CN106831939A - A kind of tussah silk protein extracting method - Google Patents
A kind of tussah silk protein extracting method Download PDFInfo
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- CN106831939A CN106831939A CN201710002466.9A CN201710002466A CN106831939A CN 106831939 A CN106831939 A CN 106831939A CN 201710002466 A CN201710002466 A CN 201710002466A CN 106831939 A CN106831939 A CN 106831939A
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- silk
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- tussah
- silk cocoon
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
- C07K1/14—Extraction; Separation; Purification
- C07K1/145—Extraction; Separation; Purification by extraction or solubilisation
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- Organic Chemistry (AREA)
- General Health & Medical Sciences (AREA)
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- Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Medicinal Chemistry (AREA)
- Molecular Biology (AREA)
- Proteomics, Peptides & Aminoacids (AREA)
- Analytical Chemistry (AREA)
- Cosmetics (AREA)
- Peptides Or Proteins (AREA)
Abstract
The invention provides a kind of method that tussah silk-fibroin scouring processes prepare tussah silk-fibroin, with tussah cocoon as raw material, first crushed with pulverizer and fragmentated, add deionized water immersion to be pre-processed；Then oxidant, stabilizer, filament expansion agent, bleeding agent, chelating agent and water are made into scouring solution, tussah cocoon and scouring solution are mixed, the colloid in tussah cocoon is fully removed using the oxidisability of peroxide, be finally separated from water fibroin, dry, the tussah silk-fibroin for obtaining.
Description
Technical field
The invention belongs to silk manufacture field, and in particular to a kind of extracting method of tussah silk-fibroin.
Background technology
Tussah silk is mainly what is be made up of two kinds of protein of silk gum and fibroin, collectively referred to as fibroin.Silk gum is enclosed in silk
Cellulose fiber top layer, plays adhesive action.Silk gum and fibroin have different structures and performance：Silk gum is globular preteins, secondary structure
Based on random coil, stability is poor, in dissolving in the solution such as hot water, acid, alkali, protease and low concentration sodium carbonate；Fibroin
It is fibrous protein, containing substantial amounts of crystalline texture, stable performance dissolves in high calcium chloride concentration, the mixing of calcium chloride ethanol water
In the solution such as liquid and lithium bromide.Therefore, it can dissolving sex differernce and practical application need in different solutions according to fibroin
Ask, select suitable lysate to carry out extraction process, the various fibroins with different structure Yu performance are obtained, for processing
Prepare the difference such as cosmetics and food additives, biological tissue's repair materials, high-absorbent material, pharmaceutical carrier and cell culture medium
Morphological function material.
At present, traditional fibroin extracts thinking：1. by cocoon layer or silk silk gum lysate（Such as boiling water, high temperature
High pressure, acid, alkali, liquid of protease etc.）Treatment and purifying, obtain partially or mostly sericin；2. first by cocoon layer or cocoon
Silk uses silk gum lysate（Such as 0.5% w/w Na2CO3 solution）Degumming process is carried out, fibroin fiber is obtained；Then, by the fibroin
Fiber fibroin lysate（Such as 50% w/w CaCl2 solution）Treatment, dialysis purification, obtain fibroin albumen.But use with
On method extract fibroin it is often not thorough, it is impossible to the fibroin in silk cocoon is extracted completely, so as to cause
The waste of material, it is therefore desirable to develop a kind of method that can completely extract fibroin in silk cocoon as far as possible, improves raw material
Utilization rate.
The content of the invention
It is an object of the invention to provide a kind of extraction side of fibroin to overcome above the deficiencies in the prior art
Method, further improves the recovery rate of fibroin.
A kind of tussah silk protein extracting method, the method is comprised the following steps：
A, selection spring tussah cocoon or summer and autumn tussah cocoon, silk cocoon fragment is ground into by silk cocoon pulverizer, and the fragment is put into band
There is equilibrium water conten in the vacuum tank of humidification and humidity-discharging device, determine the regain of fragment；Chip mass is weighed, according to regain
Calculate its silk cocoon dry weight；Deionized water is added in silk cocoon fragment, the silk in fragment is fully soaked by immersion swelling；
B, oxidant, stabilizer, swelling agent, bleeding agent, chelating agent and distilled water are made into degumming reaction solution；By silk cocoon fragment and
Degumming reaction solution mixes, and the initial pH value of degumming liquid is adjusted with NaOH solution；Reactor is put into thermostat water bath, stirring is anti-
The mixture in device is answered, water-bath is incubated after heating up, the colloid in silk is tentatively removed using the oxidisability of peroxide, obtained
To silk cocoon albumen and the mixture of impurity；
C, the mixture obtained by step B is carried out into centrifugation layering, supernatant liquor is transferred in another container, remaining concentration
Silk cocoon protein suspending liquid is put into vacuum freeze drier, is molded its freeze-drying, and the silk cocoon albumen of powder state is obtained, and finally will
Obtained silk cocoon albumen is put into refrigerating chamber storage.
In the step A, the silk cocoon fragment fineness of crushing is 400 mesh, adds distilled water to make fragment in distillation in fragment
Mass percent concentration is 11%~15% in water, and the distilled water immersion time is 36h.
It is in mass ratio 15: 20 mixing by silk cocoon fragment and degumming reaction solution, with 1500mL bottle,suctions in the step B
Used as reactor, the initial pH value for adjusting degumming liquid with 0.5mol/LNaOH solution is 8.0~9.0；Reactor is put into constant temperature
In water-bath, with magnetic stirring apparatus with the mixture in the speed continuous-stirring reactor of 500rpm, make water-bath with 10 DEG C/
The speed of min is warmed up to 150 DEG C, while being incubated 200min.
In the step C, centrifugation layering is carried out by centrifuge, centrifuge speed is 15000rpm, centrifugation number of times is 10
It is secondary；Freeze-drying shaping is carried out using liquid nitrogen, the temperature of freeze-drying shaping is -70 DEG C, the pressure 80Pa of freeze-drying shaping,
The time of freeze-drying shaping is 15h.
The oxidant is SODIUM PERCARBONATE, sodium metaperiodate, hydrogen peroxide, sodium hypochlorite, potassium percarbonate, sodium chlorate, over cure
One or more in sour ammonium.
The stabilizer is sodium salicylate, Sodium Benzoate, resorcinol, citric acid, one kind of disodium ethylene diamine tetraacetate
Or it is several.
The swelling agent is urea, ethylenediamine, liquefied ammonia, thiocarbamide, 4- methylmorpholine N-oxides, cupri ethylene diamine, dimethyl
One or two in sulfoxide.
The bleeding agent be polyvinyl alcohol, neopelex, dodecyl sodium sulfate, lauryl sodium sulfate,
One or two in AEO (JFC), peregal.
The chelating agent is Sodium Polyacrylate, sodium tartrate, the adjacent sodium of ethylenediamine two, the first of diethylenetriamine five
Fork Alendronate, ATMP, one or more in ethylene diamine tetra methylene phosphonic acid sodium.
The method provided using the present invention can farthest extract the fibroin in silk cocoon, after measured, the present invention
The fibroin extraction rate reached of the extracting method of the fibroin of offer is to more than 99.8%.
Specific embodiment
To become apparent the present invention, hereby with several preferred embodiments, it is described in detail below.
Embodiment 1
A kind of tussah silk protein extracting method, the method is comprised the following steps：
A, selection spring tussah cocoon or summer and autumn tussah cocoon, silk cocoon fragment is ground into by silk cocoon pulverizer, and the fragment is put into band
There is equilibrium water conten in the vacuum tank of humidification and humidity-discharging device, determine the regain of fragment；Chip mass is weighed, according to regain
Calculate its silk cocoon dry weight；Deionized water is added in silk cocoon fragment, the silk in fragment is fully soaked by immersion swelling；Its
In, the silk cocoon fragment fineness of crushing is 400 mesh, adds distilled water to make fragment mass percent concentration in distilled water in fragment
It is 15%, the distilled water immersion time is 36h.
B, oxidant, stabilizer, swelling agent, bleeding agent, chelating agent and distilled water are made into degumming reaction solution；Silk cocoon is broken
Piece and degumming reaction solution mix, and the initial pH value of degumming liquid is adjusted with NaOH solution；Reactor is put into thermostat water bath, is stirred
The mixture in reactor is mixed, water-bath is incubated after heating up, the glue in silk is tentatively removed using the oxidisability of peroxide
Matter, obtains the mixture of silk cocoon albumen and impurity；Wherein, in mass ratio it is specially 15 by silk cocoon fragment and degumming reaction solution:
20 mixing, using 1500mL bottle,suctions as reactor, the initial pH value for adjusting degumming liquid with 0.5mol/LNaOH solution is
8.0；Reactor is put into thermostat water bath, with magnetic stirring apparatus with the mixing in the speed continuous-stirring reactor of 500rpm
Thing, makes water-bath be warmed up to 150 DEG C with the speed of 10 DEG C/min, while being incubated 200min.
C, the mixture obtained by step B is carried out into centrifugation layering, supernatant liquor is transferred in another container, it is remaining
Concentration silk cocoon protein suspending liquid is put into vacuum freeze drier, is molded its freeze-drying, the silk cocoon albumen of powder state is obtained, most
Obtained silk cocoon albumen is put into refrigerating chamber storage afterwards；Centrifugation layering is carried out specifically by centrifuge, centrifuge speed is
15000rpm, centrifugation number of times is 10 times；Freeze-drying shaping is carried out using liquid nitrogen, the temperature of freeze-drying shaping is -70 DEG C, cold
Freeze the pressure 80Pa of drying and moulding, the time of freeze-drying shaping is 15h.
The method provided using the present invention can farthest extract the fibroin in silk cocoon, after measured, the present invention
The fibroin extraction rate reached of the extracting method of the fibroin of offer is to more than 99.8%.
Claims (4)
1. a kind of tussah silk protein extracting method, it is characterised in that the method is comprised the following steps：
A, selection spring tussah cocoon or summer and autumn tussah cocoon, silk cocoon fragment is ground into by silk cocoon pulverizer, and the fragment is put into band
There is equilibrium water conten in the vacuum tank of humidification and humidity-discharging device, determine the regain of fragment；Chip mass is weighed, according to regain
Calculate its silk cocoon dry weight；Deionized water is added in silk cocoon fragment, the silk in fragment is fully soaked by immersion swelling；
B, oxidant, stabilizer, swelling agent, bleeding agent, chelating agent and distilled water are made into degumming reaction solution；By silk cocoon fragment and
Degumming reaction solution mixes, and the initial pH value of degumming liquid is adjusted with NaOH solution；Reactor is put into thermostat water bath, stirring is anti-
The mixture in device is answered, water-bath is incubated after heating up, the colloid in silk is tentatively removed using the oxidisability of peroxide, obtained
To silk cocoon albumen and the mixture of impurity；
C, the mixture obtained by step B is carried out into centrifugation layering, supernatant liquor is transferred in another container, remaining concentration
Silk cocoon protein suspending liquid is put into vacuum freeze drier, is molded its freeze-drying, and the silk cocoon albumen of powder state is obtained, and finally will
Obtained silk cocoon albumen is put into refrigerating chamber storage.
2. tussah silk protein extracting method according to claim 1, it is characterised in that in the step A, the silk cocoon of crushing
Fragment fineness is 400 mesh, adds distilled water to make fragment mass percent concentration in distilled water be 11%~15% in fragment,
The distilled water immersion time is 36h.
3. tussah silk protein extracting method according to claim 1, it is characterised in that in the step B, by silk cocoon fragment
It is in mass ratio 15: 20 mixing with degumming reaction solution, using 1500mL bottle,suctions as reactor, uses 0.5mol/LNaOH solution
The initial pH value for adjusting degumming liquid is 8.0~9.0；Reactor is put into thermostat water bath, with magnetic stirring apparatus with 500rpm
Speed continuous-stirring reactor in mixture, water-bath is warmed up to 150 DEG C with the speed of 10 DEG C/min, at the same insulation
200min。
4. tussah silk protein extracting method according to claim 1, it is characterised in that in the step C, by centrifuge
Centrifugation layering is carried out, centrifuge speed is 15000rpm, centrifugation number of times is 10 times；Freeze-drying shaping is carried out using liquid nitrogen, it is cold
The temperature for freezing drying and moulding is -70 DEG C, the pressure 80Pa of freeze-drying shaping, and the time of freeze-drying shaping is 15h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710002466.9A CN106831939A (en) | 2017-01-03 | 2017-01-03 | A kind of tussah silk protein extracting method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710002466.9A CN106831939A (en) | 2017-01-03 | 2017-01-03 | A kind of tussah silk protein extracting method |
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| Publication Number | Publication Date |
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| CN106831939A true CN106831939A (en) | 2017-06-13 |
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| CN201710002466.9A Withdrawn CN106831939A (en) | 2017-01-03 | 2017-01-03 | A kind of tussah silk protein extracting method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107266569A (en) * | 2017-07-28 | 2017-10-20 | 浙江理工大学 | A kind of preparation method of tussah silk fibroin monoclonal antibody |
| CN113666995A (en) * | 2021-08-25 | 2021-11-19 | 浙江大学 | Method for quickly and efficiently preparing native tussah silk fibroin powder |
| CN114108310A (en) * | 2021-12-27 | 2022-03-01 | 浙江理工大学 | Machine-made silk floss refining method without hydrogen peroxide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103132157A (en) * | 2013-03-18 | 2013-06-05 | 丹东中天柞蚕生物科技有限公司 | Biological degumming cocoon reelability method for China oak silkworm |
| CN103290085A (en) * | 2013-05-13 | 2013-09-11 | 湖州新天丝生物技术有限公司 | Silk protein powder and preparation method thereof |
| CN104592376A (en) * | 2014-12-29 | 2015-05-06 | 无锡蚕魅科技有限公司 | Extraction method of fibroin |
| CN105061606A (en) * | 2015-09-01 | 2015-11-18 | 东华大学 | Method for preparing adsorbable oxycellulose through ramie oxidation degumming process |
-
2017
- 2017-01-03 CN CN201710002466.9A patent/CN106831939A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103132157A (en) * | 2013-03-18 | 2013-06-05 | 丹东中天柞蚕生物科技有限公司 | Biological degumming cocoon reelability method for China oak silkworm |
| CN103290085A (en) * | 2013-05-13 | 2013-09-11 | 湖州新天丝生物技术有限公司 | Silk protein powder and preparation method thereof |
| CN104592376A (en) * | 2014-12-29 | 2015-05-06 | 无锡蚕魅科技有限公司 | Extraction method of fibroin |
| CN105061606A (en) * | 2015-09-01 | 2015-11-18 | 东华大学 | Method for preparing adsorbable oxycellulose through ramie oxidation degumming process |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107266569A (en) * | 2017-07-28 | 2017-10-20 | 浙江理工大学 | A kind of preparation method of tussah silk fibroin monoclonal antibody |
| CN113666995A (en) * | 2021-08-25 | 2021-11-19 | 浙江大学 | Method for quickly and efficiently preparing native tussah silk fibroin powder |
| CN113666995B (en) * | 2021-08-25 | 2024-01-23 | 浙江大学 | Method for preparing native tussah silk fibroin powder |
| CN114108310A (en) * | 2021-12-27 | 2022-03-01 | 浙江理工大学 | Machine-made silk floss refining method without hydrogen peroxide |
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Application publication date: 20170613 |
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