CN106832053A - A kind of technique that shitosan is extracted in the crab from shrimp - Google Patents
A kind of technique that shitosan is extracted in the crab from shrimp Download PDFInfo
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- CN106832053A CN106832053A CN201611245173.5A CN201611245173A CN106832053A CN 106832053 A CN106832053 A CN 106832053A CN 201611245173 A CN201611245173 A CN 201611245173A CN 106832053 A CN106832053 A CN 106832053A
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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
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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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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Abstract
The invention discloses the technique that shitosan is extracted in a kind of crab from shrimp, comprise the steps：1) washing：Discarded shrimp and crab shells are cleaned with clear water, the silt and impurity on removal shrimp and crab shells surface；2) dry：By step 1) drying of the shrimp and crab shells that obtain, crush to obtain shrimp and crab shells meal；3) low-temperature grinding：By step 2) the shrimp and crab shells 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.Intermediate step of the present invention is not in black impurity, and the product color for obtaining is pure white.
Description
Technical field
A kind of work the present invention relates to extract shitosan in marine bioactivity extractive technique field, more particularly to crab from shrimp
Skill.
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.
In nature, arthropod such as shrimp, crab etc. are up to 58-85% containing chitin, and chitin is only second to cellulose
Second largest renewable resource on the earth, shrimp shell, crab shell are the discarded objects in aquatic products processing industry, and yield is huge, and cost is relatively low, contains
There is the shitosan after abundant chitin and its deacetylation.There are abundant shrimp, crab resource, the water of many shrimp crabs in Qinzhou Prefecture
The leftover bits and pieces such as shrimp shell, shrimp head, crab shell of the processing producer after processing shrimp crab are produced, it is difficult to process, because wherein containing abundant albumen
Matter, fat, after accumulation easily fermentation, it is spoiled, rise it is mould, influence environment.
But prepare chitin using shrimp, crab shell and there is also some problems that can not be ignored, one is except some large-scale seas
Outside Product processing enterprise, shrimp, crab shell are difficult concentric acquisition, general eating at home or hotel it is edible after abandoned as rubbish and
It is difficult to reclaim；Two is that shrimp, crab shell are contained within the commensals such as substantial amounts of protein and fat, pre-processes cumbersome, is processed unnet
Or be not completely dried, matter of going mouldy easily is acted during preservation.Just because of such some reasons, it is subject to shrimp, making full use of for crab shell
Great limitation.Chinese patent CN103936884A, a kind of method of the chitin extraction from shrimp and crab shells, is the conjunction of applicant
Make the earlier application of partner, the method, although the chitin content for obtaining is high, but yield is low (less than 20%), and
Color and luster is white or canescence, not ideal enough above color and luster.If can after treatment apply shrimp and crab shells, can realize giving up
The efficient utilization of gurry and make maximum resource utilization, produce huge economy and social benefit.Resource circulation utilization and ecology
Energy environment protection is the target of China's Long-and Medium-term Development most important thing.
The content of the invention
The invention provides the technique that shitosan is extracted in a kind of crab from shrimp, high income, intermediate step is not in black
Impurity, the product color for obtaining is pure white.
The present invention is achieved through the following technical solutions：
The technique that shitosan is extracted in a kind of crab from shrimp, comprises the steps:
1) washing：Discarded shrimp and crab shells are cleaned with clear water, the silt and impurity on removal shrimp and crab shells surface；
2) dry：By step 1) drying of the shrimp and crab shells that obtain, crush to obtain shrimp and crab shells meal；
3) low-temperature grinding：By step 2) the shrimp and crab shells 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 1 of the present invention) described in crab shrimp shell, with arbitrary proportion mix.
Step 2) 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, 10000-15000psi, 5-10min.
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, the chitin extraction from shrimp and crab shells, prior art after shrimp and crab shells usually are crushed into 20-60 mesh, directly adds
Hot extraction, ultrasonication, microwave treatment etc., or separated or deproteination using enzymolysis, lactobacillus-fermented, 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 shrimp and crab shells meal, it is to avoid more than cumbersome technique, directly destroy egg
White matter, fat, then with acid treatment, intermediate step is not in black impurity, and the product color for obtaining 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 shrimp and crab shells chitin extraction has no report.Present invention employs ultralow temperature crushing technology, shrimp and crab shells are entered successively
Row cryogenic freezing, low-temperature distillation dry after with liquid nitrogen as abrasive media, carried out with super-low temperature pulverizator at -80-120 DEG C low
Temperature is crushed, and using low temperature brittleness characteristic, can crush the material for being difficult in thermal sensitivity or normal temperature crush, and prevents rotten when crushing.
3rd, the shrimp and crab shells 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 shrimp and crab shells
Matter and organic matter are crushed, and beneficial to the reaction with watery hydrochloric acid, the group of protein, fat, pigment can also be destroyed, beneficial to chitin
Dissolution.
Specific embodiment
With embodiment, the invention will be further described below, but the invention is not limited in these embodiments.
Embodiment 1：
The technique that shitosan is extracted in a kind of crab from shrimp, comprises the steps:
1) washing：Discarded shrimp and crab shells are cleaned with clear water, the silt and impurity on removal shrimp and crab shells surface；
2) dry：By step 1) the shrimp and crab shells 10kg that obtains drying, granularity is crushed to ball mill obtains shrimp and crab shells in 80 mesh
Meal；
3) low-temperature grinding：By step 2) the shrimp and crab shells 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, 10min；
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 2.12kg, purity 98.77% after drying.
Embodiment 2：
The technique that shitosan is extracted in a kind of crab from shrimp, comprises the steps:
1) washing：Discarded shrimp and crab shells are cleaned with clear water, the silt and impurity on removal shrimp and crab shells surface；
2) dry：By step 1) the shrimp and crab shells 10kg that obtains drying, granularity is crushed to ball mill obtains shrimp and crab shells in 100 mesh
Meal；
3) low-temperature grinding：By step 2) the shrimp and crab shells 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, 5min；
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 2.08kg, purity 98.81% after drying.
Embodiment 3：
The technique that shitosan is extracted in a kind of crab from shrimp, comprises the steps:
1) washing：Discarded shrimp and crab shells are cleaned with clear water, the silt and impurity on removal shrimp and crab shells surface；
2) dry：By step 1) the shrimp and crab shells 10kg that obtains drying, granularity is crushed to ball mill obtains shrimp and crab shells in 80 mesh
Meal；
3) low-temperature grinding：By step 2) the shrimp and crab shells 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, 15000psi, 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 2.14kg, purity 99.16% 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.
10kg shrimp and crab shells obtain chitin 1.64kg, purity 98.23%.
Comparative example 2：
1) washing：Discarded shrimp and crab shells are cleaned with clear water, the silt and impurity on removal shrimp and crab shells surface；
2) dry：By step 1) the shrimp and crab shells 10kg that obtains drying, granularity is crushed to ball mill obtains shrimp and crab shells in 80 mesh
Meal；
3) low-temperature grinding：By step 2) the shrimp and crab shells 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 1.59kg, purity 91.76% after drying.
Comparative example 3：
1) washing：Discarded shrimp and crab shells are cleaned with clear water, the silt and impurity on removal shrimp and crab shells surface；
2) dry：By step 1) the shrimp and crab shells 10kg that obtains drying, granularity is crushed to ball mill obtains shrimp and crab shells 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, 15000psi, 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 1.55kg, purity 90.45% after drying.
Comparative example 4：
1) Feedstock treating：Rubbed after 10kg shrimps head and crab shell are cleaned with pure water；
2) ultrasonication：15 times of pure water of weight, ultrasonication 15min, effect are added in raw material after rubbing
30 DEG C of temperature, power is 250W, after the completion of filter, collect filter residue；
3) HIGH PRESSURE TREATMENT：The filter residue that step b is obtained, adds pure water, and 30min is kept in 115 DEG C, 150MPa high pressures,
Filtering, collects filter residue；
4) acid treatment：Obtain adding the 3.0mol/L hydrochloric acid solutions equivalent to 2 times of quality of filter residue in filter residue to step c, leaching
Bubble 1h, is washed to neutrality, is centrifuged, and chitin is obtained after freeze-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 1.48kg, purity 91.87% after drying.
Conclusion：The sample result of embodiment 3 is better than comparative example.
Claims (6)
1. the technique that shitosan is extracted in a kind of crab from shrimp, it is characterised in that comprise the steps：
1) washing：Discarded shrimp and crab shells are cleaned with clear water, the silt and impurity on removal shrimp and crab shells surface；
2) dry：By step 1) drying of the shrimp and crab shells that obtain, crush to obtain shrimp and crab shells meal；
3) low-temperature grinding：By step 2) the shrimp and crab shells 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. the technique that shitosan is extracted in a kind of crab from shrimp according to claim 1, it is characterised in that：Step 2) described in
Crush, be that granularity is crushed in 80-100 mesh with ball mill.
3. the technique that shitosan is extracted in a kind of crab from shrimp according to claim 1, it is characterised in that：Step 3) described in
Cryogenic freezing, temperature is 0--18 DEG C.
4. the technique that shitosan is extracted in a kind of crab from shrimp according to claim 1, it is characterised in that：Step 4) described in
It is high-pressure homogeneous, it is to add the 5-6 times of pure water of weight to be well mixed, it is subsequently adding high pressure homogenizer treatment, 10000-
15000psi、5-10min。
5. the technique that shitosan is extracted in a kind of crab from shrimp according to claim 1, it is characterised in that：Step 5) described in
Add watery hydrochloric acid immersion, 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. the technique that shitosan is extracted in a kind of crab from shrimp according to claim 1, it is characterised in that：Step 6) described in
Concentrated caustic immersion is added, is to add the 8-10 times of caustic soda of the 10mol/L of weight, 2-3h is soaked at 100 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111227026A (en) * | 2020-03-09 | 2020-06-05 | 中国海洋大学 | Method for preparing meat preservative film by using shrimp and crab shells |
| CN112552129A (en) * | 2020-12-25 | 2021-03-26 | 生态环境部南京环境科学研究所 | Repairing agent for cadmium pollution of rice planting soil, preparation method and device thereof |
| CN114437249A (en) * | 2022-02-21 | 2022-05-06 | 龙岩学院 | Method for extracting chitosan from shrimp and crab shells in one step |
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| JPH08208709A (en) * | 1995-02-04 | 1996-08-13 | Nippon Kichin Kitosan Kk | Method for eliminating bitter taste from chitosan |
| CN103936884A (en) * | 2014-04-18 | 2014-07-23 | 广西还珠海洋生物科技有限公司 | Method for extracting chitin from shrimp and crab shells |
| CN104725530A (en) * | 2014-09-11 | 2015-06-24 | 迪沙药业集团有限公司 | Preparation method of O-carboxylated chitin |
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2016
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| JPH08208709A (en) * | 1995-02-04 | 1996-08-13 | Nippon Kichin Kitosan Kk | Method for eliminating bitter taste from chitosan |
| CN103936884A (en) * | 2014-04-18 | 2014-07-23 | 广西还珠海洋生物科技有限公司 | Method for extracting chitin from shrimp and crab shells |
| CN104725530A (en) * | 2014-09-11 | 2015-06-24 | 迪沙药业集团有限公司 | Preparation method of O-carboxylated chitin |
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| 赵余庆 等: "《食疗与保健食品原料功能因子手册》", 31 March 2013 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111227026A (en) * | 2020-03-09 | 2020-06-05 | 中国海洋大学 | Method for preparing meat preservative film by using shrimp and crab shells |
| CN112552129A (en) * | 2020-12-25 | 2021-03-26 | 生态环境部南京环境科学研究所 | Repairing agent for cadmium pollution of rice planting soil, preparation method and device thereof |
| CN112552129B (en) * | 2020-12-25 | 2022-03-08 | 生态环境部南京环境科学研究所 | Repairing agent for cadmium pollution of rice planting soil, preparation method and device thereof |
| CN114437249A (en) * | 2022-02-21 | 2022-05-06 | 龙岩学院 | Method for extracting chitosan from shrimp and crab shells in one step |
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