CN111012802A - Preparation method and identification method of egg yolk oil - Google Patents

Preparation method and identification method of egg yolk oil Download PDF

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Publication number
CN111012802A
CN111012802A CN201911226599.XA CN201911226599A CN111012802A CN 111012802 A CN111012802 A CN 111012802A CN 201911226599 A CN201911226599 A CN 201911226599A CN 111012802 A CN111012802 A CN 111012802A
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solution
egg yolk
yolk oil
steps
petroleum ether
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张小康
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Anhui Huisongtang Guoji Pharmaceutical Co Ltd
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Anhui Huisongtang Guoji Pharmaceutical Co Ltd
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Priority to CN201911226599.XA priority Critical patent/CN111012802A/en
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K35/00Medicinal preparations containing materials or reaction products thereof with undetermined constitution
    • A61K35/56Materials from animals other than mammals
    • A61K35/57Birds; Materials from birds, e.g. eggs, feathers, egg white, egg yolk or endothelium corneum gigeriae galli
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P17/00Drugs for dermatological disorders
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P17/00Drugs for dermatological disorders
    • A61P17/02Drugs for dermatological disorders for treating wounds, ulcers, burns, scars, keloids, or the like
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P17/00Drugs for dermatological disorders
    • A61P17/04Antipruritics
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/90Plate chromatography, e.g. thin layer or paper chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/16Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Veterinary Medicine (AREA)
  • Physics & Mathematics (AREA)
  • Public Health (AREA)
  • Animal Behavior & Ethology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Medicinal Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • General Physics & Mathematics (AREA)
  • Pathology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Immunology (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Organic Chemistry (AREA)
  • Dermatology (AREA)
  • Biochemistry (AREA)
  • Analytical Chemistry (AREA)
  • Molecular Biology (AREA)
  • Epidemiology (AREA)
  • Plasma & Fusion (AREA)
  • Meat, Egg Or Seafood Products (AREA)

Abstract

The invention relates to a preparation method and an identification method of egg yolk oil, which comprises the following steps: and (3) putting the prepared egg yolk into a pot, heating, and decocting to obtain egg yolk oil. Further comprising the steps of: taking egg yolk oil, adding petroleum ether, washing the solution with an ethanol solution, taking a petroleum ether solution, evaporating the petroleum ether solution to dryness, pouring the evaporated petroleum ether solution into a trichloromethane solution, adding an alumina column into the solution, eluting the solution with petroleum ether and benzene in sequence, eluting with a benzene-acetone mixed solution, collecting an eluent to dryness, pouring residues into 3ml of the trichloromethane solution, sucking a test solution, spotting the test solution on a silica gel G thin-layer plate, developing with benzene-trichloromethane-acetone, taking out and drying, spraying a perchloric acid solution on the dried silica gel G thin-layer plate, and drying to detect an acid value, a saponification value and an iodine value after comparison by a detector.

Description

Preparation method and identification method of egg yolk oil
Technical Field
The invention relates to the field of food processing equipment, in particular to a preparation method and an identification method of egg yolk oil.
Background
The egg yolk oil is oil extracted from egg yolk of eggs, is also called egg fish, phoenix oil and the like, and is a good medicine for treating mild scalds because the egg yolk oil contains rich vitamin A, D, lecithin and the like, has important effects on skin regeneration and metabolism, and has good effect on treating scalds.
In the prior art, the egg yolk oil has rich medicinal value, but the prior preparation method of the egg yolk oil is relatively backward, the extraction rate is relatively low, and the egg yolk oil cannot be identified.
Disclosure of Invention
The invention aims to provide a preparation method and an identification method of egg yolk oil, which are used for solving the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of egg yolk oil comprises the following steps:
1) boiling fresh egg, removing egg shell, and taking out egg yolk for use;
2) putting the egg yolk prepared in the step 1) into a pot, and heating at 80-90 ℃ for 20-30 min;
3) heating to 90-100 deg.C for 20-30min, and decocting to obtain egg yolk oil.
Preferably, the heating in the pot in the step 2) is carried out by mild fire.
More preferably, when the temperature is increased in the step 3), the slow fire is changed into the big fire.
The identification method of egg yolk oil comprises the following steps:
1) taking 2g of egg yolk oil, adding into an open container, adding 50ml of petroleum ether, and stirring in one direction until the egg yolk oil is dissolved;
2) washing the solution with 15ml ethanol solution;
3) repeating the step 2) twice;
4) discarding the ethanol solution, and separating petroleum ether solution;
5) evaporating the petroleum ether solution obtained in the step 4) to dryness to obtain residue;
6) pouring the residue obtained in the step 5) into 2ml of trichloromethane solution to dissolve the residue;
7) adding an alumina column (150 meshes and 200 meshes, the weight of 10g and the inner diameter of 10-15mm) into the solution obtained in the step 6);
8) eluting the solution in the step 7) by using 20ml of petroleum ether and 20ml of benzene in sequence, and discarding the eluent after the elution;
9) then 20ml of benzene-acetone (4: 1) eluting the mixed solution, collecting the eluent, and evaporating to dryness to obtain residue;
10) pouring the residue into 3ml of chloroform solution, and dissolving the residue to obtain a test solution;
11) pipette 2 μ l of the sample solution from step 10) and spot on a silica gel G thin layer plate, and mix the sample solution with benzene-chloroform-acetone (8: 5: 1) after the developing agent is developed, taking out and airing;
12) spraying a 20% perchloric acid solution on the silica gel G thin-layer plate dried in the step 11), drying at 105 ℃ for 5min, and displaying colored spots for detection personnel to compare and then detect the acid value, the saponification value and the iodine value.
Preferably, the method further comprises the following steps:
13) taking β -sitosterol solution as a reference substance, and adding chloroform to prepare a solution with the density of 1 mg/ml;
14) mu.l of the solution from step 13) was taken and spotted on a silica gel G thin layer plate at the same position as the sample solution, and the surface of the silica gel G thin layer plate was coated with benzene-chloroform-acetone (8: 5: 1) after the developing agent is developed, taking out and airing;
15) spraying a 20% perchloric acid solution on the silica gel G thin-layer plate dried in the step 11), drying at 105 ℃ for 5min to display colored spots as a reference for detecting the test solution so as to assist a detector in detecting.
The identification method of egg yolk oil comprises the following steps:
1) 1g of egg oil was added with 30ml of glacial acetic acid-chloroform (6: 1) shaking to dissolve egg oil;
2) adding 1ml of potassium iodide saturated solution into the step 1), and shaking for 1 min;
3) adding 100ml of water and 1ml of starch indicator into the solution in the step 2);
4) continuously carrying out twisting titration on the solution in the step 3) by using sodium thiosulfate titration solution until the blue color disappears, and correcting the titration result by using a blank for a detection person to detect the peroxidation value of the egg yolk oil.
7. The method of claim 6, wherein the identification of egg yolk oil comprises: the consumed sodium thiosulfate titration solution in the step 4) is less than or equal to 1.5 ml.
The identification method of egg yolk oil comprises the following steps:
and (4) carrying out microbial limit inspection according to non-sterile products by using a microbial counting method, a bacteria control detection method and a non-sterile medicine microbial limit standard.
Compared with the prior art, the invention has the beneficial effects that: the egg yolk oil prepared by the preparation method has great medicinal value and higher extraction rate, and three identification methods are provided for comprehensively detecting the acid value, the saponification value, the iodine value and the peroxide value of the egg yolk oil, so that the identification effect is achieved, and the activity of the egg yolk oil is more accurately shown; the egg yolk oil prepared by the preparation method can relieve swelling and remove toxicity, heal sores and promote granulation, and is mainly used for eczema, skin itch, scalds, hand and foot rhagadia and the like.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
The invention provides a technical scheme that: a preparation method of egg yolk oil comprises the following steps:
1) boiling fresh egg, removing egg shell, and taking out egg yolk for use;
2) putting the egg yolk prepared in the step 1) into a pot, and heating at 80-90 ℃ for 20-30 min;
3) heating to 90-100 deg.C for 20-30min, and decocting to obtain egg yolk oil.
As an improvement of the scheme, the step 2) is to heat the pot with slow fire.
As an improvement of the scheme, when the temperature is increased in the step 3), the slow fire is changed into the big fire.
Comparative example 1: the king xx, male, 46 years old, suffered from eczema for 3 years, the egg oil is externally applied for one month, the eczema is obviously improved, the egg oil is continuously used for one year and is completely recovered, and the disease is revisited after three years without relapse.
Comparative example 2: horse xx, female, 52 years old, suffering from tinea manus and pedis for 4 years, the egg oil is externally applied to the affected part, the condition is obviously improved, the egg oil is completely recovered after being continuously used for half a year, and the disease is revisited after three years without relapse.
Comparative example 3: the situation is obviously improved when the egg oil is externally applied to the affected part, the affected part is completely recovered after being continuously used for half a year, and the affected part is visited after three years without relapse.
Example two
The identification method of egg yolk oil comprises the following steps:
1) taking 2g of egg yolk oil, adding into an open container, adding 50ml of petroleum ether, and stirring in one direction until the egg yolk oil is dissolved;
2) washing the solution with 15ml ethanol solution;
3) repeating the step 2) twice;
4) discarding the ethanol solution, and separating petroleum ether solution;
5) evaporating the petroleum ether solution obtained in the step 4) to dryness to obtain residue;
6) pouring the residue obtained in the step 5) into 2ml of trichloromethane solution to dissolve the residue;
7) adding an alumina column (150 meshes and 200 meshes, the weight of 10g and the inner diameter of 10-15mm) into the solution obtained in the step 6);
8) eluting the solution in the step 7) by using 20ml of petroleum ether and 20ml of benzene in sequence, and discarding the eluent after the elution;
9) then 20ml of benzene-acetone (4: 1) eluting the mixed solution, collecting the eluent, and evaporating to dryness to obtain residue;
10) pouring the residue into 3ml of chloroform solution, and dissolving the residue to obtain a test solution;
11) pipette 2 μ l of the sample solution from step 10) and spot on a silica gel G thin layer plate, and mix the sample solution with benzene-chloroform-acetone (8: 5: 1) after the developing agent is developed, taking out and airing;
12) spraying a 20% perchloric acid solution on the silica gel G thin-layer plate dried in the step 11), drying at 105 ℃ for 5min, and displaying colored spots for detection personnel to compare and then detect the acid value, the saponification value and the iodine value.
As a preferable embodiment of the above aspect, the method further includes the steps of:
13) taking β -sitosterol solution as a reference substance, and adding chloroform to prepare a solution with the density of 1 mg/ml;
14) mu.l of the solution from step 13) was taken and spotted on a silica gel G thin layer plate at the same position as the sample solution, and the surface of the silica gel G thin layer plate was coated with benzene-chloroform-acetone (8: 5: 1) after the developing agent is developed, taking out and airing;
15) spraying a 20% perchloric acid solution on the silica gel G thin-layer plate dried in the step 11), drying at 105 ℃ for 5min to display colored spots as a reference for detecting the test solution so as to assist a detector in detecting.
EXAMPLE III
The identification method of egg yolk oil comprises the following steps:
1) 1g of egg oil was added with 30ml of glacial acetic acid-chloroform (6: 1) shaking to dissolve egg oil;
2) adding 1ml of potassium iodide saturated solution into the step 1), and shaking for 1 min;
3) adding 100ml of water and 1ml of starch indicator into the solution in the step 2);
4) continuously carrying out twisting titration on the solution in the step 3) by using sodium thiosulfate titration solution until the blue color disappears, and correcting the titration result by using a blank for a detection person to detect the peroxidation value of the egg yolk oil.
As a modification of the above, the consumed sodium thiosulfate titration solution in the step 4) is less than or equal to 1.5 ml.
Example four
The identification method of egg yolk oil comprises the following steps:
and (4) carrying out microbial limit inspection according to non-sterile products by using a microbial counting method, a bacteria control detection method and a non-sterile medicine microbial limit standard.
While there have been shown and described what are at present considered the fundamental principles and essential features of the invention and its advantages, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (8)

1. A preparation method of egg yolk oil is characterized by comprising the following steps: the method comprises the following steps:
1) boiling fresh egg, removing egg shell, and taking out egg yolk for use;
2) putting the egg yolk prepared in the step 1) into a pot, and heating at 80-90 ℃ for 20-30 min;
3) heating to 90-100 deg.C for 20-30min, and decocting to obtain egg yolk oil.
2. The method for preparing egg yolk oil according to claim 1, wherein the method comprises the following steps: in the step 2), the pan is heated by slow fire.
3. The method for preparing egg yolk oil according to claim 1 or 2, wherein: and 3) when the temperature is raised in the step 3), the slow fire is changed into the big fire.
4. The identification method of egg yolk oil is characterized by comprising the following steps: the method comprises the following steps:
1) taking 2g of egg yolk oil, adding into an open container, adding 50ml of petroleum ether, and stirring in one direction until the egg yolk oil is dissolved;
2) washing the solution with 15ml ethanol solution;
3) repeating the step 2) twice;
4) discarding the ethanol solution, and separating petroleum ether solution;
5) evaporating the petroleum ether solution obtained in the step 4) to dryness to obtain residue;
6) pouring the residue obtained in the step 5) into 2ml of trichloromethane solution to dissolve the residue;
7) adding an alumina column (150 meshes and 200 meshes, the weight of 10g and the inner diameter of 10-15mm) into the solution obtained in the step 6);
8) eluting the solution in the step 7) by using 20ml of petroleum ether and 20ml of benzene in sequence, and discarding the eluent after the elution;
9) then 20ml of benzene-acetone (4: 1) eluting the mixed solution, collecting the eluent, and evaporating to dryness to obtain residue;
10) pouring the residue into 3ml of chloroform solution, and dissolving the residue to obtain a test solution;
11) pipette 2 μ l of the sample solution from step 10) and spot on a silica gel G thin layer plate, and mix the sample solution with benzene-chloroform-acetone (8: 5: 1) after the developing agent is developed, taking out and airing;
12) spraying a 20% perchloric acid solution on the silica gel G thin-layer plate dried in the step 11), drying at 105 ℃ for 5min, and displaying colored spots for detection personnel to compare and then detect the acid value, the saponification value and the iodine value.
5. The method for identifying egg yolk oil according to claim 4, wherein: further comprising the steps of:
13) taking β -sitosterol solution as a reference substance, and adding chloroform to prepare a solution with the density of 1 mg/ml;
14) mu.l of the solution from step 13) was taken and spotted on a silica gel G thin layer plate at the same position as the sample solution, and the surface of the silica gel G thin layer plate was coated with benzene-chloroform-acetone (8: 5: 1) after the developing agent is developed, taking out and airing;
15) spraying a 20% perchloric acid solution on the silica gel G thin-layer plate dried in the step 11), drying at 105 ℃ for 5min to display colored spots as a reference for detecting the test solution so as to assist a detector in detecting.
6. The identification method of egg yolk oil is characterized by comprising the following steps: the method comprises the following steps:
1) 1g of egg oil was added with 30ml of glacial acetic acid-chloroform (6: 1) shaking to dissolve egg oil;
2) adding 1ml of potassium iodide saturated solution into the step 1), and shaking for 1 min;
3) adding 100ml of water and 1ml of starch indicator into the solution in the step 2);
4) continuously carrying out twisting titration on the solution in the step 3) by using sodium thiosulfate titration solution until the blue color disappears, and correcting the titration result by using a blank for a detection person to detect the peroxidation value of the egg yolk oil.
7. The method of claim 6, wherein the identification of egg yolk oil comprises: the consumed sodium thiosulfate titration solution in the step 4) is less than or equal to 1.5 ml.
8. The identification method of egg yolk oil is characterized by comprising the following steps: the method comprises the following steps:
and (4) carrying out microbial limit inspection according to non-sterile products by using a microbial counting method, a bacteria control detection method and a non-sterile medicine microbial limit standard.
CN201911226599.XA 2019-12-04 2019-12-04 Preparation method and identification method of egg yolk oil Pending CN111012802A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113786370A (en) * 2021-11-10 2021-12-14 广州华夏职业学院 Whitening and moisturizing mask and preparation equipment thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113786370A (en) * 2021-11-10 2021-12-14 广州华夏职业学院 Whitening and moisturizing mask and preparation equipment thereof
CN113786370B (en) * 2021-11-10 2023-09-05 广州华夏职业学院 Whitening and moisturizing facial mask mixing equipment

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Application publication date: 20200417