CN104194927A - Method for extracting egg yolk oil, lecithin and egg yolk protein polypeptide powder from egg yolk powder - Google Patents
Method for extracting egg yolk oil, lecithin and egg yolk protein polypeptide powder from egg yolk powder Download PDFInfo
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- CN104194927A CN104194927A CN201410387475.0A CN201410387475A CN104194927A CN 104194927 A CN104194927 A CN 104194927A CN 201410387475 A CN201410387475 A CN 201410387475A CN 104194927 A CN104194927 A CN 104194927A
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- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention discloses a method for extracting egg yolk oil, lecithin and egg yolk protein polypeptide powder from egg yolk powder. The method comprises the following steps: carrying out supercritical CO2 fluid extraction on egg yolk powder to obtain egg yolk oil and deoiled egg yolk powder; performing alcohol extraction on the deoiled egg yolk powder and filtering to obtain ethanol extract, decompressing, distilling, condensing and drying to obtain lecithin; drying filter residue obtained from filtering to obtain coarse protein powder; and purifying and fining the deoiled and degreased coarse protein powder through a membrane separation technology to obtain egg yolk protein polypeptide powder. The method disclosed by the invention is high in product quality, high in extraction efficiency and free from residue of harmful solvent, and controls temperature within 50 DEG C and avoids loss of bioactivity of the lecithin; the obtained egg yolk oil, lecithin and egg yolk powder are relatively high in purity, and active ingredients of the egg yolk powder are utilized fully; and the method is applicable to industrial production; edible ethanol serves as an organic solvent, to avoid residue of an organic solvent; and from the perspective of food safety, harm to human bodies is avoided.
Description
Technical field
The present invention relates to yolk powder processing technique field.
Background technology
In egg yolk, contain lipid, protein, moisture, saccharic, inorganic salt etc., yolk is the part that in egg, nutritive value enriches the most.Yolk powder is that to adopt the yolk of Fresh Egg be raw material, makes through filtration, homogeneous, pasteurize, spraying, the multiple working procedure such as dry.The main component of yolk powder is Oil of egg yolk (claim again neutral lipid, main component is triglyceride level and cholesterol, is about 40%), Yelkin TTS (approximately 17%) and vitellin(Vt) (being about 40%).Traditional high temperature decocting method can extract Oil of egg yolk and Yelkin TTS in the lump, but Yelkin TTS will lose activity after exceeding 50 DEG C, and the sticky shape that the Oil of egg yolk obtaining is brown color, have the smell that is difficult for being accepted, and extraction efficiency is low; Organic solvent extractionprocess can obtain highly purified Oil of egg yolk and Yelkin TTS, but complex process, and noxious solvent residue problem cannot solve; Although the method such as column chromatography and membrane separation process can obtain the Yelkin TTS of higher concentration, treatment capacity is limited is not suitable for industrial production.
The development of China's Ovum Gallus domesticus Flavus lecithin is relatively backward, highly purified Ovum Gallus domesticus Flavus lecithin all need to be from external import, domestic market outlook are very wide, potentiality are very large, in addition, the leftover materials that extract from yolk powder after Ovum Gallus domesticus Flavus lecithin are at present abandoned, and this material contains a large amount of protein, therefore in the urgent need to a technology, ensure not only can high efficiency extraction Yelkin TTS in but also can make full use of leftover materials.The high extraction, high-quality that this invention has and without residual etc. the advantage of hazardous solvent, has very important economy and social effect for suitability for industrialized production.
Summary of the invention
Technical problem solved by the invention is, a kind of extracting method is provided, and can obtain purity is high, stability is strong Oil of egg yolk, Yelkin TTS, and yolk protein polypeptide powder.
The technical solution used in the present invention is, from the method for yolk powder extraction Oil of egg yolk, Yelkin TTS and yolk protein polypeptide powder, to comprise the following steps:
A. get yolk powder and mix with uniform filling and put into extraction kettle material barrel, the volume ratio of yolk powder and filler is 1:2, continual by 40 DEG C of above CO with topping-up pump
2squeeze in extraction kettle, start continuous extraction, extraction kettle temperature is 40 DEG C-49 DEG C, pressure is 25MPa-32MPa, separating still temperature is 40 DEG C-56 DEG C, and pressure is 6MPa-9MPa, and continuous extraction extracts Oil of egg yolk for 180 minutes-240 minutes, collecting the Oil of egg yolk in separating still, is de-oiling yolk powder in material barrel;
B. the de-oiling yolk powder in extraction kettle material barrel is separated with filler, the edible ethanol solution that de-oiling yolk powder is 80%-98% with concentration mixes, and fully stirs and extracts 40 minutes-140 minutes;
C. adopt vacuum filter to carry out suction filtration to mixing solutions, pore size filter is 10 microns-25 microns, obtains ethanol extract, filter residue is collected stand-by;
D. the ethanol extract in step c is carried out to underpressure distillation concentrated, and drying treatment, Yelkin TTS obtained; Dry with Vacuumdrier to the filter residue in step c, volatilization residual ethanol, obtains crude protein powder;
E. by the crude protein powder in steps d, grind, sieve, obtain protein powder; Every 100g protein powder adds 1900 ml waters, and stirring at room temperature mixes protein liquid in 30 minutes;
F. protein liquid step e being obtained is preheating to 37 DEG C, and regulating pH value with the sodium hydroxide of 2mol/L is 8.1, adds the trypsinase of 1g to be hydrolyzed 3 hours, and reaction finishes sterilizing in 10 minutes at latter 90 DEG C, and cool to room temperature is adjusted pH value to 9;
G. by common filter paper filtering, to reduce the pollution of impurity to film, retention filtrate is stand-by;
H. the micropore filtering film that is 0.45 μ m to the filtrate employing aperture in step g filters, and the auxiliary vaccum-pumping equipment that uses is accelerated feed liquid by the speed of microfiltration membrane, and retention filtrate is stand-by;
I, uses ultra-filtration equipment to filter the filtrate in step h, working pressure 0.2Mpa; Service temperature is room temperature; Membrane flux is 25mL/h, and retention filtrate is stand-by.
J. get the filtrate in step I, filter through nanofiltration device, the effective film area of nanofiltration membrane is 0.4m
2, pure water flux is 6-8L/h, processes by the nanofiltration membrane of 300Da molecular weight cut-off, obtains trapped substance;
K. by the material lyophilize of holding back, micronizing, 1000 orders, obtain yolk protein polypeptide powder.
The invention has the beneficial effects as follows, this method quality product is high, and extraction efficiency is high, residual without hazardous solvent, and temperature is no more than 50 DEG C, avoids the physiologically active of Yelkin TTS to lose; The Oil of egg yolk obtaining, Yelkin TTS, and the purity of yolk powder is higher, makes full use of the active principle of yolk powder, and applicable suitability for industrialized production; It is edible ethanol that organic solvent uses, and avoids organic solvent residual, considers from the angle of food safety, can not work the mischief to human body.
Brief description of the drawings
Fig. 1 is operational flowchart of the present invention.
Embodiment
Below in conjunction with embodiment, get the yolk powder of same batch, through qualification, Oil of egg yolk content is wherein 50%, the content of Yelkin TTS is 8.4%.
Embodiment mono-:
A. get yolk powder and mix with uniform filling and put into extraction kettle material barrel, the volume ratio of yolk powder and filler is 1:2, continual by 40 DEG C of above CO with topping-up pump
2squeeze in extraction kettle, start continuous extraction, extraction kettle temperature is 46 DEG C, and pressure is 30MPa, and separating still temperature is 51 DEG C, and pressure is 8MPa, and continuous extraction extracts Oil of egg yolk 141g for 200 minutes, collects the Oil of egg yolk in separating still, is de-oiling yolk powder in material barrel;
B. the de-oiling yolk powder of extraction kettle material barrel is separated with filler, the edible ethanol solution that de-oiling yolk powder is 92% with concentration mixes, and fully stirs and extracts 100 minutes;
C. adopt vacuum filter to carry out suction filtration to mixing solutions, pore size filter is 10 microns-25 microns, obtains ethanol extract, filter residue is collected stand-by;
D. the ethanol extract in step c is carried out to pressure distillation concentrated, and drying treatment, Yelkin TTS 22.428g obtained; Dry with Vacuumdrier to the filter residue in step c, volatilization residual ethanol, obtains crude protein powder 127.572g;
E. by the crude protein powder in steps d, grind, sieve, obtain protein powder; Every 100g protein powder adds 1900 ml waters and is mixed with the protein liquid that concentration is 5% (W/V), and stirring at room temperature mixes protein liquid in 30 minutes;
F. protein liquid step e being obtained is preheating to 40 DEG C, and being adjusted to needed pH with the sodium hydroxide of 2mol/L is 8.1, adds the reaction that is hydrolyzed of the trypsinase of 3g, that is to say that trypsinase add-on is 3% of crude protein opaque amount; Hydrolysis 4h, reaction finishes sterilizing in 10 minutes at latter 90 DEG C, and it is 9 that cool to room temperature is adjusted pH;
G. by common filter paper filtering, to reduce the pollution of impurity to film, obtain filtered liquid;
H. adopting aperture is that the micropore filtering film of 0.45 μ m filters, and the auxiliary vaccum-pumping equipment that uses is accelerated feed liquid by the speed of microfiltration membrane, obtains filtered liquid;
I. use ultra-filtration equipment, working pressure 0.2Mpa; Service temperature is room temperature; Membrane flux is 25mL/h, protein liquid is carried out to ultrafiltration and further hold back macromole impurity and the low high molecular weight protein of physiologically active, thereby allow active substance material permeance ultra-filtration membrane, obtains filtered liquid.
J. through nanofiltration device, nanofiltration can be held back active polypeptide and be allowed salt ion at a low price see through, and plays the object of the concentrated active polypeptide of purifying and product section desalination, and the effective film area of nanofiltration membrane is 0.4m
2, pure water flux is 6-8L/h, processes by the nanofiltration membrane of 300Da molecular weight cut-off, obtains trapped substance;
K. by the material lyophilize of holding back, micronizing, 1000 orders, obtain 84g yolk protein polypeptide powder.
Embodiment bis-
A. get yolk powder 300g and mix with uniform filling and put into extraction kettle material barrel, the volume ratio of yolk powder and filler is 1:2, continual by 40 DEG C of above CO with topping-up pump
2squeeze in extraction kettle, start continuous extraction, extraction kettle temperature is 49 DEG C, and pressure is 32MPa, and separating still temperature is 56 DEG C, and pressure is 9MPa, and continuous extraction extracts Oil of egg yolk 147g for 240 minutes, collects the Oil of egg yolk in separating still, is de-oiling yolk powder in material barrel;
B. the de-oiling yolk powder in extraction kettle material barrel is separated with filler, the edible ethanol solution that de-oiling yolk powder is 98% with concentration mixes, and fully stirs and extracts 140 minutes;
C. adopt vacuum filter to carry out suction filtration to mixing solutions, pore size filter is 10 microns-25 microns, obtains ethanol extract, filter residue is collected stand-by;
D. the ethanol extract in step c is carried out to underpressure distillation concentrated, and drying treatment, Yelkin TTS 23.94g obtained; Dry with Vacuumdrier to the filter residue in step c, volatilization residual ethanol, obtains crude protein powder 126.06g;
E. by the crude protein powder in steps d, grind, sieve, obtain protein powder; Every 100g protein powder adds 1900 ml waters and is mixed with the protein liquid that concentration is 5% (W/V), and stirring at room temperature mixes protein liquid in 30 minutes;
F. protein liquid step e being obtained is preheating to 45 DEG C, and being adjusted to needed pH with the sodium hydroxide of 2mol/L is 8.1, the trypsin trypsinase add-on that adds 5g be crude protein opaque amount 5%) reaction is hydrolyzed; Hydrolysis 4.5h, reaction finishes sterilizing in 10 minutes at latter 90 DEG C, and it is 9 that cool to room temperature is adjusted pH;
G. by common filter paper filtering, to reduce the pollution of impurity to film, obtain filtered liquid;
H. adopting aperture is that the micropore filtering film of 0.45 μ m filters, and the auxiliary vaccum-pumping equipment that uses is accelerated feed liquid by the speed of microfiltration membrane, obtains filtered liquid;
I. use ultra-filtration equipment, working pressure 0.2Mpa; Service temperature is room temperature; Membrane flux is 25mL/h, protein liquid is carried out to ultrafiltration and further hold back macromole impurity and the low high molecular weight protein of physiologically active, thereby allow active substance material permeance ultra-filtration membrane, obtains filtered liquid;
J. through nanofiltration device, nanofiltration can be held back active polypeptide and be allowed salt ion at a low price see through, and plays the object of the concentrated active polypeptide of purifying and product section desalination, and the effective film area of nanofiltration membrane is 0.4m
2, pure water flux is 6-8L/h, processes by the nanofiltration membrane of 300Da molecular weight cut-off, obtains trapped substance;
K. by the material lyophilize of holding back, micronizing, 1000 orders, obtain 81g yolk protein polypeptide powder.
Embodiment tri-
A. get yolk powder 300g and mix with uniform filling and put into extraction kettle material barrel, the volume ratio of yolk powder and filler is 1:2, continual by 40 DEG C of above CO with topping-up pump
2squeeze in extraction kettle, start continuous extraction, extraction kettle temperature is 40 DEG C, pressure is 25MPa, and separating still temperature is 40 DEG C, and pressure is 6.5MPa, continuous extraction extracts Oil of egg yolk 120g for 180 minutes, collects the Oil of egg yolk in separating still, is de-oiling yolk powder in material barrel;
B. the de-oiling yolk powder in extraction kettle material barrel is separated with filler, the edible ethanol solution that de-oiling yolk powder is 80% with concentration mixes, and fully stirs and extracts 40 minutes;
C. adopt vacuum filter to carry out suction filtration to mixing solutions, pore size filter is 10 microns-25 microns, obtains ethanol extract, filter residue is collected stand-by;
D. the ethanol extract in step c is carried out to underpressure distillation concentrated, and drying treatment, Yelkin TTS 20.16g obtained; Dry with Vacuumdrier to the filter residue in step c, volatilization residual ethanol, obtains crude protein powder 129.84g;
E. by the crude protein powder in steps d, grind, sieve, obtain protein powder; Every 100g protein powder adds 1900 ml waters and is mixed with the protein liquid that concentration is 5% (W/V), and stirring at room temperature mixes protein liquid in 30 minutes;
F. protein liquid step e being obtained is preheating to 43 DEG C, being adjusted to needed pH with the sodium hydroxide of 2mol/L is 8.1, the trypsin trypsinase add-on that adds 3g be crude protein opaque amount 3%) reaction is hydrolyzed, hydrolysis 4h, reaction finishes sterilizing in 10 minutes at latter 90 DEG C, and it is 9 that cool to room temperature is adjusted pH;
G. by common filter paper filtering, to reduce the pollution of impurity to film, obtain filtered liquid;
H. adopting aperture is that the micropore filtering film of 0.45 μ m filters, and the auxiliary vaccum-pumping equipment that uses is accelerated feed liquid by the speed of microfiltration membrane, obtains filtered liquid;
I. use ultra-filtration equipment, working pressure 0.2Mpa; Service temperature is room temperature; Membrane flux is 25mL/h, protein liquid is carried out to ultrafiltration and further hold back macromole impurity and the low high molecular weight protein of physiologically active, thereby allow active substance material permeance ultra-filtration membrane, obtains filtered liquid.
J. through nanofiltration device, nanofiltration can be held back active polypeptide and be allowed salt ion at a low price see through, and plays the object of the concentrated active polypeptide of purifying and product section desalination, and the effective film area of nanofiltration membrane is 0.4m
2, pure water flux is 6-8L/h, processes by the nanofiltration membrane of 300Da molecular weight cut-off, obtains trapped substance;
K. by the material lyophilize of holding back, micronizing, 1000 orders, obtain 87.7g yolk protein polypeptide powder.
Embodiment tetra-, considers extraction yield and production cost, and embodiment tetra-is most preferred embodiment:
A. get yolk powder 300g and mix with uniform filling and put into extraction kettle material barrel, the volume ratio of yolk powder and filler is 1:2, continual by 40 DEG C of above CO with topping-up pump
2squeeze in extraction kettle, start continuous extraction, extraction kettle temperature is 43 DEG C, pressure is 25MPa, and separating still temperature is 46 DEG C, and pressure is 7.5MPa, continuous extraction extracts Oil of egg yolk 132g for 200 minutes, collects the Oil of egg yolk in separating still, is de-oiling yolk powder in material barrel;
B. the de-oiling yolk powder in extraction kettle material barrel is separated with filler, the edible ethanol solution that de-oiling yolk powder is 82% with concentration mixes, and fully stirs and extracts 40 minutes-140 minutes;
C. adopt vacuum filter to carry out suction filtration to mixing solutions, pore size filter is 10 microns-25 microns, obtains ethanol extract, filter residue is collected stand-by;
D. the ethanol extract in step c is carried out to underpressure distillation concentrated, and drying treatment, Yelkin TTS 21.168g obtained; Dry with Vacuumdrier to the filter residue in step c, volatilization residual ethanol, obtains crude protein powder 128.832g;
E. by the crude protein powder in steps d, grind, sieve, obtain protein powder; Every 100g protein powder adds 1900 ml waters and is mixed with the protein liquid that concentration is 5% (W/V), and stirring at room temperature mixes protein liquid in 30 minutes;
F. protein liquid step e being obtained is preheating to 37 DEG C, being adjusted to needed pH with the sodium hydroxide of 2mol/L is 8.1, the trypsin trypsinase add-on that adds 1g be crude protein opaque amount 1%) reaction is hydrolyzed, hydrolysis 3h, reaction finishes sterilizing in 10 minutes at latter 90 DEG C, and it is 9 that cool to room temperature is adjusted pH;
G. by common filter paper filtering, to reduce the pollution of impurity to film, obtain filtered liquid;
H. adopting aperture is that the micropore filtering film of 0.45 μ m filters, and the auxiliary vaccum-pumping equipment that uses is accelerated feed liquid by the speed of microfiltration membrane, obtains filtered liquid;
I. use ultra-filtration equipment, working pressure 0.2Mpa; Service temperature is room temperature; Membrane flux is 25mL/h, protein liquid is carried out to ultrafiltration and further hold back macromole impurity and the low high molecular weight protein of physiologically active, thereby allow active substance material permeance ultra-filtration membrane, obtains filtered liquid.
J. through nanofiltration device, nanofiltration can be held back active polypeptide and be allowed salt ion at a low price see through, and plays the object of the concentrated active polypeptide of purifying and product section desalination, and the effective film area of nanofiltration membrane is 0.4m
2, pure water flux is 6-8L/h, processes by the nanofiltration membrane of 300Da molecular weight cut-off, obtains trapped substance;
K. by the material lyophilize of holding back, micronizing, 1000 orders, obtain 87g yolk protein polypeptide powder.
Claims (6)
1. the method for extracting Oil of egg yolk, Yelkin TTS and yolk protein polypeptide powder from yolk powder, comprises the following steps:
A. get yolk powder and mix with uniform filling and put into extraction kettle material barrel, the volume ratio of yolk powder and filler is 1:2, continual by 40 DEG C of above CO with topping-up pump
2squeeze in extraction kettle, start continuous extraction, extraction kettle temperature is 40 DEG C-49 DEG C, pressure is 25MPa-32MPa, separating still temperature is 40 DEG C-56 DEG C, and pressure is 6MPa-9MPa, and continuous extraction extracts Oil of egg yolk for 180 minutes-240 minutes, collecting the Oil of egg yolk in separating still, is de-oiling yolk powder in material barrel;
B. the de-oiling yolk powder in extraction kettle material barrel is separated with filler, the edible ethanol solution that de-oiling yolk powder is 80%-98% with concentration mixes, and fully stirs and extracts 40 minutes-140 minutes;
C. adopt vacuum filter to carry out suction filtration to mixing solutions, pore size filter is 10 microns-25 microns, obtains ethanol extract, filter residue is collected stand-by;
D. the ethanol extract in step c is carried out to underpressure distillation concentrated, and drying treatment, Yelkin TTS obtained; Dry with Vacuumdrier to the filter residue in step c, volatilization residual ethanol, obtains crude protein powder;
E. by the crude protein powder in steps d, grind, sieve, obtain protein powder; Every 100g protein powder adds 1900 ml waters, and stirring at room temperature mixes protein liquid in 30 minutes;
F. protein liquid step e being obtained is preheating to 37 DEG C-45 DEG C, regulating pH value with the sodium hydroxide of 2mol/L is 8.1, adding weight is that the trypsinase of crude protein grain weight amount 1%-5% is hydrolyzed 3 hours-4.5 hours, reaction finishes sterilizing in 10 minutes at latter 90 DEG C, and cool to room temperature is adjusted pH value to 9;
G. by common filter paper filtering, to reduce the pollution of impurity to film, retention filtrate is stand-by;
H. the micropore filtering film that is 0.45 μ m to the filtrate employing aperture in step g filters, and the auxiliary vaccum-pumping equipment that uses is accelerated feed liquid by the speed of microfiltration membrane, and retention filtrate is stand-by;
I, uses ultra-filtration equipment to filter the filtrate in step h, working pressure 0.2Mpa; Service temperature is room temperature; Membrane flux is 25mL/h, and retention filtrate is stand-by.
J. get the filtrate in step I, filter through nanofiltration device, the effective film area of nanofiltration membrane is 0.4m
2, pure water flux is 6-8L/h, processes by the nanofiltration membrane of 300Da molecular weight cut-off, obtains trapped substance;
K. by the material lyophilize of holding back, micronizing, 1000 orders, obtain yolk protein polypeptide powder.
2. the method for extracting Oil of egg yolk, Yelkin TTS and yolk protein polypeptide powder from yolk powder as claimed in claim 1, is characterized in that: in steps d, adopt Rotary Evaporators or vacuum vaporation system to process ethanol extract.
3. the method for extracting Oil of egg yolk, Yelkin TTS and yolk protein polypeptide powder from yolk powder as claimed in claim 1, is characterized in that: in step a, filler material is stainless steel, and filler specification is: CS-E-3, CS-E-5, CS-E-8, CS-E-10.
4. the method for extracting Oil of egg yolk, Yelkin TTS and yolk protein polypeptide powder from yolk powder as claimed in claim 1, is characterized in that: in step b, extraction kettle temperature is 46 DEG C, and extraction kettle pressure is 30MPa, and separating still temperature is 51 DEG C, and separating still pressure is 7.5MPa.
5. the method for extracting Oil of egg yolk, Yelkin TTS and yolk protein polypeptide powder from yolk powder as claimed in claim 1, is characterized in that: the vacuum filter in steps d is stainless steel suction filtration device, and pore size filter is 20 microns.
6. the method for extracting Oil of egg yolk, Yelkin TTS and yolk protein polypeptide powder from yolk powder as claimed in claim 1, is characterized in that: be 37 DEG C by protein liquid preheating temperature in step f, adding proteolytic enzyme weight is 1% of crude protein grain weight amount.
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CN107596728A (en) * | 2017-09-21 | 2018-01-19 | 珠海澳盈生物科技有限公司 | Using supercritical CO2The method for extracting egg oil |
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Cited By (9)
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CN105018220A (en) * | 2015-08-10 | 2015-11-04 | 四川联成迅康医药股份有限公司 | Preparation method of egg yolk oil |
CN106561968A (en) * | 2016-10-25 | 2017-04-19 | 广州白云山汉方现代药业有限公司 | Egg yolk protein powder product capable of being suspended stably in water and preparation method thereof |
CN106561968B (en) * | 2016-10-25 | 2020-08-11 | 广州白云山汉方现代药业有限公司 | Yolk protein powder product capable of being stably suspended in water and preparation method thereof |
CN107569868A (en) * | 2017-09-21 | 2018-01-12 | 珠海澳盈生物科技有限公司 | Using supercritical CO2The method for extracting de-fatted egg yolk powder |
CN107596728A (en) * | 2017-09-21 | 2018-01-19 | 珠海澳盈生物科技有限公司 | Using supercritical CO2The method for extracting egg oil |
CN113088372A (en) * | 2021-03-27 | 2021-07-09 | 浙江康莱特药业有限公司 | Novel preparation process of egg yolk oil |
CN113214314A (en) * | 2021-04-30 | 2021-08-06 | 广州白云山汉方现代药业有限公司 | Preparation method of yolk lecithin with long-term stability |
CN113214314B (en) * | 2021-04-30 | 2024-02-20 | 广州白云山汉方现代药业有限公司 | Preparation method of long-term stable egg yolk lecithin |
CN114868843A (en) * | 2022-06-28 | 2022-08-09 | 睿迪生物科技(深圳)有限公司 | Special artificial milk for aseptic young mice and preparation method thereof |
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