CN108191877A - A kind of method extracted from silkworm excrement and purify chlorophyll - Google Patents
A kind of method extracted from silkworm excrement and purify chlorophyll Download PDFInfo
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- CN108191877A CN108191877A CN201810113154.XA CN201810113154A CN108191877A CN 108191877 A CN108191877 A CN 108191877A CN 201810113154 A CN201810113154 A CN 201810113154A CN 108191877 A CN108191877 A CN 108191877A
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- chlorophyll
- silkworm excrement
- purify
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- softening
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D487/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00
- C07D487/22—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00 in which the condensed system contains four or more hetero rings
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Abstract
The present invention relates to technical field of chemistry, disclose a kind of method extracted from silkworm excrement and purify chlorophyll, are characterized in that：By weight, 100 parts of silkworm excrements are soaked into 30 parts of water, continue 30~60min, silkworm excrement after softening is made；Silkworm excrement after softening is put into extractor, then tetrahydrofuran and silkworm excrement are mixed evenly, mixing time is 30~60min, and extracting solution is made；By extracting solution by ceramic membrane, permeate is made；It will transmit through liquid importing NF membrane and carry out purifying concentration, directional separation chlorophyll；It chlorophyll will be dried after purification by vacuum compression, chlorophyll product is made.Solves the problem of existing from the method for silkworm excrement extraction chlorophyll, obtained impurity is larger, and purity is not high, seriously affects its quality or even can not be used since impurity content is higher, and the solvent extraction process used is cumbersome.
Description
Technical field
The present invention relates to technical field of chemistry, are concretely a kind of methods extracted from silkworm excrement and purify chlorophyll.
Background technology
Chlorophyll largely exists in the blade with plant, industrial means is mainly relied on to be extracted by plant, silkworm excrement
It is the excreta of silkworm, other than being promoted the use of as Chinese medicine, also with other beneficiating ingredients.
Using solvent extraction commonly used in the prior art when handling silkworm excrement, such as alcohol, gasoline, petroleum ether, ether, acetone
Deng due to containing the macromolecular substances such as a large amount of celluloses, hemicellulose, pectin, protein, one side solvent extraction effect in silkworm excrement
Rate is relatively low, and usage amount is big；A large amount of insoluble matters simultaneously（A large amount of cellulose, hemicellulose, pectin, protein etc.）Increase extracting solution
Viscosity, it is serious to restrict subsequent filter speed, virtually increase production cost and time loss.
The chlorophyll extracted from silkworm excrement using the prior art, impurity is larger, and purity is not high, seriously affects its quality, very
To higher and can not be used due to impurity content.It though studies have found that can be according to principle of polarity, using n-hexane to slightly carrying
Object is purified, with obvious effects, but technique is cumbersome, and solvent usage amount is big.
It is a kind of using silkworm excrement as simple, easy to operate, the time-consuming short, cost input of the treatment process of raw material it is therefore desirable to develop
Few, environmental pollution degree is low, and a kind of method extracted from silkworm excrement and purify chlorophyll that purity is high.
Invention content
The present invention is for existing from the method for silkworm excrement extraction chlorophyll, and obtained impurity is larger, and purity is not high, serious shadow
The problem of ring its quality or even can not be used since impurity content is higher, and the solvent extraction process used is cumbersome, carries
For a kind of method extracted from silkworm excrement and purify chlorophyll.
The present invention solves above-mentioned technical problem, the technical solution adopted is that, chlorophyll from silkworm excrement is extracted and purified to one kind
Method include to extraction after silkworm excrement softening, softening, extracting solution filtered, will transmit through liquid purifying and dry.
Further, in silkworm excrement softening, by weight, 100 parts of silkworm excrements are soaked into 30 parts of water, continue 30~
Silkworm excrement after softening is made in 60min.
The purpose designed in this way is, by obtaining swelling after silkworm excrement is impregnated to the degree crumbed with hand, conveniently dispels
Impurity component therein, is conducive to subsequent extracted.
Further, in being extracted after softening, silkworm excrement after softening is put into extractor, then extraction liquor is mixed with silkworm excrement
It stirs evenly, mixing time is 30~60min, and extracting solution is made.
Optionally, extraction liquor is tetrahydrofuran solvent, in parts by weight, tetrahydrofuran solvent and silkworm excrement ratio after softening
It is 6~10：1.
The purpose designed in this way is, the use of tetrahydrofuran is Extraction solvent, and extraction time is short, need not heat, and can incite somebody to action
Chlorophyll in silkworm excrement releases completely, improves extraction efficiency；Secondly tetrahydrofuran can be effectively dissolved in silkworm excrement raw material
Cellulose, hemicellulose, pectin, protein, fatty constituents reduce the viscosity of extracting solution, are conducive to improve the stream of solution
Dynamic property, shortens filtration time.Tetrahydrofuran is used as Extraction solvent, compared with traditional Extraction solvent acetone extraction, significantly
It reduces energy consumption and shortens the production cycle.
Further, extracting solution is filtered, by extracting solution by ceramic membrane, permeate is made.
Further, extracting solution being filtered, operation temperature is 45 DEG C~50 DEG C, goes out film pressure for 0.10~0.15Mpa, with
The Extraction solvent top of 2 times of volumes of trapped fluid is washed, and recycles permeate.
Further, liquid purifying is will transmit through, liquid importing NF membrane is will transmit through and carries out purifying concentration, directional separation chlorophyll.
Optionally, it will transmit through in liquid purifying, operation temperature is 45 DEG C~50 DEG C, goes out film pressure for 0.10~0.15Mpa.
The purpose designed in this way is that the ceramic membrane first step carries out the cellulose, hemicellulose, pectin of some macromoleculars
It removes, second step will transmit through liquid and carry out NF membrane concentrating and purifying, obtain purity higher chlorophyll, and chlorophyll can be completely molten
Liquid is in grease.Bright spot using ceramic membrane and NF membrane is collection purifying and concentrates in one, simple for process, time-consuming few；Not
It needs to use the features such as purification solvent, extraction efficiency are high, and product purity is high.
Ceramic membrane, tube wall gather micropore, and under pressure, material liquid flows in membrane tube or on the outside of film, small molecule object
Matter（Or liquid）Through film, macromolecular substances（Or solid）It is rejected by, so as to reach the mesh such as separation, concentration, purifying and environmental protection
's.According in the range of certain membrane aperture, then permeability is different for the material molecule diameter difference of infiltration, with the pressure of film both sides
For difference for driving force, film is filter medium, under certain pressure effect, when feed liquid flows through film surface, only allow water, inorganic salts,
Small-molecule substance penetrates film, and the macromolecular substances such as suspended matter, glue and microorganism in water is prevented to pass through.Ceramic membrane has separation
Efficient, effect stability, chemical stability are good, acid and alkali-resistance, organic solvent-resistant, resistance to bacterium, high temperature resistant, antipollution, high mechanical strength,
Numerous advantages such as regenerability is good, separation process is simple, low energy consumption, simple and convenient operation and maintenance, service life length, have been applied successfully
In food, beverage, plant（Medicine）The various fields such as object depth processing, biological medicine, fermentation, fine chemistry industry, available in technical process
Separation, clarification, purifying, concentration, degerming, desalination etc..
NF membrane is there are real micropore, and pore diameter range is about one to several nanometers, the retention average molecular matter of film
It is 100~1000 to measure, therefore is referred to as nanometer film.NF membrane selectivity is sharp, while has both ultrafiltration and reverse osmosis separating property,
There is distinctive feature especially for the separation of low-molecular-weight organic matter.The separating-purifying of many low molecular weight active materials includes
Multiple steps, usual final stage are intended to utilize chromatography.A large amount of solvent is needed to elute during chromatographic isolation
And the concentration of bioactive molecule is often very low, it is necessary to be concentrated with thin film evaporation or vacuum evaporation, evaporating concentration process leads to
Often take a long time, easily cause the substance denaturation being purified and decompose.Nanofiltration can replace traditional thin film evaporation, be concentrated in vacuo
The methods of with freeze-drying, increase product design, cycles of concentration can ensure that the rate of recovery of product reaches up to 10 times~50 times
95%~98%。
Optionally, the molecular weight of nanofiltration UF membrane is less than 1000, and NF membrane is hydrophobic structure.
The purpose designed in this way is, nanofiltration separation is suitable for substance of the molecular weight below 1000, and chlorophyll molecule amount
Average out to 900 or so, in the range of this.Select the purifying concentration of hydrophobicity NF membrane, through film it is organic it is molten can be recycled,
And this NF membrane has the performances such as separation accuracy height, solvent resistant, heat-resisting, resistance to oxidation and antipollution.
Extracting solution Determination of Chlorophyll color range after purifying concentration increases nearly 200 times compared with ceramic membrane permeate, entire
During concentrating and purifying, film is to the rejection of chlorophyll more than 98%.Product can be purified while concentration, because
The organic impurities and salt of small molecule, so as to obtain chlorophyll product purity height, will can be completely dissolved in oil with solvent simultaneously through film
In fat.
Permeate is concentrated as being evaporated in vacuo, and evaporating concentration process usually requires for a long time, to easily cause and be purified
Substance denaturation decompose.Nanofiltration can replace traditional vacuum concentration, increase product design, and can ensure that the rate of recovery of product reaches
98%.NF membrane also has separation process without any chemical reaction, and without heating, no phase transition does not destroy bioactivity, in addition
Nanofiltration is energy saving, advantages of environment protection.
Further, it is dry, it chlorophyll will be dried after purification by vacuum compression, chlorophyll product is made.
Beneficial effects of the present invention are at least one below：
1. the use of tetrahydrofuran being Extraction solvent, extraction time is short, need not heat, and can discharge the chlorophyll in silkworm excrement completely
Out, extraction efficiency is improved；Secondly tetrahydrofuran can effectively dissolve cellulose, hemicellulose, pectin, the egg in silkworm excrement raw material
White matter, fatty constituents reduce the viscosity of extracting solution, are conducive to improve the mobility of solution, shorten filtration time.Using
Tetrahydrofuran is Extraction solvent, compared with traditional Extraction solvent acetone extraction, considerably reduces energy consumption and shortens production week
Phase.
2. the ceramic membrane first step is removed the cellulose, hemicellulose, pectin of some macromoleculars, second step will be saturating
It crosses liquid and carries out NF membrane concentrating and purifying, obtain the higher chlorophyll of purity, and chlorophyll energy perfect solution is in grease.Using pottery
The bright spot of porcelain film and NF membrane is collection purifying and concentrates in one, simple for process, time-consuming few；Do not need to using purification solvent,
The features such as extraction efficiency is high, and product purity is high.
3. nanofiltration separation is suitable for substance of the molecular weight below 1000, and chlorophyll molecule amount average out to 900 or so, at this
In a range.The purifying concentration of hydrophobicity NF membrane is selected, organic through film molten can be recycled, and this NF membrane has separation
The performances such as precision height, solvent resistant, heat-resisting, resistance to oxidation and antipollution.
4. the extracting solution Determination of Chlorophyll color range after purifying concentration increases nearly 200 times compared with ceramic membrane permeate, whole
During a concentrating and purifying, film is to the rejection of chlorophyll more than 98%.Product can be purified while concentration, because
Organic impurities and salt for small molecule, so as to obtain chlorophyll product purity height, will can be completely dissolved in solvent simultaneously through film
In grease.
5. permeate is concentrated as being evaporated in vacuo, evaporating concentration process usually requires for a long time, to easily cause pure
The substance denaturation of change is decomposed.Nanofiltration can replace traditional vacuum concentration, increase product design, and can ensure that the rate of recovery of product reaches
98%.NF membrane also has separation process without any chemical reaction, and without heating, no phase transition does not destroy bioactivity, in addition
Nanofiltration is energy saving, advantages of environment protection.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments to the present invention
It is described in further detail.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, it is not used to limit
The fixed present invention.
Embodiment 1
By weight, 100 parts of silkworm excrements are soaked into 30 parts of water, continue 30min, silkworm excrement after softening is made；
Then silkworm excrement after softening is put into extractor, then tetrahydrofuran solvent and silkworm excrement is mixed evenly, wherein tetrahydrochysene
THF solvent is 6 with silkworm excrement weight ratio:Extracting solution is made in 1, mixing time 30min；
By extracting solution by ceramic membrane, permeate is made, ceramic membrane aperture is 0.05 μm, and operation temperature is 45 DEG C, goes out film pressure
It for 0.10Mpa, is washed with the Extraction solvent top of 2 times of volumes of trapped fluid, recycles permeate；
It will transmit through liquid importing NF membrane and carry out purifying concentration, directional separation chlorophyll, operation temperature is 45 DEG C, and going out film pressure is
0.10Mpa, the molecular weight of nanofiltration UF membrane are less than 1000, and NF membrane is hydrophobic structure, obtains chlorophyll after purification；
It chlorophyll will be dried after purification by vacuum compression, chlorophyll product is made.
The use of tetrahydrofuran is Extraction solvent, extraction time is short, need not heat, and can release the chlorophyll in silkworm excrement completely
It releases, improves extraction efficiency；Secondly tetrahydrofuran can effectively dissolve cellulose in silkworm excrement raw material, hemicellulose, pectin,
Protein, fatty constituents reduce the viscosity of extracting solution, are conducive to improve the mobility of solution, shorten filtration time.It adopts
It is Extraction solvent with tetrahydrofuran, compared with traditional Extraction solvent acetone extraction, considerably reduces energy consumption and shorten production
Period.The ceramic membrane first step is removed the cellulose, hemicellulose, pectin of some macromoleculars, and second step will transmit through liquid
NF membrane concentrating and purifying is carried out, obtains the higher chlorophyll of purity, and chlorophyll energy perfect solution is in grease.Using ceramic membrane
Bright spot with NF membrane is collection purifying and concentrates in one, simple for process, time-consuming few；It does not need to using purification solvent, extraction
It is efficient, the features such as product purity is high.Extracting solution Determination of Chlorophyll color range after purifying concentration increases compared with ceramic membrane permeate
Nearly 200 times, during entire concentrate and purify, film is to the rejection of chlorophyll more than 98%.It can be to production while concentration
Product are purified, because the organic impurities and salt of small molecule penetrate film simultaneously with solvent, so as to obtain chlorophyll product purity height,
It can be completely dissolved in grease.
Chlorophyll purity obtained is more than 98%, and the time of preparation is compared with extractions such as traditional acetone, ethyl alcohol, petroleum ethers
Solvent is compared, short without heating, extraction time in extraction process.Such as compared with acetone extraction, three points of extraction time are shortened
Two.It solves in the existing method for extracting chlorophyll from silkworm excrement, obtained impurity is larger, and purity is not high, seriously affects its product
It matter or even can not be used since impurity content is higher, and the problem of the solvent extraction process used is cumbersome.
Embodiment 2
By weight, 100 parts of silkworm excrements are soaked into 30 parts of water, continue 60min, silkworm excrement after softening is made；
Then silkworm excrement after softening is put into extractor, then tetrahydrofuran solvent and silkworm excrement is mixed evenly, wherein tetrahydrochysene
THF solvent is 6 with silkworm excrement weight ratio:Extracting solution is made in 1, mixing time 60min；
By extracting solution by ceramic membrane, permeate is made, ceramic membrane aperture is 0.05 μm, and operation temperature is 50 DEG C, goes out film pressure
It for 0.15Mpa, is washed with the Extraction solvent top of 1.5 times of volumes of trapped fluid, recycles permeate；
It will transmit through liquid importing NF membrane and carry out purifying concentration, directional separation chlorophyll, operation temperature is 50 DEG C, and going out film pressure is
0.15Mpa, the molecular weight of nanofiltration UF membrane are less than 1000, and NF membrane is hydrophobic structure, obtains chlorophyll after purification；
It chlorophyll will be dried after purification by vacuum compression, chlorophyll product is made.
The use of tetrahydrofuran is Extraction solvent, extraction time is short, need not heat, and can release the chlorophyll in silkworm excrement completely
It releases, improves extraction efficiency；Secondly tetrahydrofuran can effectively dissolve cellulose in silkworm excrement raw material, hemicellulose, pectin,
Protein, fatty constituents reduce the viscosity of extracting solution, are conducive to improve the mobility of solution, shorten filtration time.It adopts
It is Extraction solvent with tetrahydrofuran, compared with traditional Extraction solvent acetone extraction, considerably reduces energy consumption and shorten production
Period.The ceramic membrane first step is removed the cellulose, hemicellulose, pectin of some macromoleculars, and second step will transmit through liquid
NF membrane concentrating and purifying is carried out, obtains the higher chlorophyll of purity, and chlorophyll energy perfect solution is in grease.Using ceramic membrane
Bright spot with NF membrane is collection purifying and concentrates in one, simple for process, time-consuming few；It does not need to using purification solvent, extraction
It is efficient, the features such as product purity is high.Extracting solution Determination of Chlorophyll color range after purifying concentration increases compared with ceramic membrane permeate
Nearly 200 times, during entire concentrate and purify, film is to the rejection of chlorophyll more than 98%.It can be to production while concentration
Product are purified, because the organic impurities and salt of small molecule penetrate film simultaneously with solvent, so as to obtain chlorophyll product purity height,
It can be completely dissolved in grease.
Chlorophyll purity obtained is more than 98%, and the time of preparation is compared with extractions such as traditional acetone, ethyl alcohol, petroleum ethers
Solvent is compared, short without heating, extraction time in extraction process.Such as compared with acetone extraction, three points of extraction time are shortened
Two.It solves in the existing method for extracting chlorophyll from silkworm excrement, obtained impurity is larger, and purity is not high, seriously affects its product
It matter or even can not be used since impurity content is higher, and the problem of the solvent extraction process used is cumbersome.
Embodiment 3
By weight, 100 parts of silkworm excrements are soaked into 30 parts of water, continue 45min, silkworm excrement after softening is made；
Then silkworm excrement after softening is put into extractor, then tetrahydrofuran solvent and silkworm excrement is mixed evenly, wherein tetrahydrochysene
THF solvent is 6 with silkworm excrement weight ratio:Extracting solution is made in 1, mixing time 45min；
By extracting solution by ceramic membrane, permeate is made, ceramic membrane aperture is 0.05 μm, and operation temperature is 48 DEG C, goes out film pressure
It for 0.12Mpa, is washed with the Extraction solvent top of 1.0 times of volumes of trapped fluid, recycles permeate；
It will transmit through liquid importing NF membrane and carry out purifying concentration, directional separation chlorophyll, operation temperature is 48 DEG C, and going out film pressure is
0.12Mpa, the molecular weight of nanofiltration UF membrane are less than 1000, and NF membrane is hydrophobic structure, obtains chlorophyll after purification；
It chlorophyll will be dried after purification by vacuum compression, chlorophyll product is made.
The use of tetrahydrofuran is Extraction solvent, extraction time is short, need not heat, and can release the chlorophyll in silkworm excrement completely
It releases, improves extraction efficiency；Secondly tetrahydrofuran can effectively dissolve cellulose in silkworm excrement raw material, hemicellulose, pectin,
Protein, fatty constituents reduce the viscosity of extracting solution, are conducive to improve the mobility of solution, shorten filtration time.It adopts
It is Extraction solvent with tetrahydrofuran, compared with traditional Extraction solvent acetone extraction, considerably reduces energy consumption and shorten production
Period.The ceramic membrane first step is removed the cellulose, hemicellulose, pectin of some macromoleculars, and second step will transmit through liquid
NF membrane concentrating and purifying is carried out, obtains the higher chlorophyll of purity, and chlorophyll energy perfect solution is in grease.Using ceramic membrane
Bright spot with NF membrane is collection purifying and concentrates in one, simple for process, time-consuming few；It does not need to using purification solvent, extraction
It is efficient, the features such as product purity is high.Extracting solution Determination of Chlorophyll color range after purifying concentration increases compared with ceramic membrane permeate
Nearly 200 times, during entire concentrate and purify, film is to the rejection of chlorophyll more than 98%.It can be to production while concentration
Product are purified, because the organic impurities and salt of small molecule penetrate film simultaneously with solvent, so as to obtain chlorophyll product purity height,
It can be completely dissolved in grease.
Chlorophyll purity obtained is more than 98%, and the time of preparation is compared with extractions such as traditional acetone, ethyl alcohol, petroleum ethers
Solvent is compared, short without heating, extraction time in extraction process.Such as compared with acetone extraction, three points of extraction time are shortened
Two.It solves in the existing method for extracting chlorophyll from silkworm excrement, obtained impurity is larger, and purity is not high, seriously affects its product
It matter or even can not be used since impurity content is higher, and the problem of the solvent extraction process used is cumbersome.
Claims (10)
- A kind of 1. method extracted from silkworm excrement and purify chlorophyll, which is characterized in that including being carried after softening to silkworm excrement, softening It takes, extracting solution is filtered, will transmit through liquid purifying and drying.
- 2. a kind of method extracted from silkworm excrement and purify chlorophyll according to claim 1, it is characterised in that：The silkworm Sand softening, by weight, 100 parts of silkworm excrements is soaked into 30 parts of water, continue 30~60min, and silkworm excrement after softening is made.
- 3. a kind of method extracted from silkworm excrement and purify chlorophyll according to claim 2, it is characterised in that：It is described soft It is extracted after change, silkworm excrement after softening is put into extractor, then extraction liquor is mixed evenly with silkworm excrement, mixing time 30 Extracting solution is made in~60min.
- 4. a kind of method extracted from silkworm excrement and purify chlorophyll according to claim 3, it is characterised in that：It is described to carry Liquor is taken as tetrahydrofuran solvent, in parts by weight, tetrahydrofuran solvent is 6~10 with silkworm excrement ratio after softening：1.
- 5. a kind of method extracted from silkworm excrement and purify chlorophyll according to claim 3, it is characterised in that：It is described to incite somebody to action Extracting solution filters, and by extracting solution by ceramic membrane, permeate is made.
- 6. a kind of method extracted from silkworm excrement and purify chlorophyll according to claim 5, it is characterised in that：It is described to incite somebody to action Extracting solution filters, and operation temperature is 45 DEG C~50 DEG C, goes out film pressure for 0.10~0.15Mpa, with the extraction of 2 times of volumes of trapped fluid Solvent top is washed, and recycles permeate.
- 7. a kind of method extracted from silkworm excrement and purify chlorophyll according to claim 3, it is characterised in that：It is described to incite somebody to action Permeate purifies, and will transmit through liquid importing NF membrane and carries out purifying concentration, directional separation chlorophyll obtains chlorophyll after purification.
- 8. a kind of method extracted from silkworm excrement and purify chlorophyll according to claim 7, it is characterised in that：It is described to incite somebody to action Permeate purifies, and operation temperature is 45 DEG C~50 DEG C, goes out film pressure for 0.10~0.15Mpa.
- 9. a kind of method extracted from silkworm excrement and purify chlorophyll according to claim 7, it is characterised in that：It is described to receive The molecular weight of filter membrane separation is less than 1000, and NF membrane is hydrophobic structure.
- 10. a kind of method extracted from silkworm excrement and purify chlorophyll according to claim 7, it is characterised in that：It is described It is dry, it chlorophyll will be dried after purification by vacuum compression, chlorophyll product is made.
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Citations (3)
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|---|---|---|---|---|
| CN1425015A (en) * | 1999-12-01 | 2003-06-18 | 耶达研究及发展有限公司 | Chlorophyll and bacteriochlorophyll esters, and their preparation |
| CN103961381A (en) * | 2013-01-24 | 2014-08-06 | 中国林业科学研究院林产化学工业研究所 | Method for negative-pressure boiling extraction and preparation of low-acid ginkgo extract |
| CN105461822A (en) * | 2015-12-24 | 2016-04-06 | 佛山职业技术学院 | Method for extracting effective components from silkworm excrement |
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2018
- 2018-02-05 CN CN201810113154.XA patent/CN108191877A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1425015A (en) * | 1999-12-01 | 2003-06-18 | 耶达研究及发展有限公司 | Chlorophyll and bacteriochlorophyll esters, and their preparation |
| CN103961381A (en) * | 2013-01-24 | 2014-08-06 | 中国林业科学研究院林产化学工业研究所 | Method for negative-pressure boiling extraction and preparation of low-acid ginkgo extract |
| CN105461822A (en) * | 2015-12-24 | 2016-04-06 | 佛山职业技术学院 | Method for extracting effective components from silkworm excrement |
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Application publication date: 20180622 |