CN105968147A - Preparation method of oligochitosan - Google Patents
Preparation method of oligochitosan Download PDFInfo
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- CN105968147A CN105968147A CN201610318583.1A CN201610318583A CN105968147A CN 105968147 A CN105968147 A CN 105968147A CN 201610318583 A CN201610318583 A CN 201610318583A CN 105968147 A CN105968147 A CN 105968147A
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- oligochitosan
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H5/00—Compounds containing saccharide radicals in which the hetero bonds to oxygen have been replaced by the same number of hetero bonds to halogen, nitrogen, sulfur, selenium, or tellurium
- C07H5/04—Compounds containing saccharide radicals in which the hetero bonds to oxygen have been replaced by the same number of hetero bonds to halogen, nitrogen, sulfur, selenium, or tellurium to nitrogen
- C07H5/06—Aminosugars
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
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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 a preparation method of oligochitosan. The preparation method comprises the following steps: (1) adding 1-10 parts by weight of chitosan into 95-105 parts by weight of acid liquor, and mixing to obtain a mixed solution; (2) adding 45-65 parts by weight of a hydrogen peroxide solution into the mixed solution, heating up to 45-85 DEG C, and stirring for 35-55 minutes at the speed of 200-500r/min to obtain degradation liquid; (3) adding 50-150 parts by weight of alcohol liquid into the degradation liquid, mixing, standing for 10-30min, filtering and drying. The invention also discloses the oligochitosan. The oligochitosan takes the chitosan as a raw material, and is prepared by pretreatment, material liquid preparing, H2O2 and ultrasonic collaborative oxidation degradation, filtering and drying after alcohol precipitation. Compared with the prior art, the preparation method provided by the invention is short in degradation time, complete in degradation and high in yield and narrower in average molecular weight distribution of degradation products, thus being suitable for large-scale industrial production and use.
Description
Technical field
The present invention relates to nutraceutical field, be specifically related to the preparation method of a kind of oligochitosan.
Background technology
Oligochitosan, i.e. glucosamine are sought the bonded degree of polymerization by β-Isosorbide-5-Nitrae-sugar and are about 2-20's
Oligosaccharide, can be prepared by chitosan hydrolyzate, and its molecular weight is less than, in water solublity, and can be directly by human body
Absorb, be the product that in year shell element series of products, application performance is best, can be widely applied to simultaneously medicine,
The multiple industrial circles such as food, beverage, cosmetics, printing.
Oligochitosan is unique basic amine group oligosaccharide containing positive charge in nature, and green natural, nothing are secondary to be made
With, as the biological active substances that a class is new, except having enhancing immunity, antitumor is anticancer, reduce gallbladder
The function such as reparation of beggar and the absorption of ferrum and joint tissue in sterin, blood pressure lowering, blood sugar lowering, acceleration bodies
Outward, also having the effect such as antiseptic and inhibiting bacteria function, regulation human body value, this is also that oligochitosan is different from other oligosaccharide
Key character, oligochitosan has become the most emerging a kind of functional oligose.
At present both at home and abroad the method for research degradation of chitosan mainly has: chemical method, Physical, enzymatic isolation method with
And three kinds of edman degradation Edman derivative composite degradation methods.Oligochitosan generally utilizes chitosan to make through backbone breaking
Become.Along with medicine, the development of food industry, the demand of oligochitosan increases the most day by day, and tradition is passed through
The technique of hydrolyzing chitosan oligochitosan, need to consume substantial amounts of acid, hydrogen peroxide and ethanol etc., etching apparatus,
Cause environmental pollution, and productivity is the highest.
The invention provides the preparation method of a kind of oligochitosan, degradation time is short, degraded is complete, yield is high.
Summary of the invention
For above-mentioned deficiency present in prior art, the technical problem to be solved is to provide one
Plant preparation method of oligochitosan and preparation method thereof.
The present invention seeks to be achieved through the following technical solutions:
The preparation method of a kind of oligochitosan, comprises the following steps:
(1) 1-10 weight portion chitosan is joined in 95-105 weight portion acid solution and mix, mixed
Solution；
(2) 45-65 weight portion hydrogenperoxide steam generator is joined in mixed solution, is warming up to 45-85 DEG C,
200-500 rev/min is stirred 35-55 minute, obtains degradation solution；
(3) 50-150 weight portion alcohol liquid is joined in degradation solution and mix, stand 10-30 minute, mistake
Filter, drying.
Preferably, the acid solution in described step (1) is made up of the raw material of following mass percent: lactic acid
1-5%, malic acid 1-5%, citric acid 1-5%, water 87-97%.
Preferably, the aqueous solution that hydrogenperoxide steam generator is hydrogen peroxide in described step (2), peroxidating
The mass concentration of hydrogen is 15-35%.
Preferably, the alcohol liquid in described step (3) is made up of the raw material of following mass percent: 1-propanol
25-45%, 1,3-propylene glycol 25-45%, water 30-50%.
Preferably, being filtered in described step (3) uses 100-300 mesh filter-cloth filtering.
Preferably, the drying in described step (3) was at being placed in 60-100 DEG C 8-24 hour.
The invention discloses a kind of oligochitosan, with chitosan as raw material, preprocessed, feed liquid configures, H2O2
And ultrasonic synergistic oxidative degradation, filtration, alcohol analysis post-drying prepare.Compared with prior art, the present invention
The preparation method degradation time provided is short, degraded is complete, and yield is high, and catabolite mean molecule quantity divides
Cloth is narrower, is suitable for industrialization use of large-scale production.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further, the following stated, only to the present invention
Preferred embodiment, not does the restriction of other forms, any technology being familiar with this specialty to the present invention
Personnel are changed to the Equivalent embodiments changed on an equal basis possibly also with the technology contents of the disclosure above.Every
Without departing from the present invention program content, any letter following example done according to the technical spirit of the present invention
Single amendment or equivalent variations, all fall within protection scope of the present invention.
Each raw material introduction in embodiment:
Chitosan, No. CAS: 9012-76-4, the de-of Henan Qi Nuo food ingredient company limited offer is provided
Acetyl degree is the food stage chitosan of 95%.
Hydrogen peroxide, No. CAS: 7722-84-1.
Lactic acid, No. CAS: 849585-22-4.
Malic acid, i.e. L MALIC ACID, No. CAS: 97-67-6.
Citric acid, No. CAS: 77-92-9.
1-propanol, No. CAS: 71-23-8.
1,3-PD, No. CAS: 504-63-2.
Embodiment 1
The concrete preparation method of oligochitosan, comprises the following steps:
(1) 7 weight portion chitosans are joined in 100 weight portion acid solutions, be uniformly mixed, obtain
Mixed solution；
(2) 55 weight portion hydrogenperoxide steam generators are joined in mixed solution, wherein hydrogenperoxide steam generator
For the aqueous solution of hydrogen peroxide, the mass concentration of hydrogen peroxide is 30%；It is warming up to 65 DEG C, 300 turns/
Divide stirring 45 minutes, obtain degradation solution；
(3) 100 weight portion alcohol liquid are joined in degradation solution, be uniformly mixed, stand 20 minutes；
Re-use plate and frame filter to filter, use the filter cloth of 180 mesh, obtain filtering residue；Finally filtering residue is placed in
Within at 70 DEG C 12 hours, dry.Obtain the oligochitosan of embodiment 1.
Acid solution in described step (1) is made up of the raw material of following mass percent: lactic acid 2.5%, Herba Marsileae Quadrifoliae
Fruit acid 2.5%, citric acid 2.5%, distilled water 92.5%；Lactic acid, malic acid, citric acid are added distillation
Water is uniformly mixed and i.e. obtains acid solution.
Alcohol liquid in described step (3) is made up of the raw material of following mass percent: 1-propanol 35%, 1,3-
Propylene glycol 35%, distilled water 30%；1-propanol, 1,3-propylene glycol are added stirring in distilled water and mix all
Even i.e. obtain alcohol liquid.
Embodiment 2
Substantially the same manner as Example 1, differ only in: the acid solution in described step (1) is by following matter
The raw material composition of amount percentage ratio: lactic acid 3.75%, malic acid 3.75%, distilled water 92.5%；By lactic acid,
Malic acid addition distilled water is uniformly mixed and i.e. obtains acid solution.Obtain the oligochitosan of embodiment 2.
Embodiment 3
Substantially the same manner as Example 1, differ only in: the acid solution in described step (1) is by following matter
The raw material composition of amount percentage ratio: lactic acid 3.75%, citric acid 3.75%, distilled water 92.5%；By lactic acid,
Citric acid addition distilled water is uniformly mixed and i.e. obtains acid solution.Obtain the oligochitosan of embodiment 3.
Embodiment 4
Substantially the same manner as Example 1, differ only in: the acid solution in described step (1) is by following matter
The raw material composition of amount percentage ratio: malic acid 3.75%, citric acid 3.75%, distilled water 92.5%；By Fructus Mali pumilae
Acid, citric acid addition distilled water are uniformly mixed and i.e. obtain acid solution.Obtain the oligochitosan of embodiment 4.
Embodiment 5
Substantially the same manner as Example 1, differ only in: the alcohol liquid in described step (3) is by following matter
The raw material composition of amount percentage ratio: 1-propanol 70%, distilled water 30%；1-propanol is added in distilled water and stirs
Mix mix homogeneously and i.e. obtain alcohol liquid.Obtain the oligochitosan of embodiment 5.
Embodiment 6
Substantially the same manner as Example 1, differ only in: the alcohol liquid in described step (3) is by following matter
The raw material composition of amount percentage ratio: 1,3-propylene glycol 70%, distilled water 30%；1,3-propylene glycol is added and steams
Distilled water is uniformly mixed and i.e. obtains alcohol liquid.Obtain the oligochitosan of embodiment 6.
Test case 1
The yield of the oligochitosan preparing embodiment 1-6 is added up.Oligochitosan yield (%)=oligochitosan
Quality/chitosan mass × 100%.Concrete outcome is shown in Table 1.
Table 1: oligochitosan yield result list position: %
| Oligochitosan yield | |
| Embodiment 1 | 97.6 |
| Embodiment 2 | 95.2 |
| Embodiment 3 | 95.7 |
| Embodiment 4 | 94.6 |
| Embodiment 5 | 96.3 |
| Embodiment 6 | 95.1 |
Comparing embodiment 1 and embodiment 2-4, embodiment 1 (lactic acid, malic acid, citric acid are compounding) shell
Oligosaccharide yield is apparently higher than embodiment 2-4 (in lactic acid, malic acid, citric acid arbitrarily the two compounding)；
Comparing embodiment 1 and embodiment 5-6, embodiment 1 (1-propanol, 1,3-PD are compounding) oligochitosan is received
Rate is apparently higher than embodiment 5-6 (single raw material in 1-propanol, 1,3-propylene glycol).
Test case 2
Oligochitosan embodiment 1-6 prepared, is placed in 25 DEG C, preservation half a year under relative humidity 85% environment,
" GB/T 4789.2-2010 microbiological test of food hygiene total plate count mensuration " is used to carry out bacterium colony
Sum test.Concrete test result is shown in Table 2.
Table 2: total plate count test table cfu/g
| Total plate count | |
| Embodiment 1 | 1.2×103 |
| Embodiment 2 | 4.1×103 |
| Embodiment 3 | 3.3×103 |
| Embodiment 4 | 3.8×103 |
| Embodiment 5 | 4.0×103 |
| Embodiment 6 | 4.4×103 |
Inventor is found surprisingly that, comparing embodiment 1 and embodiment 2-4, embodiment 1 (lactic acid, Fructus Mali pumilae
Acid, citric acid compound) antiseptic property is substantially better than embodiment 2-4 (in lactic acid, malic acid, citric acid
Arbitrarily the two compounds)；Comparing embodiment 1 and embodiment 5-6, embodiment 1 (1-propanol, 1,3-the third two
Alcohol compounds) antiseptic property is substantially better than embodiment 5-6 (single raw material in 1-propanol, 1,3-propylene glycol).
Test case 3
In oligochitosan embodiment 1-6 prepared, the oligochitosan content of degree of polymerization 2-10 is tested.Test
The results are shown in Table 3.
Table 3: the oligochitosan content measuring result list position of degree of polymerization 2-10: %
Comparing embodiment 1 and embodiment 2-4, embodiment 1 (lactic acid, malic acid, citric acid are compounding) is poly-
The oligochitosan content of right 2-10 is apparently higher than embodiment 2-4 (in lactic acid, malic acid, citric acid arbitrarily
The two is compounding)；Comparing embodiment 1 and embodiment 5-6, (1-propanol, 1,3-PD are multiple for embodiment 1
Join) the oligochitosan content of degree of polymerization 2-10 is (in 1-propanol, 1,3-propylene glycol single apparently higher than embodiment 5-6
One raw material).
Claims (6)
1. the preparation method of an oligochitosan, it is characterised in that comprise the following steps:
(1) 1-10 weight portion chitosan is joined in 95-105 weight portion acid solution and mix, mixed
Solution；
(2) 45-65 weight portion hydrogenperoxide steam generator is joined in mixed solution, is warming up to 45-85 DEG C,
200-500 rev/min is stirred 35-55 minute, obtains degradation solution；
(3) 50-150 weight portion alcohol liquid is joined in degradation solution and mix, stand 10-30 minute, mistake
Filter, drying.
2. the preparation method of oligochitosan as claimed in claim 1, it is characterised in that: described step (1)
In acid solution be made up of the raw material of following mass percent: lactic acid 1-5%, malic acid 1-5%, citric acid
1-5%, water 87-97%.
3. the preparation method of oligochitosan as claimed in claim 1 or 2, it is characterised in that: described step
(2) hydrogenperoxide steam generator in is the aqueous solution of hydrogen peroxide, and the mass concentration of hydrogen peroxide is
15-35%.
4. the preparation method of oligochitosan as claimed in claim 1 or 2, it is characterised in that: described step
(3) the alcohol liquid in is made up of the raw material of following mass percent: 1-propanol 25-45%, 1,3-propylene glycol
25-45%, water 30-50%.
5. the preparation method of oligochitosan as claimed in claim 1 or 2, it is characterised in that: described step
(3) being filtered in uses 100-300 mesh filter-cloth filtering.
6. the preparation method of oligochitosan as claimed in claim 1 or 2, it is characterised in that: described step
(3) drying in was at being placed in 60-100 DEG C 8-24 hour.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107177648A (en) * | 2017-06-30 | 2017-09-19 | 赵景卫 | A kind of chitosan oligosaccharide enzymatic production process |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105085711A (en) * | 2015-08-21 | 2015-11-25 | 哈尔滨工业大学 | Preparation method and application of chitobiose |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105085711A (en) * | 2015-08-21 | 2015-11-25 | 哈尔滨工业大学 | Preparation method and application of chitobiose |
Non-Patent Citations (2)
| Title |
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| 张卫国 等: "有机酸及降解条件对壳聚糖降解速度的影响", 《河北科技师范学院学报》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107177648A (en) * | 2017-06-30 | 2017-09-19 | 赵景卫 | A kind of chitosan oligosaccharide enzymatic production process |
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