AU2020101598A4 - Egg yolk lecithin extraction and quality fidelity technology - Google Patents
Egg yolk lecithin extraction and quality fidelity technology Download PDFInfo
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- AU2020101598A4 AU2020101598A4 AU2020101598A AU2020101598A AU2020101598A4 AU 2020101598 A4 AU2020101598 A4 AU 2020101598A4 AU 2020101598 A AU2020101598 A AU 2020101598A AU 2020101598 A AU2020101598 A AU 2020101598A AU 2020101598 A4 AU2020101598 A4 AU 2020101598A4
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- lecithin
- egg yolk
- extraction
- purity
- yolk lecithin
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- JQWAHKMIYCERGA-UHFFFAOYSA-N (2-nonanoyloxy-3-octadeca-9,12-dienoyloxypropoxy)-[2-(trimethylazaniumyl)ethyl]phosphinate Chemical compound CCCCCCCCC(=O)OC(COP([O-])(=O)CC[N+](C)(C)C)COC(=O)CCCCCCCC=CCC=CCCCCC JQWAHKMIYCERGA-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000000605 extraction Methods 0.000 title claims abstract description 29
- 239000000787 lecithin Substances 0.000 claims abstract description 59
- 229940067606 lecithin Drugs 0.000 claims abstract description 59
- 235000010445 lecithin Nutrition 0.000 claims abstract description 59
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 claims abstract description 57
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003480 eluent Substances 0.000 claims abstract description 10
- 239000000741 silica gel Substances 0.000 claims abstract description 10
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 10
- WTJKGGKOPKCXLL-RRHRGVEJSA-N phosphatidylcholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCCC=CCCCCCCCC WTJKGGKOPKCXLL-RRHRGVEJSA-N 0.000 claims abstract description 9
- 239000012141 concentrate Substances 0.000 claims abstract description 8
- 210000002969 egg yolk Anatomy 0.000 claims abstract description 8
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 7
- 238000000746 purification Methods 0.000 claims abstract description 7
- 102000002322 Egg Proteins Human genes 0.000 claims abstract description 5
- 108010000912 Egg Proteins Proteins 0.000 claims abstract description 5
- 238000005238 degreasing Methods 0.000 claims abstract description 5
- 235000013345 egg yolk Nutrition 0.000 claims abstract description 5
- 235000013601 eggs Nutrition 0.000 claims abstract description 5
- 238000010828 elution Methods 0.000 claims abstract description 5
- 244000144977 poultry Species 0.000 claims abstract description 5
- 230000005526 G1 to G0 transition Effects 0.000 claims abstract description 4
- 238000004440 column chromatography Methods 0.000 claims abstract description 4
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 45
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- 239000012065 filter cake Substances 0.000 claims description 8
- 108010046377 Whey Proteins Proteins 0.000 claims description 6
- 102000007544 Whey Proteins Human genes 0.000 claims description 6
- 235000006708 antioxidants Nutrition 0.000 claims description 6
- 235000021119 whey protein Nutrition 0.000 claims description 6
- 239000000230 xanthan gum Substances 0.000 claims description 6
- 229920001285 xanthan gum Polymers 0.000 claims description 6
- 229940082509 xanthan gum Drugs 0.000 claims description 6
- 235000010493 xanthan gum Nutrition 0.000 claims description 6
- 229930003427 Vitamin E Natural products 0.000 claims description 5
- 230000003078 antioxidant effect Effects 0.000 claims description 5
- 239000011162 core material Substances 0.000 claims description 5
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229940092258 rosemary extract Drugs 0.000 claims description 5
- 235000020748 rosemary extract Nutrition 0.000 claims description 5
- 239000001233 rosmarinus officinalis l. extract Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000011709 vitamin E Substances 0.000 claims description 5
- 235000019165 vitamin E Nutrition 0.000 claims description 5
- 229940046009 vitamin E Drugs 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 3
- 238000004945 emulsification Methods 0.000 claims description 3
- 239000000839 emulsion Substances 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000000265 homogenisation Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000008213 purified water Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 238000001694 spray drying Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 230000007423 decrease Effects 0.000 claims description 2
- 239000002024 ethyl acetate extract Substances 0.000 claims description 2
- 239000002198 insoluble material Substances 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 abstract description 4
- 239000003094 microcapsule Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 239000003153 chemical reaction reagent Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 6
- 235000013305 food Nutrition 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 150000003904 phospholipids Chemical class 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- TZCPCKNHXULUIY-RGULYWFUSA-N 1,2-distearoyl-sn-glycero-3-phosphoserine Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@H](COP(O)(=O)OC[C@H](N)C(O)=O)OC(=O)CCCCCCCCCCCCCCCCC TZCPCKNHXULUIY-RGULYWFUSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- JZNWSCPGTDBMEW-UHFFFAOYSA-N Glycerophosphorylethanolamin Natural products NCCOP(O)(=O)OCC(O)CO JZNWSCPGTDBMEW-UHFFFAOYSA-N 0.000 description 2
- ZWZWYGMENQVNFU-UHFFFAOYSA-N Glycerophosphorylserin Natural products OC(=O)C(N)COP(O)(=O)OCC(O)CO ZWZWYGMENQVNFU-UHFFFAOYSA-N 0.000 description 2
- 239000013527 degreasing agent Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 150000008104 phosphatidylethanolamines Chemical class 0.000 description 2
- 150000003905 phosphatidylinositols Chemical class 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000005237 degreasing agent Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 125000005313 fatty acid group Chemical group 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000007902 hard capsule Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007901 soft capsule Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
- A23B5/00—Preservation of eggs or egg products
- A23B5/08—Preserving with chemicals
- A23B5/12—Preserving with chemicals in the form of liquids or solids
- A23B5/14—Organic compounds; Microorganisms; Enzymes
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B5/00—Preserving by using additives, e.g. anti-oxidants
- C11B5/0092—Mixtures
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K35/00—Medicinal preparations containing materials or reaction products thereof with undetermined constitution
- A61K35/56—Materials from animals other than mammals
- A61K35/57—Birds; Materials from birds, e.g. eggs, feathers, egg white, egg yolk or endothelium corneum gigeriae galli
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/10—Refining fats or fatty oils by adsorption
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Microbiology (AREA)
- General Chemical & Material Sciences (AREA)
- Zoology (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Fats And Perfumes (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention discloses an egg yolk lecithin extraction and quality fidelity
technology. The extraction method includes: degreasing, extraction of lecithin, and
purification of lecithin. For purification, silica gel is used as the stationary phase of
column chromatography, and ethanol-water solution is used as the elution. The
gradient of the reagent is gradually eluted, and the polarity of the eluent is gradually
increased, that is, the ethanol concentration is reduced from a 100% gradient to 80%,
and the flow rate is 1-3mL/min. Collect the eluent containing a single
phosphatidylcholine and vacuum, concentrate to obtain lecithin with purity>95%.
The invention can establish the extraction of high-purity lecithin, and at the same
time useing microcapsule technology to process egg yolk lecithin, so as to improve
the stability of lecithin and extend the shelf life of the product.
DRAWINGS
Poultry eggs - Egg yolk Degrasing Stand at low Vacuum
''I temperature filtration
Lecithin with a purity of Concentrate Vacuum Ethanol
75%-85% filtration extraction
Purification - Concentrate - Lecithin with Microencapsulation
a purity >95%
Antioxidants
Fig. 1
Description
Poultry eggs - Egg yolk Degrasing Stand at low Vacuum ''I temperature filtration
Lecithin with a purity of Concentrate Vacuum Ethanol 75%-85% filtration extraction
Purification - Concentrate - Lecithin with Microencapsulation a purity >95%
Antioxidants
Fig. 1
Egg yolk lecithin extraction and quality fidelity technology Technical field: The invention belongs to the technical field of food processing and extraction, and particularly relates to the extraction and quality fidelity technology of egg yolk lecithin. Background technique: Lecithin is a phosphorus-containing polar lipid substance, known as the "third nutrient" alongside protein and vitamins. The most abundant source of lecithin is egg yolk, which contains about 10% of the total dry matter. Lecithin is widely used in the fields of food, medicine, cosmetics and feed industry due to its unique physical and chemical properties and physiological effects. Lecithin is broadly and narrowly defined. Lecithin in a broad sense refers to a mixture of various phospholipids, including phosphatidylcholine (PC), phosphatidylethanolamine (PE), phosphatidylinositol (PI), and phosphatidylserine (PS). Lecithin in the narrow sense refers specifically to phosphatidylcholine (PC). The difference in the quality of lecithin mainly depends on the content of the phosphatidylcholine, the biologically active component, so this substance can be used as an indicator to measure the purity of lecithin. The current research on lecithin mainly focuses on the extraction of high-purity lecithin and the development of lecithin health food. The existing lecithin health products on the market mainly include tablets, granules, oral liquid, soft capsules, hard capsules and other products. However, due to the poor stability of lecithin, its fatty acid structure makes it susceptible to oxidation reactions caused by factors such as air, temperature, moisture, light and other factors, resulting in color browning and quality degradation, which has led to the development of lecithin products. Very restrictive. Therefore, how to maintain the quality of lecithin has gradually become the focus of research. The invention uses microcapsule technology to process egg yolk lecithin to improve the stability of lecithin and extend the shelf life of the product.
Summary of the invention: The present invention is aimed at the defects and deficiencies of the existing lecithin extraction technology and product stabilization, and provides an egg yolk lecithin extraction and quality fidelity technology, which realizes the extraction of high-purity lecithin and uses microcapsule technology to process egg yolk lecithin , effectively improve the quality and use value of the final product. The first object of the present invention is to provide a method for extracting egg yolk lecithin. The steps of the above method are as follows: (1) Degreasing: picking fresh poultry eggs, washing and breaking the shell, separating the yolk liquid, adding food-grade ethyl acetate, stirring at room temperature, then standing at low temperature, suction filtration to obtain filter cake, drying the filter cake to obtain Powdery ethyl acetate insolubles; (2) Extraction of lecithin: taking the powdery ethyl acetate insoluble material obtained in step (1) as raw material, adding edible ethanol for extraction, the filtrate is concentrated to obtain lecithin with a purity of 78-85%; (3) Purification of lecithin: silica gel is used as the stationary phase of column chromatography, and ethanol-water solution is used as the eluent for gradient elution. The polarity of the eluent gradually increases, that is, the ethanol concentration decreases from a 100% gradient To 80%, the flow rate is 1-3mL/min, collect the eluent containing a single
DESCRIPTION phosphatidylcholine, and concentrate in vacuo to obtain lecithin with purity>95%. The method of the present invention is further provided that, in step (1), the volume ratio of the egg yolk liquid: ethyl acetate is 1:1 to 4, and the drying temperature of the filter cake is 40 to °C; In step (2), the above powdery ethyl acetate insoluble matter: edible ethanol is in a volume ratio of 1:1 to 8, the extraction temperature is 35 to 45°C, the extraction time is 1 to 2 hours, and the concentration of the edible ethanol is 80 to 100 %; In step (3), the particle size of the above-mentioned silica gel is 100-150 mesh, and the addition amount is 40-75% of the column volume; dissolve 2-8% of the crude lecithin by weight of the silica gel in 2-10 times the volume of absolute ethanol and then apply Thus, the above vacuum concentration temperature is lower than 45°C. The method of the present invention is further configured to add 0.05 to 0.2% of an antioxidant to the lecithin with a purity of >95%. The method of the present invention is further provided that the above-mentioned antioxidant is compounded with vitamin E and fat-soluble rosemary extract in a volume ratio of 3:1. The method of the present invention is further configured such that the above-mentioned concentration gradient change value is 1%-3%. The method of the present invention is further configured to place the ethyl acetate extract at -4°C and let it stand for 5-8 hours to separate the neutral oil and lecithin. The second object of the present invention is to provide an egg yolk lecithin quality fidelity technology, first preparing the above egg yolk lecithin; the above egg yolk lecithin quality fidelity technology includes the following steps: a. Dissolve whey protein and xanthan gum in purified water at 40 ~ 50 C, mix evenly, as a wall material; b. Slowly add the lecithin with purity> 95% in step (3) as the core material to the wall material solution, and stir the mixed solution for 20-40min; c. Shear emulsification: emulsify the mixed liquid at 6000~-14000r/min speed for 2~8min; d. Homogenization: Homogenize at a pressure of 30 to 45MPa for 1 to 3 times; e. Spray drying: The homogenized emulsion is spray dried to prepare microencapsulated egg yolk lecithin. The method of the present invention is further configured such that the mass ratio of whey protein to xanthan gum is 4:1. The method of the present invention is further provided that the core material: wall material solution has a mass ratio of 1:1 to 5.
The advantages of the present invention are: (1) The present invention uses food-grade ethyl acetate for degreasing, which is safer than the ordinary degreasing agent acetone, and effectively improves the subsequent extraction rate and purity of egg yolk lecithin. (2) The present invention uses 100-150 mesh renewable silica gel as the adsorbent, and uses gradient elution method to purify lecithin. It does not require pressurization during the operation, and can ensure the separation effect. To reduce production costs. (3) The present invention uses vitamin E and fat-soluble rosemary extract as a protective
DESCRIPTION agent to inhibit the oxidation of high-purity lecithin and significantly improve its quality. (4) In the present invention, egg yolk lecithin is microencapsulated, which significantly improves the stability of lecithin and enhances its slow release performance. (5) All steps of the present invention are carried out below 50°C, and the natural activity and nutritional function characteristics of egg yolk lecithin are kept to the greatest extent.
Brief Description Fig. 1 is a flowchart of the present invention. Detailed Description The present invention will be further described below in conjunction with specific embodiments. Without departing from the spirit and essence of the present invention, modifications or replacements made to the methods, steps, or conditions of the present invention belong to the scope of the present invention. Unless otherwise specified, the technical means used in the embodiments are those skilled in the art Familiar routines. Example 1 An extraction method of egg yolk lecithin, the method steps are as follows: (1) Degreasing: Select fresh poultry eggs, wash and break the shells to separate the yolks, add 1-4 times the volume of food grade ethyl acetate, and stir at room temperature for 0.5-1h. Then put it at low temperature and let it filter to obtain filter cake. The filter cake is dried at 4045°C to obtain powdery ethyl acetate insoluble matter. The use of food-grade ethyl acetate as a degreaser for egg yolk lecithin effectively improves the purity of lecithin. (2) Extraction of lecithin: the powdery ethyl acetate insolubles obtained in step (1) is used as the raw material, the fixed material-liquid ratio is 1:1-8, the extraction temperature is 35-45°C, and the extraction time is 1-2h , Add edible ethanol with a concentration of 80-100% for extraction, and the filtrate can be concentrated to obtain lecithin with a purity of 78-85%. (3) Purification of lecithin: use silica gel with a particle size of 100-150 mesh as the stationary phase of column chromatography, add an amount of 40-75% of the column volume, dissolve crude lecithin with a silica gel weight of 2-8% in 2~ After loading 10 times volume of absolute ethanol, the sample was eluted with different concentrations of ethanol solution (gradually reduced from 100% to 80%) as the eluent, the flow rate was controlled at 1-3mL/min, and the single phospholipid was collected. The eluent of acylcholine is concentrated under vacuum below 45°C to obtain lecithin with purity >95%. To this concentrate is added 0.05-0.2% antioxidant, vitamin E: fat-soluble rosemary extract = 3:1. The gradient elution method was used to effectively separate phosphatidylcholine and other phospholipids, which significantly increased the concentration of lecithin. Vitamin E is combined with fat-soluble rosemary extract as a protective agent for lecithin, which inhibits the oxidation of high-purity lecithin and significantly improves its quality. Example 2 With reference to Example 1, a quality fidelity technology for egg yolk lecithin, first prepare high-purity egg yolk lecithin as disclosed in Example 1. The quality fidelity technology for egg yolk lecithin includes the following steps: a. Dissolve whey protein and xanthan gum at a mass ratio of 4:1 in purified water at 4050°C, mix evenly, and use it as a wall material;
DESCRIPTION b. The high-purity lecithin obtained in step (3) is slowly added to the wall material solution at a ratio of core material: wall material of 1:1 to 5, and the mixed solution is stirred for 20 to 40 minutes; c. Shear emulsification: emulsify the mixed liquid at 6000~-14000r/min speed for 2~8min; d. Homogenization: Homogenize at a pressure of 30 to 45MPa for 1 to 3 times; e. Spray drying: The homogenized emulsion is spray dried to prepare microencapsulated egg yolk lecithin. The lecithin has high biological activity, stable performance and long shelf life. The mixture of whey protein and xanthan gum is used as the wall material, and the lecithin is treated with microcapsule technology to improve the stability of the lecithin product and extend its shelf life. The above are only the preferred embodiments of the present invention, and the scope of protection of the present invention is not limited to the examples, and all technical solutions that belong to the idea of the present invention belong to the scope of protection of the present invention. It should be noted that for those of ordinary skill in the art, several improvements and retouching without departing from the principles of the present invention, these improvements and retouching should also be regarded as the scope of protection of the present invention.
Claims (9)
- CLAIMS 1. An extraction method of egg yolk lecithin, characterized in that the method steps are as follows: (1) Degreasing: picking fresh poultry eggs, washing and breaking the shell, separating the yolk liquid, adding food-grade ethyl acetate, stirring at room temperature, then standing at low temperature, suction filtration to obtain filter cake, drying the filter cake to obtain Powdery ethyl acetate insolubles; (2) Extraction of lecithin: taking the powdery ethyl acetate insoluble material obtained in step (1) as raw material, adding edible ethanol for extraction, the filtrate is concentrated to obtain lecithin with a purity of 78-85%; (3) Purification of lecithin: silica gel is used as the stationary phase of column chromatography, and ethanol-water solution is used as the eluent for gradient elution. The polarity of the eluent gradually increases, that is, the ethanol concentration decreases from a 100% gradient to 80%, the flow rate is 1-3mL/min, collect the eluent containing a single phosphatidylcholine, and concentrate in vacuo to obtain lecithin with purity>95%.
- 2. The method for extracting egg yolk lecithin according to claim 1, characterized in that: in step (1), the volume ratio of the egg yolk liquid: ethyl acetate is 1:1-4, and the filter cake is dried The temperature is 40-45°C; in step (2), the powdery ethyl acetate insoluble matter: edible ethanol is in a volume ratio of 1:1 to 8, the extraction temperature is 35 to 45°C, the extraction time is 1 to 2 hours, and the concentration of the edible ethanol is 80 ~ 10 0 %;in step (3), the particle size of the silica gel is 100-150 mesh, and the addition amount is -75% of the column volume; after dissolving 2-8% of the crude lecithin by weight of the silica gel in 2-10 volumes of absolute ethanol Sample loading, the vacuum concentration temperature is lower than 45 C.
- 3. The method for extracting egg yolk lecithin according to claim 1, wherein an antioxidant of 0.05-0.2% is added to the lecithin with a purity of >95%.
- 4. The method for extracting egg yolk lecithin according to claim 3, wherein the antioxidant is compounded by vitamin E and fat-soluble rosemary extract in a volume ratio of 3:1.
- 5. The method for extracting egg yolk lecithin according to claim 1, wherein the concentration gradient change value is 1%- 3 %.
- 6. The method for extracting egg yolk lecithin according to claim 1, wherein the ethyl acetate extract is left at 0-4°C for 5-8 hours to separate neutral oil and lecithin.
- 7. The quality fidelity technology of egg yolk lecithin, characterized in that the egg yolk lecithin according to any one of claims 1-5 is first prepared; the quality fidelity technology of egg yolk lecithin includes the following steps: a. Dissolve whey protein and xanthan gum in purified water at 40 ~ 50 C, mix evenly, as a wall material; b. Slowly add lecithin with a purity of >95% as the core material in the step (3) to the wall material solution, and stir the mixed solution for 20-40min; c. Shear emulsification: emulsify the mixed liquid at 6000~-14000r/min speed for 2-8min; d. Homogenization: Homogenize at a pressure of 30 to 45MPa for 1 to 3 times; e. Spray drying: The homogenized emulsion is spray dried to prepare microencapsulated egg yolk lecithin.
- 8. The fidelity technology of egg yolk lecithin according to claim 6, wherein the mass ratioCLAIMS of whey protein to xanthan gum is 4:1.
- 9. The fidelity technology of egg yolk lecithin according to claim 7, wherein the mass ratio of the core material to the wall material solution is 1:1 to 5.Fig. 1 DRAWINGS
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| CN113528603A (en) * | 2021-07-09 | 2021-10-22 | 浙江省农业科学院 | Method for co-producing pig brain proliferation promoting peptide-phospholipid in brain |
| CN113528603B (en) * | 2021-07-09 | 2024-04-12 | 浙江省农业科学院 | Pig brain proliferation-promoting peptide-in-brain phospholipid co-production method |
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