CN106397620A - Novel carrageenan, preparation method and application thereof - Google Patents
Novel carrageenan, preparation method and application thereof Download PDFInfo
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- CN106397620A CN106397620A CN201610804175.7A CN201610804175A CN106397620A CN 106397620 A CN106397620 A CN 106397620A CN 201610804175 A CN201610804175 A CN 201610804175A CN 106397620 A CN106397620 A CN 106397620A
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- sargassum
- solution
- carrageenan
- glue
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- 229920001525 carrageenan Polymers 0.000 title claims abstract description 73
- 235000010418 carrageenan Nutrition 0.000 title claims abstract description 73
- 239000000679 carrageenan Substances 0.000 title claims abstract description 71
- 229940113118 carrageenan Drugs 0.000 title claims abstract description 71
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 235000013305 food Nutrition 0.000 claims abstract description 10
- 229920001577 copolymer Polymers 0.000 claims abstract description 7
- 238000012545 processing Methods 0.000 claims abstract description 3
- 241000195474 Sargassum Species 0.000 claims description 62
- 239000003292 glue Substances 0.000 claims description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 25
- 238000002604 ultrasonography Methods 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000000499 gel Substances 0.000 claims description 19
- 230000009514 concussion Effects 0.000 claims description 17
- IBZYPBGPOGJMBF-UHFFFAOYSA-N 3,6 anhydrogalactose Natural products CCC=CCC1C(CC(=O)NC(C(C)CC)C(O)=O)CCC1=O IBZYPBGPOGJMBF-UHFFFAOYSA-N 0.000 claims description 15
- WZYRMLAWNVOIEX-BGPJRJDNSA-N 3,6-anhydro-D-galactose Chemical compound O=C[C@H](O)[C@H]1OC[C@@H](O)[C@@H]1O WZYRMLAWNVOIEX-BGPJRJDNSA-N 0.000 claims description 15
- DCQFFOLNJVGHLW-UHFFFAOYSA-N 4'-Me ether-Punctatin+ Natural products O1C(O)C(O)C2OCC1C2O DCQFFOLNJVGHLW-UHFFFAOYSA-N 0.000 claims description 15
- WZYRMLAWNVOIEX-UHFFFAOYSA-N cinnamtannin B-2 Natural products O=CC(O)C1OCC(O)C1O WZYRMLAWNVOIEX-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 230000002255 enzymatic effect Effects 0.000 claims description 11
- 239000000284 extract Substances 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 150000002148 esters Chemical class 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 8
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 claims description 8
- 238000000108 ultra-filtration Methods 0.000 claims description 8
- 244000050510 Cunninghamia lanceolata Species 0.000 claims description 7
- 241000719329 Trentepohlia Species 0.000 claims description 7
- 159000000007 calcium salts Chemical class 0.000 claims description 7
- 239000000084 colloidal system Substances 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 238000010306 acid treatment Methods 0.000 claims description 5
- 239000012141 concentrate Substances 0.000 claims description 5
- 230000018044 dehydration Effects 0.000 claims description 5
- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 239000004744 fabric Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 108090000790 Enzymes Proteins 0.000 claims description 4
- 102000004190 Enzymes Human genes 0.000 claims description 4
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 4
- 238000000643 oven drying Methods 0.000 claims description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 4
- 230000004044 response Effects 0.000 claims description 4
- 108010059892 Cellulase Proteins 0.000 claims description 3
- 235000013361 beverage Nutrition 0.000 claims description 3
- 229940106157 cellulase Drugs 0.000 claims description 3
- 235000009508 confectionery Nutrition 0.000 claims description 3
- 235000013399 edible fruits Nutrition 0.000 claims description 3
- 238000007603 infrared drying Methods 0.000 claims description 3
- 235000015110 jellies Nutrition 0.000 claims description 3
- 239000008274 jelly Substances 0.000 claims description 3
- 235000013622 meat product Nutrition 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 235000013336 milk Nutrition 0.000 claims description 3
- 239000008267 milk Substances 0.000 claims description 3
- 210000004080 milk Anatomy 0.000 claims description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 108030004827 Galactose-6-sulfurylases Proteins 0.000 claims description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 2
- 229910052925 anhydrite Inorganic materials 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 229920002678 cellulose Polymers 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 229940088598 enzyme Drugs 0.000 claims description 2
- 238000005984 hydrogenation reaction Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 229920002492 poly(sulfone) Polymers 0.000 claims description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 2
- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 239000000920 calcium hydroxide Substances 0.000 claims 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims 1
- 241000195493 Cryptophyta Species 0.000 abstract description 5
- 239000011575 calcium Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052791 calcium Inorganic materials 0.000 abstract description 3
- 241001147462 Gigartinaceae Species 0.000 abstract 1
- 150000002256 galaktoses Chemical class 0.000 abstract 1
- 229910021653 sulphate ion Inorganic materials 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 12
- 238000004140 cleaning Methods 0.000 description 11
- 239000000047 product Substances 0.000 description 9
- 241001428166 Eucheuma Species 0.000 description 4
- 241001491613 Gigartina skottsbergii Species 0.000 description 4
- 241000940372 Eucheuma denticulatum Species 0.000 description 3
- 241001147486 Sarcothalia crispata Species 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 102000005701 Calcium-Binding Proteins Human genes 0.000 description 2
- 108010045403 Calcium-Binding Proteins Proteins 0.000 description 2
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000003995 emulsifying agent Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000000796 flavoring agent Substances 0.000 description 2
- 235000019634 flavors Nutrition 0.000 description 2
- 239000003349 gelling agent Substances 0.000 description 2
- 235000015243 ice cream Nutrition 0.000 description 2
- 239000008101 lactose Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 230000019635 sulfation Effects 0.000 description 2
- 238000005670 sulfation reaction Methods 0.000 description 2
- 239000000375 suspending agent Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002562 thickening agent Substances 0.000 description 2
- 241000206576 Chondrus Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- 108091005804 Peptidases Proteins 0.000 description 1
- 239000004365 Protease Substances 0.000 description 1
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 235000019462 natural additive Nutrition 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000006069 physical mixture Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 229920002397 thermoplastic olefin Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0036—Galactans; Derivatives thereof
- C08B37/0042—Carragenan or carragen, i.e. D-galactose and 3,6-anhydro-D-galactose, both partially sulfated, e.g. from red algae Chondrus crispus or Gigantia stellata; kappa-Carragenan; iota-Carragenan; lambda-Carragenan; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Sustainable Development (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention belongs to the technical field of food processing, and particularly relates to a novel carrageenan, a preparation method and the application thereof. The novel carrageenan is extracted from Gigartinaceae algae. The carrageenan comprises copolymers formed based on the covalent combination of 3, 6-dehydrated galactose and 3, 6-dehydrated galactose-2-sulphate at a molar ratio of 1-3:1. The prepared carrageenan is strong in capacity of binding calcium, strong in gel strength, good in water retention effect and good in solubility.
Description
Technical field
The invention belongs to food processing technology field is and in particular to a kind of new carrageenan and its preparation method and application.
Background technology
Carrageenan be a class extract from the marine red algas such as Eucheuma, Killeen, China fir Trentepohlia, Chondruses hydrophilic
Property colloid, is a kind of wide variety of natural additive for foodstuff.All carrageenans all contain by α -1,3 glycosidic bond and β -1,4 sugar
The galactose unit of the repetition that glycosidic bond is alternately formed by connecting, and generally all by sulfation to some extent.The type of carrageenan
Can be distinguished it is also possible to by extracting their Sargassum come area in a way by the degree of their sulfations and position
Point.Due to the difference of wherein sulfuric ester combining form, create 7 kinds of major type of carrageenans：κ-type, ι-type, λ-type, γ-
Type, ν-type, ξ-type, μ-type.Commercial production and using most be κ-type and ι-type carrageenan.Eucheuma is to extract κ-type
With the optimum feed stock of ι-type carrageenan, the extraction mainly from E. cottonii of wherein κ-type carrageenan, its 3,6- dehydration half
Lactose -2- sulfuric ester is generally below 10% with respect to the mol ratio content of 3,6- Anhydrogalactose., and this glue forms hard and crisp glue,
Water outlet is big, affects mouthfeel, and its solution temperature is high, and this all limits its application in some food；ι-type carrageenan is main
It is to extract from Eucheuma spinosum, its 3,6- Anhydrogalactose. -2- sulfuric ester contains with respect to the mol ratio of 3,6- Anhydrogalactose.
Amount is generally 80%-100%, and this glue forms soft and resilient glue, and water outlet is little, good in taste, and solution temperature is low, but its
Intensity is too low, and expensive, and this also makes it be difficult to extensively apply.In actual applications, use intensity and water-retaining property are often needed
Etc. property between κ-type and ι-type carrageenan carrageenan therebetween, κ-type and ι-type carrageenan mixing are often made by current people
With however, the simple composite of κ-type and ι-type carrageenan, operating procedure is cumbersome, and using effect needs repeatedly to be tested and gropes, can
Also perfect condition can not reached, and ι-type carrageenan price is more much higher than κ-type carrageenan, cost too high it is difficult to widely use.
Content of the invention
Invention broadly provides a kind of new carrageenan and its preparation method and application, the carrageenan of preparation is combined with calcium
Ability is strong, and gel strength is low, and Water-saving effect is good, and dissolubility is good.Its technical scheme is as follows：
A kind of new carrageenan, it extracts from Shan Zao section Sargassum, and described carrageenan comprises 3,6- Anhydrogalactose. and 3,6-
Anhydrogalactose. -2- sulfuric ester is with mol ratio as 1-3:1 covalently bound copolymer.
Preferably, described Shan Zao section Sargassum includes China fir Trentepohlia frond or the China fir Trentepohlia algae of mixing generation of gametophytic generation
Body.
A kind of preparation method of new carrageenan, comprises the following steps：
1) acid treatment：Shan Zao section Sargassum acid supplemented solution is processed in 20-40KHz low frequency ultrasound concussion；
2) wash：By step 1) gained Sargassum cleaned in 20-40KHz low frequency ultrasound with water, clean Sargassum drained；
3) alkali process or ferment treatment：To step 2) add in gained Sargassum aqueous slkali or enzymatic solution heating to be reacted,
Then 20-40KHz low frequency ultrasound concussion reaction；
4) carry glue：By step 3) gained Sargassum solution temperature is set to 80-95 DEG C, anti-in the concussion of 20-40KHz low frequency ultrasound
Should, extract glue；
5) filter：By step 4) filtration of gained Sargassum glue, obtain dilute glue；
6) concentrate cooling：Dilute glue is concentrated with ultrafiltration membrance filter, by the dense glue cooling obtaining；
7) gel：Add organic solvent or potassium salt soln or calcium salt soln to be precipitated in dense glue, form gel；
8) dehydrate：Gained gel ethanol solution is rinsed repeatedly, press dewatering, be dried after extracting moisture, obtain glue
Body；
9) pulverize and sieve：Colloid is pulverized, and crosses 80-120 eye mesh screen, obtain finished product carrageenan.
Preferably, step 1) in acid solution mass content be 0.01%-1%, preferably 0.02%-0.8%, Shan Zao section
Sargassum is 1 with the mass ratio of acid solution:5-20, process time is 0.5-2h, preferably 0.5-1.5h.
Preferably, step 2) in using ultrasonic cleaning equipment be cleaned by ultrasonic Sargassum, described ultrasonic cleaning equipment include operate
Case, net cage, agitating device, ultrasonic generator and mechanical hand, net cage is placed in control box, and agitating device, in net cage, surpasses
Acoustic generator located at the bottom of control box and is located at the lower section of net cage, and mechanical hand is suspended in the top of net cage to take in control box
Go out net cage, the two bottom sides of control box are respectively equipped with high pressure water inlet and discharge outlet.
Preferably, step 3) described in aqueous slkali be Ca (OH)2In solution, KOH solution, NaOH solution, KCl solution one
Plant or several；The concentration of described aqueous slkali is 0.01-0.2mol/L, preferably 0.05-0.1mol/L, Shan Zao section Sargassum and alkali
The mass ratio of solution is 1:10-40, preferably 1:15-35, using infrared heating temperature to 60-150 DEG C, preferably
75-95 DEG C, the response time is 3-12h, preferably 4-8h.
Preferably, step 3) described in enzymatic solution be cellulase solution, protein enzyme solution, sulfo group hydrogenation enzymatic solution, D-
One or more of galactose-6-sulfurylase solution, system pH is the optimum pH of enzyme used；Described enzymatic solution dense
Spend for 40-100u/L, preferably 50-80u/L, Shan Zao section Sargassum is 1 with the mass ratio of enzymatic solution:10-40, preferably 1:
15-35, using infrared heating temperature to 40-50 DEG C, the response time is 0.5-12h, preferably 1-6h.
Preferably, step 4) the low-mid-frequency ultrasonic concussion reaction time be 0.5-2h；Step 5) in use filter-cloth filtering Sargassum
Glue；Step 6) in ultrafiltration membrane material be cellulose esters, polysulfones, TPO, poly- fluoroolefins class, polrvinyl chloride, pottery,
One of metal, after filtration, dense glue is cooled to 35-37 DEG C.
Preferably, step 7) described in organic solvent be selected from ethanol, isopropanol, glycerol, methanol, N, N- dimethylacetamide
One or more of amine, diethylene glycol, organic solvent concentration is 40-80wt%, preferably 60-70wt%；Described potassium salt is molten
Liquid is selected from KCl, KNO3、K2SO4One or more of, potassium salt soln concentration is 0.5-10wt%, preferably 0.8-8wt%；
Described calcium salt soln is selected from CaCl2、Ca(NO3)2、CaSO4One or more of, calcium salt soln concentration is 0.5-10wt%, excellent
Choosing for 0.8-8wt%.
Step 8) in ethanol solution concentration be 40-80wt%, preferably 50-70wt%, drying mode be oven drying,
Infrared drying, vacuum drying or sun dehydration.
The new carrageenan that the present invention provides is (to include China fir Trentepohlia frond or the mixing of gametophytic generation from Shan Zao section Sargassum
The China fir Trentepohlia frond of generation) in extract comprise 3,6- Anhydrogalactose. and 3,6- Anhydrogalactose. -2- sulfuric ester with a definite proportion
The covalently bound copolymer of example, clearly distinguishes over κ-type carrageenan and the physical mixture of ι-type carrageenan.Its 3,6- dehydration half
Lactose -2- sulfuric ester is 25%-50% with respect to the mol ratio content of 3,6- Anhydrogalactose., this colloidality matter between κ-type and ι -
Between type carrageenan, the gel strength of formation is relatively low, and water-retaining property preferably, forms softer and resilient glue.This new carrageenan
There is stronger albumino reaction and calcium-binding capacity strong, gel strength is relatively low, good water-retaining property, elasticity is good, viscosity is low, dissolve
Property good and calcium salt or the features such as potassium salt plastic, and low production cost, can be used as suspending agent, thickening agent, emulsifying agent, gellant, steady
Determine agent, dispersant etc. for, in the food such as beverage, ice cream, fruit jelly, soft sweet, milk product, meat productss, the steady of product can be improved
Qualitative and good taste and flavor can be kept.The simple composite thing of κ-type carrageenan and ι-type carrageenan does not reach this novel clamp
Draw application effect in terms of food for the glue.At present, domestic and international patent does not also announce this kind of carrageenan, does not yet find domestic enterprise
Produce this kind of product, the invention of this new carrageenan and preparation have important function in terms of promoting the development of food service industry.
In addition, China's existing carrageenan production technology usually first adopts concentrated base heat treated, then it is washed till with a large amount of clear water
After neutrality, boil glue, filter, saltout or precipitate extraction carrageenan, generally existing consumption alkali, water consumption are big, and sewage is serious, production efficiency
Low problem.The production technology of a kind of new carrageenan that the present invention provides, is that Sargassum is first used acid solution low frequency ultrasound process
Afterwards, cleaned using Sargassum ultrasonic cleaning device, then processed using dilute alkaline soln or enzymatic solution infrared heating low frequency ultrasound, subsequently
Glue is concentrated with ultrafiltration membrance filter again, and process need not be rinsed to neutrality with a large amount of clear water.The master of wherein Sargassum ultrasonic cleaning device
Acting on is：Water under high pressure enters cleaning equipment, forms high flow rate water and a large amount of bubble, the two-way water being formed by double stirring paddles
Stream, and use cooperatively ultrasonic wave added, Sargassum is carried out with 360 degree of cleanings, can more efficient cleaning Sargassum surface attachments；In addition, net
Case is more conducive to Sargassum and is separated with attachment, and mechanical hand greatly reduces labour force, improves efficiency simultaneously.This equipment has and subtracts
Less cleaning water consumption (save 2/3 water yield), reduce artificial, shorten the process time, improve the beneficial effects such as efficiency, reduces cost
Really.In a word, the production technology of a kind of new carrageenan that the present invention provides solves and consumes alkali, water consumption in prior art greatly, dirty
Water is serious, and time-consuming, and production cost is high, the problems such as low production efficiency.
New carrageenan is prepared using said method, it has advantages below：
(1) the new carrageenan prepared by the present invention, gelling properties are located between κ-type and ι-type carrageenan, have stronger
Albumino reaction and calcium-binding capacity strong, gel strength is relatively low, good water-retaining property, elasticity is good, viscosity is low, dissolubility good and calcium
The features such as salt or potassium salt plastic, and low production cost, can be used as suspending agent, thickening agent, emulsifying agent, gellant, stabilizer, dispersion
Agent etc. is used in the food such as beverage, ice cream, fruit jelly, soft sweet, milk product, meat productss, can improve stability and the energy of product
Keep good taste and flavor, compensate for κ-type and ι-type carrageenan weak point in the application, promote food service industry
Development aspect there is important function；
(2) the invention provides preparing the Sargassum ultrasonic cleaning device of new carrageenan, its Main Function is：Water under high pressure enters
Enter cleaning equipment, form high flow rate water and a large amount of bubble, agitating device is double stirring paddle, the two-way water being formed by double stirring paddles
Stream, and use cooperatively ultrasonic wave added, Sargassum is carried out with 360 degree of cleanings, can more efficient cleaning Sargassum surface attachments；In addition, net
Case is more conducive to Sargassum and is separated with attachment, and mechanical hand greatly reduces labour force, improves efficiency simultaneously, and this equipment has and subtracts
Less cleaning water consumption (save 2/3 water yield), reduce artificial, shorten the process time, improve the beneficial effects such as efficiency, reduces cost
Really；
(3) the invention provides the production technology of new carrageenan, it has, and simple to operate, reaction condition is gentle, cost
The advantages of low, efficiency high, pollution are little, solves that in prior art, consumption alkali, water consumption are big, and sewage is serious, and time-consuming, production cost
Height, the problems such as low production efficiency.
Brief description
Fig. 1 is ultrasonic cleaning device structure chart in the present invention；
Fig. 2 is Sarcothalia crispata Sargassum source picture；
Fig. 3 is Gigartina skottsbergii Sargassum source picture；
Fig. 4 is Eucheuma cottonii Sargassum source picture；
Fig. 5 is Eucheuma spinosum Sargassum source picture.
Wherein, 1 is control box, and 2 is net cage, and 3 is agitating device, and 4 is ultrasonic generator, and 5 is mechanical hand, and 6 is high press-in
The mouth of a river, 7 is discharge outlet.
Specific embodiment
Embodiment 1
The preparation method of carrageenan is as follows：
1) acid treatment：1 Dun Shan algae section Sargassum Sarcothalia crispata is added 15 ton of 0.05% acid solution in 30KHz
Low frequency ultrasound concussion processes 1.5h；
2) wash：By step 1) gained Sargassum cleaned in 40KHz low frequency ultrasound cleaning equipment with suitable quantity of water, except depigmentaton and
Impurity, clean Sargassum is drained；
3) alkali process：To step 2) add 20 tons of 0.1mol/L Ca (OH) in gained Sargassum2Solution, infrared heating is extremely
90 DEG C, 20KHz low frequency ultrasound concussion reaction 8h；
4) carry glue：By step 3) gained Sargassum solution temperature is set to 95 DEG C, 40KHz low frequency ultrasound concussion reaction 1h, carry
Take glue；
5) filter：By step 4) gained Sargassum solution filter-cloth filtering, obtain dilute glue；
6) concentrate cooling：By step 5) the TPO ultrafiltration membrance filter concentration of gained dilute glue, the cooling of gained dense glue
To 36 DEG C；
7) gel：To step 6) add in gained filtrate 60wt% aqueous isopropanol to be precipitated, form gel；
8) dehydrate：By step 7) gained gel rinses repeatedly with 60wt% ethanol solution, press dewatering, extracts moisture
After be placed in 55 DEG C of oven drying 6h；
9) pulverize and sieve：By step 8) gained colloid is pulverized with pulverizer, and cross 80 eye mesh screens, obtain finished product carrageenan.
Wherein, step 2) described in ultrasonic cleaning device as shown in figure 1, it include control box 1, net cage 2, agitating device 3,
Ultrasonic generator 4 and mechanical hand 5, net cage 2 is placed in control box 1, and in net cage 2, ultrasonic generator 4 sets agitating device 3
Bottom in control box 1 lower section positioned at net cage 2, mechanical hand 5 is suspended in the top of net cage 2 to take out net in control box 1
Case 2, the two bottom sides of control box 1 are respectively equipped with high pressure water inlet 6 and discharge outlet 7.
3,6- Anhydrogalactose. and 3,6- Anhydrogalactose. -2- sulfuric ester is comprised with mol ratio for 3 in prepared carrageenan:
1 covalently bound copolymer.
Embodiment 2
1) acid treatment：By 1 Dun Shan algae section Sargassum Gigartina skottsbergii add 5 ton of 0.01% acid solution in
The concussion of 20KHz low frequency ultrasound processes 0.5h；
2) wash：By step 1) gained Sargassum cleaned in 30KHz low frequency ultrasound cleaning equipment with suitable quantity of water, except depigmentaton and
Impurity, clean Sargassum is drained；
3) alkali process：To step 2) add the KOH solution of 30 tons of 0.2mol/L in gained Sargassum, system pH is adjusted to 7
～8, infrared heating to 150 DEG C, 40KHz low frequency ultrasound concussion reaction 3h；
4) carry glue：By step 3) gained Sargassum solution temperature is set to 95 DEG C, 30KHz low frequency ultrasound concussion reaction 1.5h,
Extract glue；
5) filter：By step 4) gained Sargassum solution filter-cloth filtering, obtain dilute glue；
6) concentrate cooling：By step 5) gained dilute glue Pvc Ultrafiltration Membrane filtering and concentrating, the cooling of gained dense glue
To 37 DEG C；
7) gel：To step 6) add in gained filtrate glycerol to be precipitated, form gel；
8) dehydrate：By step 7) gained gel rinses repeatedly with 50wt% ethanol solution, press dewatering, extracts moisture
Infrared drying 8h afterwards；
9) pulverize and sieve：By step 8) gained colloid is pulverized with pulverizer, and cross 120 eye mesh screens, obtain finished product carrageenan.
3,6- Anhydrogalactose. and 3,6- Anhydrogalactose. -2- sulfuric ester is comprised with mol ratio for 2 in prepared carrageenan:
1 covalently bound copolymer.
Embodiment 3
1) acid treatment：By 1 Dun Shan algae section Sargassum Gigartina skottsbergii add 12 ton of 0.1% acid solution in
The concussion of 20KHz low frequency ultrasound processes 1h；
2) wash：By step 1) gained Sargassum cleaned in 30KHz low frequency ultrasound cleaning equipment with suitable quantity of water, except depigmentaton and
Impurity, clean Sargassum is drained；
3) ferment treatment：To step 2) add in gained Sargassum 10 tons of 80u/L cellulase and the mixing of 50u/L protease molten
Liquid, system pH is adjusted to 7～8, infrared heating to 40 DEG C, 40KHz low frequency ultrasound concussion reaction 1h；
4) carry glue：By step 3) gained Sargassum solution temperature is set to 95 DEG C, 30KHz low frequency ultrasound concussion reaction 1.5h,
Extract glue；
5) filter：By step 4) gained Sargassum solution filter-cloth filtering, obtain dilute glue；
6) concentrate cooling：By step 5) the TPO ultrafiltration membrance filter concentration of gained dilute glue, the cooling of gained dense glue
To 35 DEG C；
7) gel：To step 6) add in gained filtrate 1wt%KCl solution to be precipitated, form gel；
8) dehydrate：By step 7) gained gel rinses repeatedly with 70wt% ethanol solution, press dewatering, extracts moisture
After be placed in 60 DEG C of oven drying 8h；
9) pulverize and sieve：By step 8) gained colloid is pulverized with pulverizer, and cross 80 eye mesh screens, obtain finished product carrageenan.
3,6- Anhydrogalactose. and 3,6- Anhydrogalactose. -2- sulfuric ester is comprised with mol ratio for 1 in prepared carrageenan:
1 covalently bound copolymer.
Quality index test and test result
1. the Sargassum source of the new carrageenan of the inventive method preparation as shown in Figures 2 and 3, in Fig. 1 is
Sarcothalia crispata, color is kermesinus, and substantially, in coralliform, frond branch launches like blade branch, frivolous,
Smooth.In Fig. 2 is Gigartina skottsbergii, and color is kermesinus, and lamellar, no branch are abundant, smooth.New
The molecular structure of carrageenan is
As shown in figure 4, it is Eucheuma cottonii, color is brown color in κ-type carrageenan Sargassum source, and branch is obvious,
In smooth Cornu Cervi shape, round and smooth, κ-type carrageenan molecule structural formula is
As shown in figure 5, it is Eucheuma spinosum, color is light brown yellow in ι-type carrageenan Sargassum source, and branch is bright
Aobvious, in thorn-like, apicule thorn-like, ι-type carrageenan molecule structural formula is
2. the new carrageenan of Example 1-3 preparation, measures its quality index, result is as shown in table 1.
Table 1 carrageenan quality index
It will be apparent to those skilled in the art that can technical scheme as described above and design, make other various
Corresponding change and deformation, and all these change and deformation all should belong to the protection domain of the claims in the present invention
Within.
Claims (10)
1. a kind of new carrageenan it is characterised in that：It extracts from Shan Zao section Sargassum, and described carrageenan comprises 3,6- dehydration gala
Sugar and 3,6- Anhydrogalactose. -2- sulfuric ester are with mol ratio as 1-3:1 covalently bound copolymer.
2. new carrageenan according to claim 1 it is characterised in that：Described Shan Zao section Sargassum includes gametophytic generation
China fir Trentepohlia frond or the China fir Trentepohlia frond of mixing generation.
3. a kind of preparation method of new as claimed in claim 1 carrageenan it is characterised in that：Comprise the following steps：
1) acid treatment：Shan Zao section Sargassum acid supplemented solution is processed in 20-40KHz low frequency ultrasound concussion；
2) wash：By step 1) gained Sargassum cleaned in 20-40KHz low frequency ultrasound with water, clean Sargassum drained；
3) alkali process or ferment treatment：To step 2) add in gained Sargassum aqueous slkali or enzymatic solution heating to be reacted, then
20-40KHz low frequency ultrasound concussion reaction；
4) carry glue：By step 3) gained Sargassum solution temperature is set to 80-95 DEG C, in 20-40KHz low frequency ultrasound concussion reaction,
Extract glue；
5) filter：By step 4) filtration of gained Sargassum glue, obtain dilute glue；
6) concentrate cooling：Dilute glue is concentrated with ultrafiltration membrance filter, by the dense glue cooling obtaining；
7) gel：Add organic solvent or potassium salt soln or calcium salt soln to be precipitated in dense glue, form gel；
8) dehydrate：Gained gel ethanol solution is rinsed repeatedly, press dewatering, be dried after extracting moisture, obtain colloid；
9) pulverize and sieve：Colloid is pulverized, and crosses 80-120 eye mesh screen, obtain finished product carrageenan.
4. new carrageenan according to claim 3 preparation method it is characterised in that：Step 1) in acid solution quality contain
Measure as 0.01%-1%, Shan Zao section Sargassum is 1 with the mass ratio of acid solution:5-20, process time is 0.5-2h.
5. new carrageenan according to claim 3 preparation method it is characterised in that：Step 2) middle use ultrasonic cleaning
Equipment is cleaned by ultrasonic Sargassum, and described ultrasonic cleaning device includes control box (1), net cage (2), agitating device (3), ultrasonic generator
(4) and mechanical hand (5), net cage (2) is placed in control box (1), agitating device (3) in net cage (2), ultrasonic generator
(4) located at the bottom of control box (1) and be located at the lower section of net cage (2), mechanical hand (5) is suspended in the top of net cage (2) with from behaviour
Make to take out net cage (2) in case (1), the two bottom sides of control box (1) are respectively equipped with high pressure water inlet (6) and discharge outlet (7).
6. new carrageenan according to claim 3 preparation method it is characterised in that：Step 3) described in aqueous slkali be
Ca(OH)2One or more of solution, KOH solution, NaOH solution, KCl solution；The concentration of described aqueous slkali is 0.01-
0.2mol/L, Shan Zao section Sargassum is 1 with the mass ratio of aqueous slkali:10-40, using infrared heating temperature to 60-150 DEG C, instead
It is 3-12h between seasonable.
7. new carrageenan according to claim 3 preparation method it is characterised in that：Step 3) described in enzymatic solution be
One or more of cellulase solution, protein enzyme solution, sulfo group hydrogenation enzymatic solution, D- galactose-6-sulfurylase solution,
System pH is the optimum pH of enzyme used；The concentration of described enzymatic solution is 40-100u/L, the matter of Shan Zao section Sargassum and enzymatic solution
Amount ratio is 1:10-40 uses infrared heating temperature to 40-50 DEG C, and the response time is 0.5-12h.
8. new carrageenan according to claim 3 preparation method it is characterised in that：Step 4) low-mid-frequency ultrasonic concussion
Response time is 0.5-2h；Step 5) in use filter-cloth filtering Sargassum glue；Step 6) in ultrafiltration membrane material be cellulose esters,
One of polysulfones, TPO, poly- fluoroolefins class, polrvinyl chloride, pottery, metal, after filtration, dense glue are cooled to
35-37℃.
9. new carrageenan according to claim 3 preparation method it is characterised in that：Step 7) described in organic solvent
Selected from one or more of ethanol, isopropanol, glycerol, methanol, N,N-dimethylacetamide, diethylene glycol, organic solvent concentration
For 40-80wt%；Described potassium salt soln is selected from KCl, KNO3、K2SO4One or more of, potassium salt soln concentration is 0.5-
10wt%；Described calcium salt soln is selected from CaCl2、Ca(NO3)2、CaSO4One or more of, calcium salt soln concentration is 0.5-
10wt%；Step 8) in ethanol solution concentration be 40-80wt%, drying mode be oven drying, infrared drying, vacuum drying
Or sun dehydration.
10. application in food processing field for the new carrageenan described in claim 1 or 2, described food includes beverage, ice
River in Henan Province pouring, fruit jelly, soft sweet, milk product and meat productss.
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| CN111560079A (en) * | 2020-05-18 | 2020-08-21 | 集美大学 | Preparation method of Iota carrageenan glue solution |
| CN116003644A (en) * | 2022-09-15 | 2023-04-25 | 集美大学 | Alkali extraction method for extracting kappa-carrageenan from red algae |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109965011A (en) * | 2019-04-08 | 2019-07-05 | 河北兄弟伊兰食品科技股份有限公司 | A kind of preparation method of low gel strength carragheen |
| CN110028599A (en) * | 2019-05-14 | 2019-07-19 | 深圳市仙迪化妆品有限公司 | A kind of preparation method of algae chitosan |
| CN111560079A (en) * | 2020-05-18 | 2020-08-21 | 集美大学 | Preparation method of Iota carrageenan glue solution |
| CN116003644A (en) * | 2022-09-15 | 2023-04-25 | 集美大学 | Alkali extraction method for extracting kappa-carrageenan from red algae |
| CN116003644B (en) * | 2022-09-15 | 2024-03-29 | 集美大学 | Alkali extraction method for extracting kappa-carrageenan from red algae |
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