CN106749739A - A kind of method that shitosan is extracted from oyster shell - Google Patents
A kind of method that shitosan is extracted from oyster shell Download PDFInfo
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- CN106749739A CN106749739A CN201611243847.8A CN201611243847A CN106749739A CN 106749739 A CN106749739 A CN 106749739A CN 201611243847 A CN201611243847 A CN 201611243847A CN 106749739 A CN106749739 A CN 106749739A
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- 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
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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- 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
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Abstract
The invention discloses a kind of method that shitosan is extracted from oyster shell, comprise the steps：1) washing：Discarded oyster shell is cleaned with clear water, the silt and impurity on removal oyster shell surface；2) dry：By step 1) drying of the oyster shell that obtains, crush to obtain oyster shell meal；3) low-temperature grinding：By step 2) the oyster shell meal that obtains, carry out cryogenic freezing successively and after low-temperature distillation is dried with liquid nitrogen as abrasive media, carry out low-temperature grinding with super-low temperature pulverizator at 80 120 DEG C；4) it is high-pressure homogeneous：By step 3) material that obtains adds pure water to be well mixed, and is subsequently adding high pressure homogenizer treatment；5) acid treatment：To step 4) material that obtains, watery hydrochloric acid immersion is added, neutrality is washed to, it is centrifuged, obtain chitin after drying；6) deacetylation, shitosan is obtained after drying.Whole activity time of the invention shortens, and, intermediate step is not in black impurity, and the product color for obtaining is pure white.
Description
Technical field
The present invention relates to marine bioactivity extractive technique field, more particularly to a kind of shitosan is extracted from oyster shell
Method.
Background technology
Shitosan is that chitin (Chitin) deacetylate under basic conditions is just obtained.Chitin, also referred to as chitin,
Find that 1823 by Ou Jier (0dier) from crustacean shell by French scholar Bu Lakenuo (Braconno) within 1811
Extract, and be named as CHITIN, translated name is chitin.Chitin be by N- acetyl -2-amino-2-deoxy-D-Glucose with β -
Isosorbide-5-Nitrae glycosidic bond form is formed by connecting, i.e. the glycan of N-ACETYL-D-GLUCOSAMINE.Because chitin can take off in process of production
Fall part acetyl group, thus commercialization chitin be all N-ACETYL-D-GLUCOSAMINE and D-Glucose amine copolymer.
Chitin is the second largest living resources that cellulose is only second in nature quantity, estimates annual biosynthesis
Chitin is up to 10,000,000,000 tons, is one of organic matter most abundant on the earth, is the inexhaustible living resources of the mankind, is also 20
One of natural resources not being fully utilized in century, wherein marine organisms growing amount are up to 1,000,000,000 tons.Chitin has anticancer, suppresses
Cancer, oncocyte transfer, improve body immunity and liver detoxification effect.It is particularly suited for diabetes, liver-kidney diseases, hypertension, fertilizer
It is fat to wait disease, be conducive to prevention cancer cell lesion and chemoradiation therapy treatment tumor disease.And torpescence on chitin chemistry, not with
Body fluid changes, and can not organize foreign body reaction, nontoxic, with antithrombotic, it is high temperature-resistant disinfected the features such as.
Because the cellulosic structure being widely present in the chemical constitution of chitin and plant is closely similar, therefore is also called animal
Cellulose, chitin is widely present in the crust of Crustaceans shrimp, crab, the crust of insect, the cell of fungi (yeast, mould)
In the cell membrane of wall and plant (such as mushroom).In nature, arthropod such as shrimp, crab etc. are up to 58-85% containing chitin；Shrimp
Shell, crab shell are the discarded objects in aquatic products processing industry, and yield is huge, and cost is relatively low, containing abundant chitin and its deacetylated
Shitosan after base.Shitosan therein being extracted, by can be applied to various aspects after modification, discarded object can be realized
Efficiently utilize and make maximum resource utilization, produce huge economy and social benefit.
Oyster shell is to be adjusted to be formed by biomineralization by organic matter, i.e., with a small amount of organic matter macromolecular (protein, sugared egg
White or polysaccharide) it is framework, molecule manipulation, the multiple microlayer structures of the high-sequential of composition are carried out in units of calcium carbonate.Oyster
The material composition of shell is divided into inanimate matter and organic matter two parts.Inanimate matter part accounts for oyster shell quality 90% based on calcium carbonate
More than, wherein calcium constituent accounts for (39.78 ± 0.23) %, additionally contains the various trace elements of copper, iron, zinc, manganese, strontium etc. 20.It is male
The organic principle of oyster shell accounts for the 3-5% of oyster shell quality, contains 17 kinds of amino acid such as glycine, cystine, methionine.Shell
Organic matter fractions be divided into SOM and insoluble organic matter again, its content with shell species it is different with growth period and
It is different, the 0.01-10% of shell dry mass is typically constituted from, wherein SOM content is less, accounts for 0.03-5%.
Because the yield of shrimp, crab shell is higher, higher (general chitin content has chitin content in more than 20-30%
Up to 60-85%), preparation method it is simpler, therefore prepare chitin and mainly use shrimp, crab shell at present.But using shrimp, crab
Shell prepares chitin and there is also some problems that can not be ignored, and one is shrimp, crab in addition to some large-scale marine products processing enterprises
Shell is difficult concentric acquisition, and general eating at home or hotel are abandoned as rubbish and be difficult to reclaim after eating；Two is shrimp, crab shell
The commensals such as substantial amounts of protein and fat are contained within, pretreatment is cumbersome, treatment is not net or is not completely dried, pole during preservation
Easily act matter of going mouldy.Just because of such some reasons, it is greatly limited shrimp, making full use of for crab shell.Chinese patent
CN103936884A, a kind of method of the chitin extraction from shrimp and crab shells, is our previous application, but the method, it is right
In treatment oyster husk as raw material, effect is bad.University Of Suzhou's paper, Liu Hongxi, the extraction of oyster shell chitin and its derivative are in print
Application in dye, it is noted that the extraction of oyster shell chitin, but focus on the application of the chitin that obtains in printing and dyeing, its life
Production. art is laboratory lab scale, such as filtering uses filter paper, and many processing steps and parameter are not suitable for industrialized production.
The content of the invention
The invention provides a kind of method that shitosan is extracted from oyster shell, whole activity time shortens, and, it is middle
Operation is not in black impurity, and the product color for obtaining is pure white.
The present invention is achieved through the following technical solutions：
A kind of method that shitosan is extracted from oyster shell, comprises the steps:
1) washing：Discarded oyster shell is cleaned with clear water, the silt and impurity on removal oyster shell surface；
2) dry：By step 1) drying of the oyster shell that obtains, crush to obtain oyster shell meal；
3) low-temperature grinding：By step 2) the oyster shell meal that obtains, carry out cryogenic freezing successively and after low-temperature distillation is dried
With liquid nitrogen as abrasive media, low-temperature grinding is carried out with super-low temperature pulverizator at -80--120 DEG C；
4) it is high-pressure homogeneous：By step 3) material that obtains adds pure water to be well mixed, it is subsequently adding at high pressure homogenizer
Reason；
5) acid treatment：To step 4) material that obtains, watery hydrochloric acid immersion is added, neutrality is washed to, it is centrifuged, obtained after drying
Chitin；
6) deacetylation：By step 5) chitin that obtains, add concentrated caustic immersion, washing, adjustment pH to neutrality, water
Wash, be centrifuged, shitosan is obtained after drying.
Step 2 of the present invention) described in crushing, granularity is preferably crushed in 80-100 mesh with ball mill.
Step 3) described in cryogenic freezing, 0--18 DEG C of preferable temperature, more preferably -10--18 DEG C.
Step 4) described in it is high-pressure homogeneous, be preferably added to the 5-6 times of pure water of weight be well mixed, be subsequently adding high pressure equal
The treatment of matter machine, 10000-18000psi, 10-20min.
Step 5) described in addition watery hydrochloric acid immersion, be preferably added to the 3-5 times of watery hydrochloric acid of the 1mol/L of weight at room temperature
Immersion 0.5-1.0h；Described centrifugation, preferably 1500r/min, 10min.
Step 6) described in addition concentrated caustic immersion, the 8-10 times of caustic soda of the 10mol/L of weight is preferably added to, at 100 DEG C
Lower immersion 2-3h.
Compared with prior art, advantages of the present invention：
1st, chitin extraction or shitosan from oyster shell, seek to remove a large amount of calcium carbonate in oyster shell first, existing
There is technology, after oyster shell usually is crushed into 20-60 mesh, is directly added into watery hydrochloric acid and sloughs the mineral matters such as calcium carbonate, but so
Place comprehend generation protein suspension and black impurity (protein suspension can adhering device inwall, influence production is and black
Colored foreign can influence finished product color and luster), then with diluted alkaline deproteinising, degreasing, (acid-base neutralization can cause grease and alkali to occur again
Saponification, makes liquid turns turbid), in order to color and luster is pure white, what is had can also be decolourized with liquor potassic permanganate, although color and luster is had
Improve, but have black impurity presence, and, whole operation needs multiple times of filtration, washing, causes production to waste.And this
Invention is by carrying out low-temperature grinding, high-pressure homogeneous treatment to oyster shell meal, it is to avoid more than cumbersome technique, directly destroy egg
White matter, fat, then with acid treatment, whole activity time shortens, and, intermediate step is not in black impurity, the product for obtaining
Product color and luster is pure white.
2nd, freeze grinding technology, because the price of refrigerant is higher, is restricted, the now in actual industrial production
Useless cold liquid nitrogen of producing has been succeeded during using natural gas gasifying, and liquid nitrogen prices, freeze grinding technology is just developed, but
The technology application oyster shell chitin extraction or shitosan have no report.Present invention employs ultralow temperature crushing technology, by oyster
Shell is carried out after cryogenic freezing, low-temperature distillation are dried with liquid nitrogen as abrasive media successively, is crushed with ultralow temperature at -80-120 DEG C
Machine carries out low-temperature grinding, using low temperature brittleness characteristic, can crush the material for being difficult in thermal sensitivity or normal temperature crush, and prevents from crushing
Shi Bianzhi.
3rd, the oyster husk as raw material that the present invention is obtained using high pressure homogenization method treatment, does not use adventitious solvent, by high pressure
Material can be directly crushed to cellular level by the powerful shearing force and impulsive force that homogeneous method is produced, inorganic by what is contained in oyster shell
Matter and organic matter are crushed, and beneficial to calcium carbonate and the reaction of acid, the group of protein, fat, pigment can also be destroyed, beneficial to crust
The dissolution of element.
Specific embodiment
With embodiment, the invention will be further described below, but the invention is not limited in these embodiments.
Embodiment 1：
A kind of method that shitosan is extracted from oyster shell, comprises the steps:
1) washing：Discarded oyster shell is cleaned with clear water, the silt and impurity on removal oyster shell surface；
2) dry：By step 1) the oyster shell 100kg that obtains drying, granularity is crushed to ball mill obtains oyster shell in 80 mesh
Meal；
3) low-temperature grinding：By step 2) the oyster shell meal that obtains, 0 DEG C of cryogenic freezing is carried out successively and low-temperature distillation is dried
Afterwards with liquid nitrogen as abrasive media, low-temperature grinding is carried out with super-low temperature pulverizator at -80 DEG C；
4) it is high-pressure homogeneous：By step 3) material that obtains adds 5 times of pure water of weight to be well mixed, and is subsequently adding high pressure
Homogenizer treatment, 10000psi, 20min；
5) acid treatment：To step 4) material that obtains, add the watery hydrochloric acid of 3 times of 1mol/L of weight to soak at room temperature
1.0h, is washed to neutrality, centrifugation, and 1500r/min, 10min obtain chitin after drying；
6) deacetylation：By step 5) chitin that obtains, 8 times of caustic soda of the 10mol/L of weight are added, at 100 DEG C
Immersion 2h, washing, adjustment pH to neutrality, washing, centrifugation obtains shitosan 3.11kg, purity 98.68% after drying.
Embodiment 2：
A kind of method that shitosan is extracted from oyster shell, comprises the steps:
1) washing：Discarded oyster shell is cleaned with clear water, the silt and impurity on removal oyster shell surface；
2) dry：By step 1) the oyster shell 100kg that obtains drying, granularity is crushed to ball mill obtains oyster in 100 mesh
Shell meal；
3) low-temperature grinding：By step 2) the oyster shell meal that obtains, -10 DEG C of cryogenic freezings are carried out successively and low-temperature distillation is dry
With liquid nitrogen as abrasive media after dry, low-temperature grinding is carried out with super-low temperature pulverizator at -100 DEG C；
4) it is high-pressure homogeneous：By step 3) material that obtains adds 6 times of pure water of weight to be well mixed, and is subsequently adding high pressure
Homogenizer treatment, 15000psi, 15min；
5) acid treatment：To step 4) material that obtains, add the watery hydrochloric acid of 4 times of 1mol/L of weight to soak at room temperature
1.0h, is washed to neutrality, centrifugation, and 1500r/min, 10min obtain chitin after drying；
6) deacetylation：By step 5) chitin that obtains, 10 times of caustic soda of the 10mol/L of weight are added, at 100 DEG C
Immersion 3h, washing, adjustment pH to neutrality, washing, centrifugation obtains shitosan 3.15kg, purity 98.72% after drying.
Embodiment 3：
A kind of method that shitosan is extracted from oyster shell, comprises the steps:
1) washing：Discarded oyster shell is cleaned with clear water, the silt and impurity on removal oyster shell surface；
2) dry：By step 1) the oyster shell 100kg that obtains drying, granularity is crushed to ball mill obtains oyster shell in 80 mesh
Meal；
3) low-temperature grinding：By step 2) the oyster shell meal that obtains, -18 DEG C of cryogenic freezings are carried out successively and low-temperature distillation is dry
With liquid nitrogen as abrasive media after dry, low-temperature grinding is carried out with super-low temperature pulverizator at -120 DEG C；
4) it is high-pressure homogeneous：By step 3) material that obtains adds 5 times of pure water of weight to be well mixed, and is subsequently adding high pressure
Homogenizer treatment, 18000psi, 10min；
5) acid treatment：To step 4) material that obtains, add the watery hydrochloric acid of 5 times of 1mol/L of weight to soak at room temperature
1.0h, is washed to neutrality, centrifugation, and 1500r/min, 10min obtain chitin after drying；
6) deacetylation：By step 5) chitin that obtains, 10 times of caustic soda of the 10mol/L of weight are added, at 100 DEG C
Immersion 3h, washing, adjustment pH to neutrality, washing, centrifugation obtains shitosan 3.11kg, purity 99.13% after drying.
Comparative example 1：
20 mesh -1mol/L watery hydrochloric acid of washing-dry-be crushed to slough mineral matter-washing -2.5mol/L, and dilute caustic soda sloughs egg
White matter, degreasing-chitin crude product -0.7%KMnO4Bleaching-chitin-concentrated caustic deacetylation-be washed to is neutral-and it is dry
Dry-shitosan.
100kg oyster shells obtain chitin 2.68kg, purity 98.25%.
Comparative example 2：
1) washing：Discarded oyster shell is cleaned with clear water, the silt and impurity on removal oyster shell surface；
2) dry：By step 1) the oyster shell 100kg that obtains drying, granularity is crushed to ball mill obtains oyster shell in 80 mesh
Meal；
3) low-temperature grinding：By step 2) the oyster shell meal that obtains, -18 DEG C of cryogenic freezings are carried out successively and low-temperature distillation is dry
With liquid nitrogen as abrasive media after dry, low-temperature grinding is carried out with super-low temperature pulverizator at -120 DEG C；
4) acid treatment：To step 3) material that obtains, add the watery hydrochloric acid of 5 times of 1mol/L of weight to soak at room temperature
1.0h, is washed to neutrality, centrifugation, and 1500r/min, 10min obtain chitin after drying；
5) deacetylation：By step 4) chitin that obtains, 10 times of caustic soda of the 10mol/L of weight are added, at 100 DEG C
Immersion 3h, washing, adjustment pH to neutrality, washing, centrifugation obtains shitosan 1.68kg, purity 92.32% after drying.
Comparative example 3：
1) washing：Discarded oyster shell is cleaned with clear water, the silt and impurity on removal oyster shell surface；
2) dry：By step 1) the oyster shell 100kg that obtains drying, granularity is crushed to ball mill obtains oyster shell in 80 mesh
Meal；
3) it is high-pressure homogeneous：By step 2) material that obtains adds 5 times of pure water of weight to be well mixed, and is subsequently adding high pressure
Homogenizer treatment, 18000psi, 10min；
4) acid treatment：To step 3) material that obtains, add the watery hydrochloric acid of 5 times of 1mol/L of weight to soak at room temperature
1.0h, is washed to neutrality, centrifugation, and 1500r/min, 10min obtain chitin after drying；
5) deacetylation：By step 4) chitin that obtains, 10 times of caustic soda of the 10mol/L of weight are added, at 100 DEG C
Immersion 3h, washing, adjustment pH to neutrality, washing, centrifugation obtains shitosan 1.56kg, purity 89.79% after drying.
Conclusion：The sample result of embodiment 3 is better than comparative example.
Claims (6)
1. it is a kind of from oyster shell extract shitosan method, it is characterised in that comprise the steps：
1) washing：Discarded oyster shell is cleaned with clear water, the silt and impurity on removal oyster shell surface；
2) dry：By step 1) drying of the oyster shell that obtains, crush to obtain oyster shell meal；
3) low-temperature grinding：By step 2) the oyster shell meal that obtains, carry out cryogenic freezing successively and after low-temperature distillation is dried with liquid
Nitrogen is abrasive media, and low-temperature grinding is carried out with super-low temperature pulverizator at -80--120 DEG C；
4) it is high-pressure homogeneous：By step 3) material that obtains adds pure water to be well mixed, and is subsequently adding high pressure homogenizer treatment；
5) acid treatment：To step 4) material that obtains, watery hydrochloric acid immersion is added, neutrality is washed to, it is centrifuged, obtain crust after drying
Element；
6) deacetylation：By step 5) chitin that obtains, add concentrated caustic immersion, washing, adjustment pH to neutrality, washing, from
The heart, shitosan is obtained after drying.
2. it is according to claim 1 it is a kind of from oyster shell extract shitosan method, it is characterised in that：Step 2) it is described
Crushing, be that granularity is crushed in 80-100 mesh with ball mill.
3. it is according to claim 1 it is a kind of from oyster shell extract shitosan method, it is characterised in that：Step 3) it is described
Cryogenic freezing, temperature be 0--18 DEG C.
4. it is according to claim 1 it is a kind of from oyster shell extract shitosan method, it is characterised in that：Step 4) it is described
It is high-pressure homogeneous, be to add 5-6 times of pure water of weight to be well mixed, be subsequently adding high pressure homogenizer treatment, 10000-
18000psi、10-20min。
5. it is according to claim 1 it is a kind of from oyster shell extract shitosan method, it is characterised in that：Step 5) it is described
The immersion of addition watery hydrochloric acid, be that the watery hydrochloric acid for adding the 3-5 times of 1mol/L of weight soaks 0.5-1.0h at room temperature, it is described from
The heart, 1500r/min, 10min.
6. it is according to claim 1 it is a kind of from oyster shell extract shitosan method, it is characterised in that：Step 6) it is described
Addition concentrated caustic immersion, be add the 8-10 times of caustic soda of the 10mol/L of weight, soak 2-3h at 100 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108359022A (en) * | 2018-02-28 | 2018-08-03 | 漯河中德双成功能食品研究院有限公司 | A kind of preparation method of lentinan |
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| CN104558240A (en) * | 2013-10-11 | 2015-04-29 | 李文金 | A process of extracting chitosan from shrimp shells |
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Application publication date: 20170531 |