transformation efficiency is high, not only can be used as the zinc source in food and animal-feed, can also provide and there is bioactive oligosaccharides, make it can play respective physiologically active, again there is synergistic effect, its equipment is simple simultaneously, cost is low, easy to operate.The comprehensive utilization Enteromorpha resource that the present invention's energy is effective and reasonable, improves its commodity value and economic value added, for the minimizing wasting of resources and environmental pollution, improves the economic benefit of oceanic resources, social benefit and ecological benefits and has important practical significance.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (9)
1. an Enteromorpha functional oligosaccharide zinc, is characterized in that: described functional oligosaccharide zinc is by the Enteromorpha functional oligosaccharide extracted in Enteromorpha and Zn
2+the organic zinc salt that complexing is formed.
2. a preparation method for Enteromorpha functional oligosaccharide zinc as claimed in claim 1, is characterized in that: comprise the extraction of Enteromorpha functional oligosaccharide, deproteinated, Polysaccharide removing, metal complex legal system for the step of Enteromorpha functional oligosaccharide zinc.
3. the preparation method of Enteromorpha functional oligosaccharide zinc according to claim 2, it is characterized in that: the extraction of described Enteromorpha functional oligosaccharide is the Enteromorpha powder getting drying, pulverizing, excessively 60-80 mesh sieve, volume ratio 1:15-40 adds the ethanolic soln infiltration 30-60min that mass concentration is 30%-80% by weight, then in 30-60 DEG C, supersound extraction 2 times under 100-500 W, each 30-90min, united extraction liquid, suction filtration, filtrate reduced in volume is to 5% of original volume.
4. the preparation method of Enteromorpha functional oligosaccharide zinc according to claim 2, it is characterized in that: described metal complex legal system is that the Enteromorpha functional oligosaccharide extract lyophilize after deproteination and polysaccharide is become pressed powder for Enteromorpha functional oligosaccharide zinc, then Enteromorpha functional oligosaccharide sample liquid is mixed with ethanolic soln, regulate pH, and slowly add zinc solution under agitation, it is made to carry out complex reaction, reaction terminates rear centrifugal, collect the throw out obtained, washing is to obtaining Enteromorpha functional oligosaccharide zinc finished product without after Free Zinc through lyophilize.
5. the preparation method of Enteromorpha functional oligosaccharide zinc according to claim 4, it is characterized in that: the pressed powder of Enteromorpha functional oligosaccharide extract used and the weightmeasurement ratio of ethanolic soln are 1:8-15, wherein, the mass concentration of ethanolic soln is 10%-50%.
6. the preparation method of Enteromorpha functional oligosaccharide zinc according to claim 4, is characterized in that: the concentration of described Enteromorpha functional oligosaccharide sample liquid is 0.5-5.0 mg/mL.
7. the preparation method of Enteromorpha functional oligosaccharide zinc according to claim 4, is characterized in that: the citric acid of food grade or sodium carbonate are joined in Enteromorpha functional oligosaccharide sample liquid, regulates its pH to be 6.0-11.0.
8. the preparation method of Enteromorpha functional oligosaccharide zinc according to claim 4, it is characterized in that: described zinc solution is acetic acid zinc solution or solution of zinc sulfate, strength of solution is 5.0-15.0mg/mL.
9. the preparation method of Enteromorpha functional oligosaccharide zinc according to claim 4, is characterized in that: the time of complex reaction is 30-60 min.
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Cited By (7)
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| CN105394351A (en) * | 2015-10-27 | 2016-03-16 | 南宁市泽威尔饲料有限责任公司 | Oligosaccharide chelated composite trace element mineral matter supplement and preparation method thereof |
| CN105542022A (en) * | 2015-12-17 | 2016-05-04 | 浙江工商大学 | Enteromorpha polysaccharide biological activity improving method |
| CN106538843A (en) * | 2016-09-30 | 2017-03-29 | 江西中创汇智智能科技有限公司 | A kind of method that utilization Enteromorpha manufactures trace mineral supplement |
| CN106674365A (en) * | 2016-10-21 | 2017-05-17 | 福建海兴保健食品有限公司 | Method for separating and purifying small molecule oligosaccharides from green algae |
| CN107118284A (en) * | 2017-06-02 | 2017-09-01 | 福建农林大学 | A kind of sulfated oligosaccharide zinc and preparation method thereof |
| CN109734761A (en) * | 2019-02-28 | 2019-05-10 | 福建农林大学 | A kind of preparation method and applications of Enteromorpha fucose complex compound |
| CN110713626A (en) * | 2019-10-14 | 2020-01-21 | 福建农林大学 | Preparation method of ulva oligosaccharide compound with auxiliary anti-tumor effect |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105394351A (en) * | 2015-10-27 | 2016-03-16 | 南宁市泽威尔饲料有限责任公司 | Oligosaccharide chelated composite trace element mineral matter supplement and preparation method thereof |
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| CN107118284A (en) * | 2017-06-02 | 2017-09-01 | 福建农林大学 | A kind of sulfated oligosaccharide zinc and preparation method thereof |
| CN107118284B (en) * | 2017-06-02 | 2019-05-03 | 福建农林大学 | A kind of sulfated oligosaccharide zinc and preparation method thereof |
| CN109734761A (en) * | 2019-02-28 | 2019-05-10 | 福建农林大学 | A kind of preparation method and applications of Enteromorpha fucose complex compound |
| CN110713626A (en) * | 2019-10-14 | 2020-01-21 | 福建农林大学 | Preparation method of ulva oligosaccharide compound with auxiliary anti-tumor effect |
| CN110713626B (en) * | 2019-10-14 | 2021-06-01 | 福建农林大学 | Preparation method of ulva oligosaccharide compound with auxiliary anti-tumor effect |
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