CN105087149A - Comprehensive utilization method of silkworm chrysalis - Google Patents
Comprehensive utilization method of silkworm chrysalis Download PDFInfo
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Abstract
The invention relates to a comprehensive utilization method of silkworm chrysalis, comprising the following steps: S1, silkworm chrysalis pretreatment: taking silk-reeled wet silkworm chrysalis, removing bad chrysalis, adding the silk-reeled wet silkworm chrysalis into 0.05-1wt% of an ascorbic acid solution to be immersed for 0.5h-3h, adjusting pH to neutral, drying and crushing; and S2, extraction of chrysalis oil: extracting by using any one of propane, n-butane and isobutane as an extraction agent by a subcritical low-temperature extraction technology at the temperature of 30-50 DEG C, carrying out reduction vaporization on the extraction agent after extraction, and filtering to obtain chrysalis oil. Extraction condition of chrysalis oil is mild, and other nutritional ingredients will not be destroyed. Defatted silkworm chrysalis can be continuously used as a raw material for extracting protein and chitin. Oil extraction efficiency is high, and there is no residual oil to influence quality of protein and chitin. No residual organic solvent can be realized during the whole extraction process. Production costs are low, and pollution is little during the technological process. The method provided by the invention is suitable for industrial production.
Description
Technical field
The present invention relates to food processing technology field, in particular, relate to a kind of method of comprehensive utilization of silkworm chrysalis.
Background technology
At present, the main method of the extraction silkworm chrysalis oil of report has milling process, organic solvent lixiviation process, supercritical CO
2extraction process, ultrasonic extraction.It is very low that milling process extracts pupal fat yield, the resid amount of pupa slag exceedes half, discarded pupa slag is very easily putrid and deteriorated becomes secondary pollutant, and during mechanical expression service temperature up to about 140 DEG C, pupa albumen sex change is serious, affects the recycling of degreasing pupa powder, also makes the unsaturated fatty acids in silkworm chrysalis oil easily oxidative rancidity occur, affect the quality of oil product, greatly weaken the using value of this method.Organic solvent lixiviation process is present stage industrial main method, but obtained silkworm chrysalis oil is used for preparing anti-inflammatory, antianaphylaxis, reducing blood-fat, hypotensive, hypoglycemic, anti-ageing, prevention myocardial infarction, prevention cerebral infarction medicine and/or healthcare products, extract concentrate long with organic solvent recovery time, the problem such as temperature is high, organic solvent residual is very large to the qualitative effects of pupal fat, also have disadvantageous effect to follow-up pupa albumen quality, organic solvent loss further increases product cost.
No. CN101100627A extracting process that patent discloses a kind of silkworm chrysalis oil, adopts supercritical CO
2technology extracts silkworm chrysalis oil, concrete steps: select in high-quality silkworm chrysalis baking oven and carry out drying and make its water content below 5%, pulverized afterwards, choose granularity 10 ~ 80 object silkworm chrysalis grain and be placed in extractor, participation in the election extraction temperature is 15 ~ 50 DEG C, and extraction time is 0.5 ~ 4h, CO
2flow is 15 ~ 35kg/h, and extracting pressure is 10 ~ 30MPa, can obtain rough silkworm chrysalis oil, obtain purer silkworm chrysalis oil after centrifugal removal of impurities through needle-valve, separator, collector.No. CN102746945A patent discloses a kind of method extracting silkworm chrysalis oil, the method by silkworm chrysalis extraction temperature be 55 DEG C, extracting pressure uses supercritical CO under being the condition of 25MPa
2fluid extraction, then separation temperature be 50 ~ 65 DEG C, separating pressure is separated under being the condition of 8 ~ 10MPa, collect liquid, obtain silkworm chrysalis oil.Such adopts supercritical CO
2extraction process, cost is too high, operation and maintenance of the equipment loaded down with trivial details, disposable input is excessive, is not suitable for the large-scale industrial production of silkworm chrysalis oil.
No. CN101781601B patent discloses a kind of method that ultrasonic wave extracts silkworm chrysalis oil from silkworm chrysalis, by silkworm chrysalis pre-treatment, ultrasonic extraction, prepare silkworm chrysalis oil, refinement step forms, compared with solvent extraction method, have employed ultrasonic extraction step, extraction time shortened to 30 minutes by 2 hours, extraction yield brings up to 96.3% by 81.1%, and product yield brings up to 28.9% by 24.3%.But the problems such as the method still needs in a large number with an organic solvent, residual still exist.
No. CN103435716A patent discloses a kind of silkworm chrysalis chitin extraction technology, No. CN103540639A a kind of method that patent discloses aqueous biochemical Production by Enzymes silkworm chrysalis Gly-His-Lys and the silkworm chrysalis dregs of rice, this type of optionally make use of a certain composition in silkworm chrysalis about the research that silkworm chrysalis utilizes, remaining component substantially can only abandon process, cause the significant wastage of resource.
Summary of the invention
Technical problem to be solved by this invention is, there is provided a kind of method of comprehensive utilization of silkworm chrysalis, the problem such as overcome serious waste of resources in existing silkworm chrysalis complete processing, silkworm chrysalis oil organic solvent residual, Silkworm pupa protein fat residue, output is restricted, product sensory is poor.
The technical scheme that the present invention solves the problem is: the method for comprehensive utilization providing a kind of silkworm chrysalis, and described method comprises the steps:
S1, silkworm chrysalis pre-treatment: wet silkworm chrysalis after getting filature, reject bad pupa, joining massfraction is soak 0.5h ~ 3h in the ascorbic acid solution of 0.05% ~ 1%, regulates pH to neutral post-drying, pulverizes to obtain dried silkworm chrysalis meal;
S2, extraction silkworm chrysalis oil: adopt subcritical low-temperature extraction technology, any one in use propane, normal butane, Trimethylmethane is as extraction agent, at temperature is 30 DEG C ~ 50 DEG C, extracts described dried silkworm chrysalis meal, has extracted extraction agent described in rear reduction vaporization, filtered to obtain silkworm chrysalis oil.
In method of comprehensive utilization of the present invention, described step S2 comprises further:
The extraction conditions of described subcritical abstraction technology is: the solid-liquid ratio 1:4 ~ 1:8 of described dried silkworm chrysalis meal and described extraction agent, extracting pressure 0.2MPa ~ 5MPa, and temperature is 30 DEG C ~ 50 DEG C, and extract 1 ~ 2 time, each 0.5h ~ 2h, extraction agent obtains degreasing pupa powder;
By extracting after gained extraction liquid is decompressed to vacuum tightness 0.07MPa ~ 0.1MPa at every turn, at 5 DEG C ~ 40 DEG C, evaporate described extraction agent, filter to obtain silkworm chrysalis oil.
In method of comprehensive utilization of the present invention, described method comprises the steps: further
S3, extraction protein: described degreasing pupa powder is joined in dilute alkaline soln and dissolves, filter to obtain crude protein liquid and pupa slag.
In method of comprehensive utilization of the present invention, described dilute alkaline soln to be mass percent be 0.5% ~ 3% aqueous sodium hydroxide solution, calcium hydroxide aqueous solution, any one in potassium hydroxide aqueous solution.
In method of comprehensive utilization of the present invention, described step S3 comprises further:
S31, decoloration and deodorization: the hydrogen peroxide solution adding mass percent 8% ~ 15% in gained crude protein liquid carries out decoloration and deodorization;
S32, isoelectric precipitation isolated protein: regulate the pH of the crude protein liquid after decoloration and deodorization to iso-electric point 4.0 ~ 4.5 with hydrochloric acid, precipitating proteins, the mode isolated protein of centrifugation and/or membrane sepn;
S33, washing: separating obtained albumen is added ethanol and/or water repetitive scrubbing 2 ~ 5 times;
S34, drying: after washing, gained protein is dry, obtains purified protein powder.
In method of comprehensive utilization of the present invention, described membrane sepn adopts organic membrane or the mineral membrane of molecular weight cut-off 30 ~ 100 kilodalton.
In method of comprehensive utilization of the present invention, described step S34 adopts vacuum lyophilization or spraying dry.
In method of comprehensive utilization of the present invention, described method comprises further:
S4, prepare chitin: gained pupa slag will be filtered after acid-alkali washing, decolouring, deacetylation, rinsing, and dry to obtain refining chitin.
In method of comprehensive utilization of the present invention, described step S4 comprises further:
S41, acid-alkali washing: the hydrochloric acid of described pupa slag functional quality per-cent 2% ~ 4% soaks 20h ~ 40h at 20 DEG C ~ 40 DEG C, after filtration, functional quality per-cent be 3% ~ 8% aqueous sodium hydroxide solution at 70 DEG C ~ 100 DEG C, soak 2h ~ 8h;
S42, decolouring: the pupa slag after acid-alkali washing is filtered, the hydrogen peroxide solution of functional quality per-cent 8% ~ 15% decolours 1h ~ 2h at 40 DEG C ~ 60 DEG C, obtains chitin work in-process;
S43, deacetylation: by described chitin work in-process, functional quality per-cent is that the aqueous sodium hydroxide solution of 35% ~ 55% is at 85 DEG C ~ 100 DEG C deacetylation 3h ~ 6h;
S44, rinsing: clear water rinsing 1h ~ 48h, obtain described refining chitin.
Implement beneficial effect of the present invention to be: the silkworm chrysalis oil produced by the present invention, protein and chitin quality better, nutrient component damages is little, and organic solvent-free remains, and production cost is low, pollutes little in technological process, is applicable to suitability for industrialized production.
Embodiment
Be clearly and completely described to the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
There are the following problems for existing silkworm chrysalis Application way: 1, product quality is poor, there is organic solvent residual in silkworm chrysalis oil, there is organic solvent and fat residue in Silkworm pupa protein, and seldom carry out the process such as screening to bad pupa.2, serious waste of resources, only make use of a certain composition in silkworm chrysalis usually, remaining component substantially can only abandon process.Innovative point of the present invention is: before silkworm chrysalis processing, carry out pre-treatment, ensure the quality of raw material; Adopt subcritical low-temperature extraction technology to extract silkworm chrysalis oil, nutrient component damages is minimum, and organic solvent-free remains; Degreasing pupa powder is subsequently for extracting albumen, and the pupa slag after deproteinated is used for chitin extraction, and stage-by-stage extraction realizes ensureing product quality while resource makes full use of.
The method of comprehensive utilization of silkworm chrysalis of the present invention comprises the steps:
S1, silkworm chrysalis pre-treatment: wet silkworm chrysalis after getting filature, reject bad pupa, joining massfraction is soak 0.5h ~ 3h in the ascorbic acid solution of 0.05% ~ 1%, regulates neutral post-drying, pulverizing.Silkworm chrysalis generally can, with pigment accumulation, cause darkening in necrosis progression, and report is along with serious rancid, does not reject and can have a strong impact on product quality.After bad pupa is rejected, silkworm chrysalis being joined massfraction is soak 0.5h ~ 3h in the ascorbic acid solution of 0.05% ~ 1%, regulate neutral to reduce the silkworm chrysalis oil of subsequent extracted in the aggravation effect of acidic conditions to Oxidation of Fat and Oils, obtain dried silkworm chrysalis meal after oven dry, pulverizing for subsequent use.
S2, extraction silkworm chrysalis oil: adopt subcritical low-temperature extraction technology, any one in use propane, normal butane, Trimethylmethane, as extraction agent, extracts dried silkworm chrysalis meal, has extracted rear reduction vaporization extraction agent, filtered to obtain silkworm chrysalis oil at temperature is 30 DEG C ~ 50 DEG C.Extraction agent used in the present invention is if propane, normal butane or Trimethylmethane boiling point are all lower than zero degree, but to be above the boiling point temperature but lower than critical temperature in extraction temperature, and pressure lower than its emergent pressure when, extraction agent exists with fluid form, namely exist with the form of subcritical fluids, subcritical fluids has excellent diffusion, to apolar substance, there is good perviousness and stronger dissolving power, and have that extraction efficiency is high, good, the eco-friendly unique advantage of production process security.By the lixiviate of subcritical fluids to silkworm chrysalis dry powder, silkworm chrysalis oil is dissolved in extraction agent rapidly, and extraction temperature is 30 DEG C ~ 50 DEG C, can not destroy other nutritive ingredient, does not affect the quality of following protein and chitin.Extraction agent is after solid-liquid separation, reduction vaporization extraction agent, extraction agent used in the present invention is gaseous state under normal temperature environment, therefore in the ordinary course of things (except the place that temperature is extremely low) only needs simple decompression operation extraction agent and volatilizable for gas, non-volatile fraction is silkworm chrysalis oil crude product, remove the silkworm chrysalis dry powder of doping through Plate Filtration or ceramic membrane filter, can silkworm chrysalis oil be obtained.The silkworm chrysalis oil obtained by aforesaid method is as clear as crystal, yellow and bright color, does not have organic solvent residual, is rich in α ~ linolenic acid, as light industry industry and medicine industry raw material, also can directly can use as nutritive health-care grease.
Preferably, the extraction conditions of subcritical abstraction technology used in the present invention is: solid-liquid ratio 1:4 ~ 1:8, extracting pressure 0.2MPa ~ 5MPa, and temperature is 30 DEG C ~ 50 DEG C, and extract 1 ~ 2 time, each 0.5h ~ 2h, extraction agent obtains degreasing pupa powder; To extract at every turn gained extraction liquid decompression after evaporation agent at 5 DEG C ~ 40 DEG C, post-decompression vacuum tightness is 0.07MPa ~ 0.1MPa, filters to obtain silkworm chrysalis oil.Select reextraction technique, suitably can reduce extraction agent and such as select solid-liquid ratio 1:4, and reduce extracting pressure such as 0.2MPa; In single extraction technique, in order to ensure percentage extraction, needing to increase extraction agent volume and such as selecting solid-liquid ratio 1:8.The reduction of extracting pressure and the raising of extraction temperature can extraction efficiencies, and extraction process can be completed the soonest in 1h.The extraction agent of volatilization is drained to extraction agent withdrawing can, makes solvent become liquid state from gaseous state, realize the recycling of extraction agent by pressurized operation.
Preferably, the method for comprehensive utilization of silkworm chrysalis of the present invention, after silkworm chrysalis oil has extracted, also comprises the steps:
S3, extraction protein: degreasing pupa powder is joined in dilute alkaline soln and dissolves, filter to obtain crude protein liquid and pupa slag.Preferably, the dilute alkaline soln that uses of the present invention for mass percent be 0.5% ~ 3% aqueous sodium hydroxide solution, calcium hydroxide aqueous solution, any one in potassium hydroxide aqueous solution.Use dilute alkaline soln stripping protein, the raw material that remaining pupa slag can also extract as chitin.
Preferably, the dilute alkaline soln of solubilising protein can obtain purified protein powder after following steps process:
S31, decoloration and deodorization: the hydrogen peroxide solution adding mass percent 8% ~ 15% in gained crude protein liquid carries out decoloration and deodorization.Silkworm chrysalis has a kind of distinctive fishy odor, can exist if do not removed always, and in silkworm chrysalis, the existence of pigment also can have a strong impact on the quality of obtained protein powder.Existing decolouring and deodorizing technique uses gac etc., and not only can not remove pigment and this fishy odor completely, and often need repeatedly to carry out, considerably increase workload, the gac remained in protein powder also can pollute product.In the homodisperse dilute alkaline soln of protein, add hydrogen peroxide, can realize a decolouring and deodorizing, convenient and swift, the disintegrate of hydrogen peroxide does not have residual yet, and decoloration and deodorization safety thoroughly.
S32, isoelectric precipitation isolated protein: with salt acid for adjusting pH to iso-electric point 4.0 ~ 4.5, precipitating proteins, centrifugation and/or membrane sepn obtain albumen and clear liquid, carry out subsequent disposal, for the preparation of protein powder after collecting protein; Clear liquid is recycled, and is reused for configuration dilute alkaline soln, reduces the water consumption in protein extraction operation, has reclaimed unprecipitated protein in supernatant liquor simultaneously, improve protein recovery.Preferably, described membrane sepn adopts organic membrane or the mineral membrane of molecular weight cut-off 30 ~ 100 kilodalton, the inorganic oxide zirconium etc. of polysulfones PM30, Orelis company of such as Millipore company.Centrifugation and membrane sepn can also be with the use of, and such as, clear liquid mixing repeatedly after membrane sepn, re-uses centrifugation and collect albumen.The clear liquid recycled repeatedly can also remove superfluous mineral ion by the mode of dialysis, avoids impacting isoelectric precipitation.Certainly, crude protein liquid after decoloration and deodorization also first can use organic membrane or the inorganic membrane filtration portion of water of molecular weight cut-off 50 ~ 100 kilodalton, the inorganic oxide zirconium etc. of polysulfones PM50, Orelis company of the Millipore company selected, such as by concentrated 2 ~ 3 times of the crude protein liquid after decoloration and deodorization, then carrying out above-mentioned isoelectric precipitation, separating step.
S33, washing: gained albumen is added ethanol and/or water repetitive scrubbing 2 ~ 5 times.Repetitive scrubbing removes acid, alkali, oxidizer residual, such as, after 1 absolute ethanol washing, in Reusability 2 ~ 4 water washings, still adopts centrifugal mode to realize solid-liquid separation after each washing.
S34, drying: after washing, gained albumen is dry, obtains purified protein powder.Preferably, this drying adopts vacuum lyophilization or spraying dry.
Preferably, after dilute alkaline soln solubilising protein, remaining pupa slag is used for the extraction of chitin, and concrete steps comprise:
S4, prepare chitin: gained pupa slag will be filtered after acid-alkali washing, decolouring, deacetylation, rinsing, and dry to obtain refining chitin.Chitin has anticancer suppression cancer, oncocyte transfer, improves body immunity and liver detoxification effect, is particularly useful for the diseases such as diabetes, liver-kidney diseases, hypertension, obesity, is conducive to prevention cancer cells pathology and chemoradiation therapy treatment tumor disease.
Preferably, the step preparing chitin comprises further:
S41, acid-alkali washing: the hydrochloric acid of described pupa slag functional quality per-cent 2% ~ 4% soaks 20h ~ 40h at 20 DEG C ~ 40 DEG C, after filtration, functional quality per-cent be 3% ~ 8% aqueous sodium hydroxide solution at 70 DEG C ~ 100 DEG C, soak 2h ~ 8h.Use diluted acid and dilute alkaline soln to process pupa slag successively, dilute acid soln Main Function is decalcification and other inorganic salt, dissolves remaining polysaccharide in pupa slag, the impurity such as the further Polysaccharide removing of dilute alkaline soln, albumen simultaneously.
S42, decolouring: filtered by the pupa slag after acid-alkali washing, the hydrogen peroxide solution of functional quality per-cent 8% ~ 15% decolours 1h ~ 2h at 40 DEG C ~ 60 DEG C, obtains chitin work in-process.In chitin work in-process now, chitin content is more than 90%, but does not have the chitin of deacetylation to be difficult to be absorbed by the body, and therefore refining chitin product also needs subsequent disposal.
S43, deacetylation: by described chitin work in-process, functional quality per-cent is that the aqueous sodium hydroxide solution of 35% ~ 55% is at 85 DEG C ~ 100 DEG C deacetylation 3h ~ 6h.High alkali liquid is used to carry out deacetylation under the high temperature conditions; normal reaction 3h ~ 6h; but the deacetylation of a 3h ~ 6h does not make deacetylation complete completely; deacetylation is 40% ~ 50%; after complete reaction, deacetylation is more than 90%; the solubleness of the chitosan produced after complete reaction in water is higher; therefore product yield can greatly be reduced; and deacetylation generally needs to reuse the aqueous sodium hydroxide solution that mass percent is 35% ~ 55% completely, again reacts 3h ~ 6h at 85 DEG C ~ 100 DEG C.
S44, rinsing: clear water rinsing 1h ~ 48h obtains refining chitin.Clear water rinsing is used after can using sodium hydroxide in dilute hydrochloric acid and residual, or repeatedly a large amount of clear water rinsings, now the content of chitin is greater than 99%.
Embodiment 1 extracts silkworm chrysalis oil
I, the bad pupa in wet silkworm chrysalis is rejected, joining mass percent is soak 3h in the ascorbic acid solution of 0.05%, dry rapidly at 60 DEG C after regulating PH to neutrality, pulverized 40 mesh sieves, take the dry dried silkworm chrysalis meal of 20kg, use propane as extraction agent, with solid-liquid ratio 1:4, extracting pressure 0.2MPa, temperature is 50 DEG C, extract 2 times, each 0.5h, by extracting gained extraction liquid at every turn, to be decompressed to vacuum tightness be evaporation agent at 5 DEG C after 0.07MPa ~ 0.1MPa, after filtration residue silkworm chrysalis oil 5.43kg, yield reaches 27.15%, degreasing silkworm chrysalis residual oil content 1.45%.
II, the bad pupa in wet silkworm chrysalis is rejected, joining mass percent is soak 0.5h in the ascorbic acid solution of 1%, dry rapidly at 60 DEG C after regulating PH to neutrality, pulverized 40 mesh sieves, take the dry dried silkworm chrysalis meal of 20kg, use normal butane as extraction agent, with solid-liquid ratio 1:6, extracting pressure 5MPa, temperature is 30 DEG C, extraction 1h, extraction gained extraction liquid being decompressed to vacuum tightness is evaporation agent at 40 DEG C after 0.07MPa ~ 0.1MPa, obtain silkworm chrysalis oil 5.48kg after filtration residue, yield reaches 27.40%, degreasing silkworm chrysalis residual oil content 1.24%.
III, the bad pupa in wet silkworm chrysalis is rejected, joining mass percent is soak 1h in the ascorbic acid solution of 0.1%, dry rapidly at 60 DEG C after regulating PH to neutrality, pulverized 40 mesh sieves, take the dry dried silkworm chrysalis meal of 20kg, use Trimethylmethane as extraction agent, with solid-liquid ratio 1:8, extracting pressure 1MPa, temperature is 40 DEG C, extraction 2h, extraction gained extraction liquid being decompressed to vacuum tightness is evaporation agent at 20 DEG C after 0.07MPa ~ 0.1MPa, obtain silkworm chrysalis oil 5.40kg after filtration residue, yield reaches 27.00%, degreasing silkworm chrysalis residual oil content 1.19%.
Embodiment 2 extracts protein
Degreasing pupa powder after the present embodiment uses the complete silkworm chrysalis oil of extraction in embodiment 1 ~ III extracts protein.
I, extracting degreasing pupa powder 5kg joins mass percent is dissolve in the calcium hydroxide aqueous solution 30L of 0.5%, filter to obtain crude protein liquid and pupa slag, the hydrogen peroxide solution 2L adding 8% in gained crude protein liquid carries out decoloration and deodorization 1h, crude protein liquid iso-electric point 4.0 protein precipitation is regulated with 3mol/L hydrochloric acid, clear liquid and protein is separated with horizontal spiral centrifuge, after 1 absolute ethanol washing, in Reusability 2 water washings, spraying dry gained albumen, obtain purified protein powder 0.714kg, the rate of recovery accounts for 14.28% of degreasing pupa powder.
II, extracting degreasing pupa powder 5kg joins mass percent is dissolve in the potassium hydroxide aqueous solution 30L of 3%, filter to obtain crude protein liquid and pupa slag, the hydrogen peroxide solution 2L adding 15% in gained crude protein liquid carries out decoloration and deodorization 1h, crude protein liquid iso-electric point 4.5 protein precipitation is regulated with 3mol/L hydrochloric acid, clear liquid and protein is separated, Reusability 2 water washings, vacuum lyophilization gained albumen with horizontal spiral centrifuge, obtain purified protein powder 0.783kg, the rate of recovery accounts for 15.66% of degreasing pupa powder.
III, extracting degreasing pupa powder 5kg joins mass percent is dissolve in the aqueous sodium hydroxide solution 30L of 2%, filter to obtain crude protein liquid and pupa slag, the hydrogen peroxide solution 2L adding 10% in gained crude protein liquid carries out decoloration and deodorization 1h, crude protein liquid iso-electric point 4.2 protein precipitation is regulated with 3mol/L hydrochloric acid, clear liquid and protein is separated, Reusability 5 water washings, spraying dry gained albumen with horizontal spiral centrifuge, obtain purified protein powder 0.726kg, the rate of recovery accounts for 14.52% of degreasing pupa powder.
Embodiment 3 chitin extraction
Pupa slag after the present embodiment uses the finished white matter of extraction in embodiment 2 ~ III carrys out chitin extraction.
I, pupa slag 2kg is got; the hydrochloric acid of functional quality per-cent 2% soaks 40h at 40 DEG C; after filtration; functional quality per-cent be 3% aqueous sodium hydroxide solution at 100 DEG C, soak 2h; pupa slag after acid-alkali washing is filtered; the hydrogen peroxide solution of 8% is used to decolour at 60 DEG C 2h; obtain chitin work in-process; functional quality per-cent is that the aqueous sodium hydroxide solution of 35% is at 100 DEG C of deacetylation 6h; clear water rinsing 1h after filtering, obtain refining chitin 50g, the rate of recovery accounts for 2.5% of pupa slag; chitin purity 94%, chitin deacetylase degree is 40% ~ 50%.
II, pupa slag 2kg is got; the hydrochloric acid of functional quality per-cent 4% soaks 20h at 20 DEG C; after filtration; functional quality per-cent be 8% aqueous sodium hydroxide solution at 70 DEG C, soak 8h; pupa slag after acid-alkali washing is filtered; the hydrogen peroxide solution of 15% is used to decolour at 40 DEG C 1h; obtain chitin work in-process; functional quality per-cent is that the aqueous sodium hydroxide solution of 55% is at 85 DEG C of deacetylation 3h; clear water rinsing 48h after filtering, obtain refining chitin 46g, the rate of recovery accounts for 2.3% of pupa slag; chitin purity 96%, chitin deacetylase degree is 40% ~ 50%.
III, pupa slag 2kg is got; the hydrochloric acid of functional quality per-cent 3% soaks 30h at 30 DEG C; after filtration; functional quality per-cent be 5% aqueous sodium hydroxide solution at 80 DEG C, soak 4h; pupa slag after acid-alkali washing is filtered; the hydrogen peroxide solution of 10% is used to decolour at 50 DEG C 1h; obtain chitin work in-process; functional quality per-cent is that the aqueous sodium hydroxide solution of 45% is at 90 DEG C of deacetylation 4h; clear water rinsing 24h after filtering, obtain refining chitin 49g, the rate of recovery accounts for 2.45% of pupa slag; chitin purity 96%, chitin deacetylase degree is 40% ~ 50%.
Claims (9)
1. a method of comprehensive utilization for silkworm chrysalis, is characterized in that, described method comprises the steps:
S1, silkworm chrysalis pre-treatment: wet silkworm chrysalis after getting filature, reject bad pupa, joining massfraction is soak 0.5h ~ 3h in the ascorbic acid solution of 0.05% ~ 1%, regulates pH to neutral post-drying, pulverizes to obtain dried silkworm chrysalis meal;
S2, extraction silkworm chrysalis oil: adopt subcritical low-temperature extraction technology, any one in use propane, normal butane, Trimethylmethane is as extraction agent, at temperature is 30 DEG C ~ 50 DEG C, extracts described dried silkworm chrysalis meal, has extracted extraction agent described in rear reduction vaporization, filtered to obtain silkworm chrysalis oil.
2. method according to claim 1, is characterized in that, described step S2 comprises further:
The extraction conditions of described subcritical abstraction technology is: the solid-liquid ratio 1:4 ~ 1:8 of described dried silkworm chrysalis meal and described extraction agent, extracting pressure 0.2MPa ~ 5MPa, and temperature is 30 DEG C ~ 50 DEG C, and extract 1 ~ 2 time, each 0.5h ~ 2h, extraction agent obtains degreasing pupa powder;
By extracting after gained extraction liquid is decompressed to vacuum tightness 0.07MPa ~ 0.1MPa at every turn, at 5 DEG C ~ 40 DEG C, evaporate described extraction agent, filter to obtain silkworm chrysalis oil.
3. method according to claim 2, is characterized in that, described method comprises the steps: further
S3, extraction protein: described degreasing pupa powder is joined in dilute alkaline soln and dissolves, filter to obtain crude protein liquid and pupa slag.
4. method according to claim 3, is characterized in that, described dilute alkaline soln to be mass percent be 0.5% ~ 3% aqueous sodium hydroxide solution, calcium hydroxide aqueous solution, any one in potassium hydroxide aqueous solution.
5. method according to claim 3, is characterized in that, described step S3 comprises further:
S31, decoloration and deodorization: the hydrogen peroxide solution adding mass percent 8% ~ 15% in gained crude protein liquid carries out decoloration and deodorization;
S32, isoelectric precipitation isolated protein: regulate the pH of the crude protein liquid after decoloration and deodorization to iso-electric point 4.0 ~ 4.5 with hydrochloric acid, precipitating proteins, the mode isolated protein of centrifugation and/or membrane sepn;
S33, washing: separating obtained albumen is added ethanol and/or water repetitive scrubbing 2 ~ 5 times;
S34, drying: after washing, gained protein is dry, obtains purified protein powder.
6. method according to claim 5, is characterized in that, described membrane sepn adopts organic membrane or the mineral membrane of molecular weight cut-off 30 ~ 100 kilodalton.
7. method according to claim 5, is characterized in that, described step S34 adopts vacuum lyophilization or spraying dry.
8. method according to claim 3, is characterized in that, described method comprises further:
S4, prepare chitin: gained pupa slag will be filtered after acid-alkali washing, decolouring, deacetylation, rinsing, and dry to obtain refining chitin.
9. method according to claim 8, is characterized in that, described step S4 comprises further:
S41, acid-alkali washing: the hydrochloric acid of described pupa slag functional quality per-cent 2% ~ 4% soaks 20h ~ 40h at 20 DEG C ~ 40 DEG C, after filtration, functional quality per-cent be 3% ~ 8% aqueous sodium hydroxide solution at 70 DEG C ~ 100 DEG C, soak 2h ~ 8h;
S42, decolouring: the pupa slag after acid-alkali washing is filtered, the hydrogen peroxide solution of functional quality per-cent 8% ~ 15% decolours 1h ~ 2h at 40 DEG C ~ 60 DEG C, obtains chitin work in-process;
S43, deacetylation: by described chitin work in-process, functional quality per-cent is that the aqueous sodium hydroxide solution of 35% ~ 55% is at 85 DEG C ~ 100 DEG C deacetylation 3h ~ 6h;
S44, rinsing: clear water rinsing 1h ~ 48h, obtain described refining chitin.
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| CN201410208938.2A CN105087149A (en) | 2014-05-16 | 2014-05-16 | Comprehensive utilization method of silkworm chrysalis |
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| CN106974253A (en) * | 2017-05-04 | 2017-07-25 | 广西壮族自治区蚕业技术推广总站 | A kind of method of silkworm chrysalis comprehensive utilization |
| CN108285477A (en) * | 2018-03-08 | 2018-07-17 | 浙江汇能生物股份有限公司 | The efficient degreasing method of silkworm chrysalis |
| CN108543055A (en) * | 2018-02-06 | 2018-09-18 | 成都世煌生物科技有限责任公司 | A kind of hero silkworm egg white tiles production technology |
| CN113278669A (en) * | 2021-06-28 | 2021-08-20 | 广西大学 | Silkworm chrysalis peptide and preparation and application thereof |
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| CN113278669A (en) * | 2021-06-28 | 2021-08-20 | 广西大学 | Silkworm chrysalis peptide and preparation and application thereof |
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