CN102050883B - Method for extracting chitosan from yellow mealworm shell - Google Patents
Method for extracting chitosan from yellow mealworm shell Download PDFInfo
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- CN102050883B CN102050883B CN2009100446914A CN200910044691A CN102050883B CN 102050883 B CN102050883 B CN 102050883B CN 2009100446914 A CN2009100446914 A CN 2009100446914A CN 200910044691 A CN200910044691 A CN 200910044691A CN 102050883 B CN102050883 B CN 102050883B
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Abstract
The invention discloses a method for extracting chitosan from yellow mealworm shell, which comprises the following steps of: drying and crushing the yellow mealworm shell, adding 1 to 2 mol/L solution of hydrochloric acid to remove ash through an acid leaching method, and removing protein through an alkaline method with stirring in a boiling water bath of 8 to 10 percent sodium hydroxide; decoloring in 6 to 8 percent hydrogen peroxide; and finally, deacetylating in the presence of concentrated alkali at the temperature of 150 DEG C in 45 to 50 percent sodium hydroxide. The produced chitosan of yellow mealworm is light white and has no peculiar smell and high deacetylated degree; and the process flow is easy to operate and master and is low in cost.
Description
Technical field:
The present invention relates to the process for extracting of the chitosan in the chitin in a kind of insect shell, specifically, relate to the process for extracting of the chitosan in the chitin in a kind of tenebrio molitor shell.
Background technology:
Tenebrio molitor cries the bread worm again, originates in NA, and introduce China from the Soviet Union and raise the fifties, and the tenebrio molitor dry product is fatty 30%, contains protein up to more than 50%, contains major element and various trace elements such as phosphorus, potassium, iron, sodium, aluminium in addition.Its reproduction speed is than very fast, and meeting then have chitin through the process of shell in the shell in developmental process.Chitosan is the product of chitin N-deacetylation, and generally speaking, the N-ethanoyl is sloughed and just can be referred to as chitosan more than 55%.Chitosan has excellent chemical physics performance, and its oligose has important biological, makes it obtain in fields such as foodstuffs industry, medical and health industry, biotechnology, papermaking weavings using widely.Therefore the skin under can also tenebrio molitor after bright worm is extracted protein and grease in process of growth, sloughing off is a raw material; Chitin extraction; Through the processing modified chitosan for preparing, so not only can make full use of the tenebrio molitor resource, improve its added value of product; And can improve the performance of like product, for the tenebrio molitor resource is opened up new application approach.
But the existing preparation chitosan is to adopt natural resources processing, not environmental protection and directly cause cost higher, moreover complex process, and equipment requirements is high, is not suitable for the processing of small serial production.
Summary of the invention:
Technical problem to be solved by this invention is: low to extraction yield in the domestic research that utilizes insect shell extraction chitosan at present; Purity and deacetylation are also very low; The deficiency that technology is not mature enough; The process for extracting of chitosan in a kind of tenebrio molitor shell is provided, extracts high deacetylized chitosan with minimum cost.
In order to solve the problems of the technologies described above, the technical scheme that the present invention adopted is: the process for extracting of chitosan in a kind of tenebrio molitor shell, this method comprises the steps:
A, raw material are handled: the tenebrio molitor shell was taken out in 45～55 ℃ of dryings in 10～14 hours, cross twice of 20 mesh sieve; Pulverize the back after 60～80 mesh sieves, it is subsequent use to collect worm shell powder;
B, remove ash content: the worm shell powder behind the crushing screening is immersed in 1～2mol/L hydrochloric acid soln in the ratio that 1g worm powder adds the 10mL hydrochloric acid soln, and stirring at room is after 3.5～6 hours, spinning 18-22min, and suction filtration, distilled water wash is to neutral under the room temperature;
C, remove protein: will going up ratio that material that a step obtains adds the 10mL sodium hydroxide solution in 1g, to immerse mass concentration be in 8～10% the sodium hydroxide solution; Boiling water bath (100 ℃) stirred 3～6 hours; Spinning 10-20min, suction filtration, distilled water wash is to neutral under the room temperature;
D, decolouring: will going up ratio that the material that obtains of step adds the 10mL ydrogen peroxide 50 in 1g, to immerse mass concentration be in 6～8% the ydrogen peroxide 50, and stirring at room 3～5h, distilled water wash be to neutral, suction filtration;
E, deacetylation: will going up ratio that a step gained material adds the 20mL sodium hydroxide solution in 1g, to add mass concentration be in 45～50% the sodium hydroxide solution; 150 oil baths reaction 5～8 hours; Filter, to neutral, lyophilize makes chitosan with 65-75 ℃ distilled water wash.
Above-mentionedly remove ash content and remove that centrifugal rotational speed is 4800～5200r/min in the protein step.Above-mentionedly remove ash content, the vacuum tightness when removing suction filtration in protein and the decolouring step is 0～0.03MPa.Carrying out in the above-mentioned deacetylation step two periods of 150 ℃ of oil bath 5～8 little time-divisions of reaction, soon the time period is divided into two sections, uses distilled water wash behind the reaction half the time, and once more in 150 ℃ of oil baths second half times of reaction.Lyophilize in the above-mentioned deacetylation step is for freezing 8～12 hours until becoming solid-state under-50 ℃～-10 ℃, in normal atmosphere is the vacuum of 1.3～13Pa, handle 2～4 hours until drying then.
Compared with prior art, the advantage of the inventive method is: technical process is simple to operate, is prone to grasp; Can the resource maximum using be turned waste into wealth, improved the utility value of tenebrio molitor; The easy purchase price of plant and instrument in the making processes is cheap and easy to operate; Cost is lower, and profit margin is bigger.
Embodiment:
Embodiment 1:
The tenebrio molitor shell is tiled on the plate washer, places taking-up in 14 hours in 55 ℃ of electric drying oven with forced convections.Cross 20 mesh sieves twice, cross 60 mesh sieves after pulverizing with kibbler then, it is subsequent use to collect worm shell powder; The worm shell powder that obtains is immersed in the 2mol/LHCL solution in the ratio that 1g adds 10mL hydrochloric acid, stirring at room reaction 6 hours, spinning 5200r/min * 22min, suction filtration (vacuum tightness is 0.03MPa), distilled water wash is to neutral; It is that boiling water bath stirred after 6 hours in 10% the sodium hydroxide solution that the ratio that the material that obtains is added the 10mL sodium hydroxide solution in 1g immerses mass concentration, spinning 5000r/min * 20min, and suction filtration (vacuum tightness is 0.03MPa), distilled water wash is to neutral; It is in 8% the ydrogen peroxide 50 that the ratio that the material that obtains is added the 10mL ydrogen peroxide 50 in 1g immerses mass concentration, and stirring at room 5h, distilled water wash be to neutral, suction filtration (vacuum tightness is 0.03MPa); It is in 50% the sodium hydroxide solution that the ratio that a last step gained material is added the 20mL sodium hydroxide solution in 1g adds mass concentration; Use distilled water wash 150 ℃ of oil bath reactions after 4 hours; And once more in 150 ℃ of oil bath reactions 4 hours; Filter, to neutral, make chitosan after the lyophilize with 75 ℃ distilled water washs.Sterilize half a hour for 110～121 ℃ putting into Autoclave after the chitosan sealing that obtains.
Embodiment 2:
The tenebrio molitor shell is tiled on the plate washer, places taking-up in 12 hours in 50 ℃ of electric drying oven with forced convections.Cross 20 mesh sieves twice, cross 60 mesh sieves after pulverizing with kibbler then, it is subsequent use to collect worm shell powder; The worm shell powder that obtains is immersed in the 1mol/L HCL solution in the ratio that 1g adds 10mL hydrochloric acid, stirring at room reaction 4.5 hours, spinning 5000r/min * 20min, suction filtration (vacuum tightness is 0.01MPa), distilled water wash is to neutral; It is that boiling water bath stirred after 5 hours in 9% the sodium hydroxide solution that the ratio that the material that obtains is added the 10mL sodium hydroxide solution in 1g immerses mass concentration, spinning 5000r/min * 15min, and suction filtration (vacuum tightness is 0.01MPa), distilled water wash is to neutral; It is in 7% the ydrogen peroxide 50 that the ratio that the material that obtains is added the 10mL ydrogen peroxide 50 in 1g immerses mass concentration, and stirring at room 4h, distilled water wash be to neutral, suction filtration (vacuum tightness is 0.01MPa); It is in 48% the sodium hydroxide solution that the ratio that a last step gained material is added the 20mL sodium hydroxide solution in 1g adds mass concentration; Use distilled water wash 150 ℃ of oil bath reactions after 3 hours; And once more in 150 ℃ of oil bath reactions 3 hours; Filter, to neutral, make chitosan after the lyophilize with 70 ℃ distilled water washs.Sterilize half a hour for 110～121 ℃ putting into Autoclave after the chitosan sealing that obtains.
Embodiment 3:
The tenebrio molitor shell is tiled on the plate washer, places taking-up in 10 hours in 45 ℃ of electric drying oven with forced convections.Cross 20 mesh sieves twice, cross 60 mesh sieves after pulverizing with kibbler then, it is subsequent use to collect worm shell powder; The worm shell powder that obtains is immersed in the 1mol/L HCL solution in the ratio that 1g adds 10mL hydrochloric acid, stirring at room reaction 3.5 hours, spinning 4800r/min * 18min, suction filtration (vacuum tightness is 0MPa), distilled water wash is to neutral; It is that boiling water bath stirred after 3 hours in 8% the sodium hydroxide solution that the ratio that the material that obtains is added the 10mL sodium hydroxide solution in 1g immerses mass concentration, spinning 4800r/min * 10min, and suction filtration (vacuum tightness is 0MPa), distilled water wash is to neutral; It is in 6% the ydrogen peroxide 50 that the ratio that the material that obtains is added the 10mL ydrogen peroxide 50 in 1g immerses mass concentration, and stirring at room 3h, distilled water wash be to neutral, suction filtration (vacuum tightness is 0MPa); It is in 45% the sodium hydroxide solution that the ratio that a last step gained material is added the 20mL sodium hydroxide solution in 1g adds mass concentration; Use distilled water wash 150 ℃ of oil bath reactions after 2.5 hours; And once more in 150 ℃ of oil bath reactions 2.5 hours; Filter, to neutral, make chitosan after the lyophilize with 65 ℃ distilled water washs.Sterilize half a hour for 110～121 ℃ putting into Autoclave after the chitosan sealing that obtains.
The chitosan that the inventive method embodiment extracted is compared with the chitosan product that extracts by conventional art, and the result sees the following form 1:
The quality contrast table of table 1 product of the present invention and traditional product
| Product 1 of the present invention | Product 2 of the present invention | Product 3 of the present invention | Traditional product | |
| Outward appearance | White powder is opaque basically | White powder is opaque basically | White powder is opaque basically | White powder is translucent |
| Smell | Substantially tasteless | Substantially tasteless | Substantially tasteless | Substantially tasteless |
| Deacetylation | 84.53％ | 82.13％ | 81.22％ | Look kind and decide |
| Ash content | 1.3％ | 1.3％ | 1.3％ | Look kind and decide |
| Moisture | 8.8％ | 9％ | 9％ | 11％ |
Can know that by last table the chitosan that the inventive method is extracted is a white powder, and is opaque basically; Basic odorlessness, deacetylation is higher than 81.2%, and moisture content is lower than 9%; Ash oontent is lower than 1.3%, and basic heavy metal free, and total number of bacterial colonies is lower than 1000cfu/g; Coliform count is lower than 30cfu/g, no pathogenic bacterium.
Claims (5)
1. the process for extracting of chitosan in the tenebrio molitor shell, it is characterized in that: this method comprises the steps:
A, raw material are handled: the tenebrio molitor shell was taken out in 45～55 ℃ of dryings in 10～14 hours, cross twice of 20 mesh sieve; Pulverize the back after 60～80 mesh sieves, it is subsequent use to collect worm shell powder;
B, remove ash content: the worm shell powder behind the crushing screening is immersed in 1～2mol/L hydrochloric acid soln in the ratio that 1g worm shell powder adds the 10mL hydrochloric acid soln, and stirring at room is after 3.5～6 hours, spinning 18-22min, and suction filtration, distilled water wash is to neutral under the room temperature;
C, remove protein: will going up ratio that material that a step obtains adds the 10mL sodium hydroxide solution in 1g, to immerse mass concentration be in 8～10% the sodium hydroxide solution; Boiling water bath stirred 3～6 hours; Spinning 10-20min, suction filtration, distilled water wash is to neutral under the room temperature;
D, decolouring: will going up ratio that the material that obtains of step adds the 10mL ydrogen peroxide 50 in 1g, to immerse mass concentration be in 6～8% the ydrogen peroxide 50, and stirring at room 3～5h, distilled water wash be to neutral, suction filtration;
E, deacetylation: will going up ratio that a step gained material adds the 20mL sodium hydroxide solution in 1g, to add mass concentration be in 45～50% the sodium hydroxide solution; 150 ℃ of oil bath reactions 5～8 hours; Filter, to neutral, lyophilize makes chitosan with 65～75 ℃ distilled water washs.
2. the process for extracting of chitosan in the tenebrio molitor shell as claimed in claim 1 is characterized in that: said b, and the c step in centrifugal rotational speed be 4800～5200r/min.
3. the process for extracting of chitosan in the tenebrio molitor shell as claimed in claim 1 is characterized in that: the vacuum tightness in said b, c and the d step during suction filtration is 0～0.03MPa.
4. the process for extracting of chitosan in the tenebrio molitor shell as claimed in claim 1; It is characterized in that: carrying out in the said e step two periods of 150 ℃ of oil bath 5～8 little time-divisions of reaction; Soon the time period is divided into two sections; Use distilled water wash behind the reaction half the time, and once more in 150 ℃ of oil bath second half times of reaction.
5. the process for extracting of chitosan in the tenebrio molitor shell as claimed in claim 1; It is characterized in that: the lyophilize in the said e step is for freezing 8～12 hours until becoming solid-state under-50 ℃～-10 ℃, in normal atmosphere is the vacuum of 1.3～13Pa, handles 2～4 hours until drying then.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100446914A CN102050883B (en) | 2009-11-04 | 2009-11-04 | Method for extracting chitosan from yellow mealworm shell |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100446914A CN102050883B (en) | 2009-11-04 | 2009-11-04 | Method for extracting chitosan from yellow mealworm shell |
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| CN102050883A CN102050883A (en) | 2011-05-11 |
| CN102050883B true CN102050883B (en) | 2012-08-15 |
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| CN2009100446914A Expired - Fee Related CN102050883B (en) | 2009-11-04 | 2009-11-04 | Method for extracting chitosan from yellow mealworm shell |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276758B (en) * | 2011-08-10 | 2013-07-03 | 绵阳师范学院 | Method for comprehensively utilizing insect Chinese medicine dregs |
| CN102702385B (en) * | 2012-06-15 | 2014-02-12 | 山东省花生研究所 | Preparation method for extracting chitosan from holotrichia parallela |
| CN104878057A (en) * | 2015-04-22 | 2015-09-02 | 山西农业大学 | Large-scale production method for tenebrio molitor chitosan |
| CN104961844A (en) * | 2015-07-22 | 2015-10-07 | 天津泰康生物制药有限公司 | Method for preparing chitosan from low-age insect larvae at normal temperature |
| CN113667036A (en) * | 2021-08-11 | 2021-11-19 | 青岛新农康源生物工程有限公司 | Method for extracting tenebrio molitor chitosan |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101565470A (en) * | 2009-05-31 | 2009-10-28 | 中南林业科技大学 | Method for preparing chitin and chitosan from dendrolimus punctatus larvae |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101565470A (en) * | 2009-05-31 | 2009-10-28 | 中南林业科技大学 | Method for preparing chitin and chitosan from dendrolimus punctatus larvae |
Non-Patent Citations (1)
| Title |
|---|
| 窦珍伟等.黄粉虫中甲壳素和壳聚糖的提取工艺研究.《山东大学学报（工学版）》.2008,第38卷(第5期),第107-112页，第116页. * |
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Address after: 410006 a unit 202 room, women's compound courtyard, Jinxing Road, Changsha, Hunan, Yuelu District Patentee after: Hunan Saibang Biological Technology Co. Ltd. Address before: 410006 a unit 202 room, women's compound courtyard, Jinxing Road, Changsha, Hunan, Yuelu District Patentee before: Changsha Saibang Biotechnology Co., Ltd. |
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Granted publication date: 20120815 Termination date: 20181104 |