CN107789407B - Extraction process of flavonoids of chaenomeles speciosa - Google Patents
Extraction process of flavonoids of chaenomeles speciosa Download PDFInfo
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- 229930003935 flavonoid Natural products 0.000 title claims abstract description 103
- 235000017173 flavonoids Nutrition 0.000 title claims abstract description 103
- 150000002215 flavonoids Chemical class 0.000 title claims abstract description 100
- 240000000425 Chaenomeles speciosa Species 0.000 title claims abstract description 50
- 235000005078 Chaenomeles speciosa Nutrition 0.000 title claims abstract description 50
- 238000000605 extraction Methods 0.000 title claims abstract description 27
- 235000009467 Carica papaya Nutrition 0.000 claims abstract description 64
- 241000219173 Carica Species 0.000 claims abstract description 57
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000000843 powder Substances 0.000 claims abstract description 33
- 239000000047 product Substances 0.000 claims abstract description 27
- 238000000227 grinding Methods 0.000 claims abstract description 25
- 239000012074 organic phase Substances 0.000 claims abstract description 24
- 239000012071 phase Substances 0.000 claims abstract description 18
- 239000013067 intermediate product Substances 0.000 claims abstract description 17
- 238000005360 mashing Methods 0.000 claims abstract description 13
- 238000007599 discharging Methods 0.000 claims abstract description 9
- 239000002002 slurry Substances 0.000 claims abstract description 9
- 238000002791 soaking Methods 0.000 claims abstract description 9
- 239000011347 resin Substances 0.000 claims abstract description 8
- 229920005989 resin Polymers 0.000 claims abstract description 8
- 238000001704 evaporation Methods 0.000 claims abstract description 5
- 230000008020 evaporation Effects 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 74
- 239000011259 mixed solution Substances 0.000 claims description 30
- LZDKZFUFMNSQCJ-UHFFFAOYSA-N 1,2-diethoxyethane Chemical compound CCOCCOCC LZDKZFUFMNSQCJ-UHFFFAOYSA-N 0.000 claims description 24
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 18
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 12
- 235000013399 edible fruits Nutrition 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000005520 cutting process Methods 0.000 claims description 7
- 239000011148 porous material Substances 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 abstract description 21
- 239000003960 organic solvent Substances 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 9
- 239000002274 desiccant Substances 0.000 abstract description 5
- 239000007787 solid Substances 0.000 abstract description 5
- 238000007605 air drying Methods 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000004537 pulping Methods 0.000 abstract description 2
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 66
- 238000000746 purification Methods 0.000 description 30
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 20
- XCIXKGXIYUWCLL-UHFFFAOYSA-N cyclopentanol Chemical compound OC1CCCC1 XCIXKGXIYUWCLL-UHFFFAOYSA-N 0.000 description 17
- 229960005070 ascorbic acid Drugs 0.000 description 10
- 235000010323 ascorbic acid Nutrition 0.000 description 10
- 239000011668 ascorbic acid Substances 0.000 description 10
- 230000002000 scavenging effect Effects 0.000 description 9
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 8
- 240000006432 Carica papaya Species 0.000 description 7
- 244000251905 Pseudocydonia sinensis Species 0.000 description 7
- 235000017831 Pseudocydonia sinensis Nutrition 0.000 description 7
- 235000006264 Asimina triloba Nutrition 0.000 description 6
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 5
- 229930003944 flavone Natural products 0.000 description 5
- 150000002212 flavone derivatives Chemical class 0.000 description 5
- 235000011949 flavones Nutrition 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 5
- -1 flavonoid compounds Chemical class 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000002292 Radical scavenging effect Effects 0.000 description 2
- 235000004789 Rosa xanthina Nutrition 0.000 description 2
- 241000220222 Rosaceae Species 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 244000144730 Amygdalus persica Species 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 241001507936 Chaenomeles Species 0.000 description 1
- 241000723267 Diospyros Species 0.000 description 1
- 235000011511 Diospyros Nutrition 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 241000721662 Juniperus Species 0.000 description 1
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 1
- 244000141359 Malus pumila Species 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 235000006040 Prunus persica var persica Nutrition 0.000 description 1
- 241000220324 Pyrus Species 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 235000021016 apples Nutrition 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003467 diminishing effect Effects 0.000 description 1
- 235000011869 dried fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 239000002420 orchard Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000021017 pears Nutrition 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 150000003648 triterpenes Chemical class 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/73—Rosaceae (Rose family), e.g. strawberry, chokeberry, blackberry, pear or firethorn
- A61K36/732—Chaenomeles, e.g. flowering quince
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/31—Extraction of the material involving untreated material, e.g. fruit juice or sap obtained from fresh plants
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
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- Coloring Foods And Improving Nutritive Qualities (AREA)
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Abstract
The invention discloses an extraction process of flavonoids in chaenomeles speciosa, which comprises the following steps: (1) adding fructus Chaenomelis pulp and water into tissue mashing machine, mashing; (2) pulping; (3) air-drying the slurry; (4) crushing the air-dried product, grinding the crushed product into powder and discharging the powder to obtain shine skin papaya powder; (5) adding shine skin papaya powder into water, and soaking to obtain an intermediate product A; (6) adding an organic solvent into the intermediate product A, and stirring; (7) standing for layering, separating out an organic phase, extracting the water phase twice with the same amount of organic solvent, and combining the three organic phases; (8) adding a solid desiccant into the organic phase, removing the solid desiccant, and removing the organic solvent by reduced pressure evaporation on a rotary evaporator; (9) and (4) adsorbing and purifying the product obtained in the step (8) by using D140 macroporous resin. The method for extracting flavonoids from chaenomeles speciosa has the advantages of simple operation process, low cost and mild requirements, and is suitable for large-scale popularization and application.
Description
The application is a divisional application with the name of 'a method for extracting flavonoids from shine skin papaya', the application date of which is 2015, 3 and 5, and the application number of which is 201510097303.4.
Technical Field
The invention relates to a method for extracting functional components from pawpaw, in particular to a process for extracting flavonoids from shine skin pawpaw.
Background
Papaya (Chaenomeles sinensis) is a plant of the genus Chaenomeles of the family Rosaceae (Rosaceae), and is also called Chaenomeles speciosa because its dried fruit peel is still smooth and non-shrunken. The fruit is rich in nutrition, contains rich compounds such as organic acid, amino acid, polysaccharide, flavone, triterpene and glycosides thereof, has the effects of resisting bacteria, diminishing inflammation, resisting tumors and the like, is one of novel economic trees which integrate edibility, medicine and appreciation and have high development value, and has wide market prospect. At present, pawpaw is used as a characteristic medicinal material and a processed edible fruit in many places such as Shandong lotus, Hubei Yunyu county, Shaanxi Baihe, Henan juniper and the like.
For a long time, the cultivation of the chaenomeles speciosa adopts seedlings to build an orchard, and the yield is uneven. Meanwhile, the processing and utilization basis of the papaya product is weak, and the papaya product is influenced by the low price of the traditional Chinese medicine in China, so that the benefit is low, and the smooth papaya is mainly used for enjoying value. However, the glabrous skin papaya contains a large amount of flavonoid compounds, wherein the highest content of the flavonoid compounds in the glabrous skin papaya in the Changsha producing area can reach 34.30g/kg, which is far higher than that of fruits such as persimmons, apples, peaches, pears and the like, so that the method has important development and utilization prospects, can greatly increase the product additional value of papaya fruits by extracting the flavonoid from the fruits, and has important significance for forest farmers to lose poverty and become rich. In the prior art, the following extraction methods are mainly adopted for flavonoid compounds: hot water extraction, organic solvent extraction, enzymolysis, ultrasonic assisted extraction, microwave and supercritical fluid extraction. However, the prior method for extracting flavonoids from chaenomeles speciosa has the following technical defects: the extraction rate is low, the content of total flavonoids in the extract is low, and the purity of the purified extract is low. In addition, the papaya with glabrous skin has higher hardness and is difficult to fully crush, so that flavonoids in the papaya with glabrous skin cannot be extracted more thoroughly.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the method for extracting the flavonoids of the chaenomeles speciosa, which has high extraction rate and high content of the flavonoids of the chaenomeles speciosa in the purified extract.
The technical scheme of the invention is realized as follows: a process for extracting flavonoids from chaenomeles speciosa comprises the following steps:
(1) picking fresh fructus Chaenomelis, cleaning, cutting to remove seeds to obtain pulp, adding pulp and water into tissue mashing machine, and mashing;
(2) adding the crushed material into a beater for beating;
(3) air-drying the slurry obtained in the step (2);
(4) grinding the air-dried product in the step (3), and then grinding and discharging the ground product by using a grinding machine to obtain shine skin papaya powder;
(5) adding shine skin papaya powder into water, and soaking to obtain an intermediate product A;
(6) adding an organic solvent into the intermediate product A, and stirring;
(7) standing for layering, separating out an organic phase, extracting the water phase twice with the same amount of organic solvent, and combining the three organic phases;
(8) adding a solid desiccant into the organic phase, removing the solid desiccant, and removing the organic solvent by reduced pressure evaporation on a rotary evaporator;
(9) and (4) adsorbing and purifying the product obtained in the step (8) by using D140 macroporous resin.
The extraction process of the flavonoids of the chaenomeles speciosa comprises the following steps of (1): the mass ratio of the pulp to the water is 1: 0.5-1.
The extraction process of the flavonoids in the chaenomeles speciosa comprises the following steps of (2): the diameter of the sieve pore of the beater is 0.4-1.0 mm.
The extraction process of the flavonoids in the chaenomeles speciosa comprises the following steps of (3): naturally drying the slurry obtained in the step (2) at the temperature of 15-40 ℃.
The extraction process of the flavonoids of the chaenomeles speciosa comprises the following steps of (4): and (4) grinding and discharging by using a superfine grinding mill.
The extraction process of the flavonoids in the chaenomeles speciosa comprises the following steps of (5): adding the shine skin papaya powder into water according to the mass ratio of the shine skin papaya powder to the water of 1:3-5, and soaking for more than 24 hours.
The extraction process of the flavonoids in the chaenomeles speciosa comprises the following steps of (6): at the temperature of 5-15 ℃, according to the mass ratio of the shine skin papaya powder to the organic solvent of 1: 2-3, adding the organic solvent into the intermediate product A, and stirring for more than 0.5 hour.
The extraction process of the flavonoids of the chaenomeles speciosa comprises the following steps of: ethanol, ethyl acetate, a mixed solution of ethanol and cyclopentanol, a mixed solution of ethyl acetate and cyclopentanol, a mixed solution of ethanol and ethylene glycol diethyl ether, a mixed solution of ethyl acetate and ethylene glycol diethyl ether, and a mixed solution of cyclopentanol and ethylene glycol diethyl ether.
The extraction process of the flavonoids in the chaenomeles speciosa comprises the following steps of (8): the solid desiccant is anhydrous sodium sulfate, anhydrous magnesium sulfate or anhydrous calcium chloride.
The extraction process of the flavonoids in the chaenomeles speciosa comprises the following steps of (9): washing with water until the effluent is light or colorless, and eluting with 30-65% ethanol solution to obtain fructus Chaenomelis flavonoid.
The invention has the beneficial effects that: (1) the method for extracting flavonoids from chaenomeles speciosa has the advantages of simple operation process, low cost and mild conditions required by the extraction method, and is suitable for large-scale popularization and application. (2) Compared with the extraction method in the prior art, the extraction selectivity is good, the extraction rate can reach 98 percent at most, and the purity of the papaya flavone after extraction is higher. (3) Compared with the papaya flavone obtained in the prior art, the purity of the total flavone of the papaya with glabrous skin finally obtained is higher. (4) The hardness of the shine skin papaya is high, and if the papaya flesh cannot be thoroughly crushed, the shine skin papaya flavone cannot be fully extracted; according to the invention, the technology of mashing and pulping fresh pawpaw, and then carrying out air drying and grinding is adopted, so that the shine skin pawpaw fruit can be very easily crushed into fine particles, and an extraction solvent is preferably selected, so that flavonoid substances of the shine skin pawpaw can be extracted without heating and refluxing.
Detailed Description
Example 1
A process for extracting flavonoids from chaenomeles speciosa comprises the following steps:
(1) picking fresh papaya fruits, cleaning, cutting to remove seeds to obtain pulp, adding the pulp and water into a tissue mashing machine to be mashed, wherein the mass ratio of the pulp to the water is 1: 0.5.
(2) And adding the crushed material into a beater to be beaten, wherein the diameter of a sieve pore of the beater is 0.4 mm.
(3) And (3) naturally drying the slurry obtained in the step (2) at 15 ℃.
(4) And (4) grinding the air-dried product in the step (3), and then grinding and discharging the ground product by using a superfine grinding mill to obtain the shine skin papaya powder.
(5) Adding 100 g of shine skin papaya powder into 300 g of water according to the mass ratio of the shine skin papaya powder to the water of 1:3, and soaking for 24 hours to obtain an intermediate product A; the total amount of flavonoids in intermediate A is 2876mg determined by high performance liquid chromatography in the prior art.
(6) At the temperature of 5 ℃, according to the mass ratio of the shine skin papaya powder to the ethyl acetate of 1: 2, 200 g of ethyl acetate was added to the intermediate product A, and the mixture was stirred for 0.5 hour.
(7) Standing for layering, separating out an organic phase, extracting the water phase twice with the same amount of ethyl acetate, and combining the three organic phases; the total amount of flavonoids in the aqueous phase was 949 mg as determined by high performance liquid chromatography of the prior art, i.e. 1927 mg of flavonoids in the aqueous phase was transferred to ethyl acetate.
(8) To the organic phase was added anhydrous sodium sulfate, dried for 24 hours, and the anhydrous sodium sulfate was removed, and ethyl acetate was evaporated under reduced pressure on a rotary evaporator.
(9) Dissolving the product obtained in the step (8) by using ethanol, and then adsorbing and purifying by using D140 macroporous resin; washing with water until the effluent is colorless, eluting with 30% ethanol solution, collecting eluate, and determining total amount of flavonoids in the eluate by high performance liquid chromatography in the prior art to be 1638 mg.
The oxidation resistance of the papaya total flavonoids is tested according to the method in the prior art in this example: and (3) with ascorbic acid as a reference, respectively determining the reducing capacity of the chaenomeles speciosa before and after the purification of the total flavonoids when the total flavonoids concentration is 5 mug/mL, wherein the A700 value before the purification is 0.4, and the A700 value after the purification is 0.8. And (3) with ascorbic acid as a reference, respectively determining the scavenging capacity of the total flavonoids of the chaenomeles speciosa to hydroxyl free radicals before and after the purification when the concentration of the total flavonoids is 40 mug/mL, wherein the scavenging rate before the purification is 60%, and the scavenging rate after the purification is 80%. The higher the purity of the total flavonoids of the chaenomeles speciosa is, the higher the reduction capability and the capability of removing hydroxyl free radicals of the total flavonoids of the chaenomeles speciosa are, so that the purity of the flavonoids of the chaenomeles speciosa finally obtained by the extraction method of the flavonoids of the chaenomeles speciosa is greatly improved.
Example 2
A process for extracting flavonoids from chaenomeles speciosa comprises the following steps:
(1) picking fresh papaya fruits with smooth peel, cleaning, cutting and removing seeds to obtain pulp, adding the pulp and water into a tissue mashing machine for mashing, wherein the mass ratio of the pulp to the water is 1: 1.
(2) And adding the crushed material into a beater to be beaten, wherein the diameter of a sieve pore of the beater is 0.4 mm.
(3) And (3) naturally drying the slurry obtained in the step (2) at 25 ℃.
(4) And (4) grinding the air-dried product in the step (3), and then grinding and discharging the ground product by using a superfine grinding mill to obtain the shine skin papaya powder.
(5) Adding 100 g of shine skin papaya powder into 400 g of water according to the mass ratio of the shine skin papaya powder to the water of 1:4, and soaking for 48 hours to obtain an intermediate product A; the total amount of flavonoids in intermediate A is 2768mg by high performance liquid chromatography.
(6) At the temperature of 5 ℃, mixing the shine skin papaya powder with a mixed solution of ethanol and ethyl acetate according to a mass ratio of 1: 2.5 volume ratio of ethanol to ethyl acetate in the mixed solution of ethanol and ethyl acetate was 1:5, and 250 g of the mixed solution of ethanol and ethyl acetate was added to intermediate A and stirred for 1 hour.
(7) Standing for layering, separating out an organic phase, extracting the water phase twice with the same amount of mixed solution of ethanol and ethyl acetate, and combining the organic phases obtained by three times; the total amount of flavonoids in the water phase was 941 mg as determined by high performance liquid chromatography in the prior art, i.e. 1827 mg of flavonoids in the water phase was transferred to the mixed solution of ethanol and ethyl acetate.
(8) To the organic phase was added anhydrous sodium sulfate, dried for 24 hours, and the anhydrous sodium sulfate was removed, and ethanol and ethyl acetate were removed by evaporation under reduced pressure on a rotary evaporator.
(9) Dissolving the product obtained in the step (8) by using ethanol, and then adsorbing and purifying by using D140 macroporous resin; washing with water until the effluent is colorless, eluting with 45% ethanol solution, collecting eluate, and determining the total amount of flavonoids in the eluate to 1535 mg by high performance liquid chromatography of the prior art.
The oxidation resistance of the papaya total flavonoids is tested according to the method in the prior art in this example: the reducing capacity before and after the purification of the total flavonoids of the chaenomeles sinensis is respectively measured when the concentration of the total flavonoids is 5 mug/mL by using ascorbic acid as a reference, the A700 value before the purification is 0.5, and the A700 value after the purification is 0.85. And (3) with ascorbic acid as a reference, respectively determining the scavenging capacity of the total flavonoids of the chaenomeles speciosa to hydroxyl free radicals before and after the purification when the concentration of the total flavonoids is 40 mug/mL, wherein the scavenging rate before the purification is 63%, and the scavenging rate after the purification is 84%. The higher the purity of the total flavonoids of the chaenomeles speciosa is, the higher the reduction capability and the capability of removing hydroxyl free radicals of the total flavonoids of the chaenomeles speciosa are, which shows that the purity of the flavonoids of the chaenomeles speciosa finally obtained by the extraction method of the flavonoids of the chaenomeles speciosa is very high.
Example 3
A process for extracting flavonoids from chaenomeles speciosa comprises the following steps:
(1) picking fresh papaya fruits, cleaning, cutting to remove seeds to obtain pulp, adding the pulp and water into a tissue mashing machine to be mashed, wherein the mass ratio of the pulp to the water is 1: 0.8.
(2) And adding the crushed material into a beater to be beaten, wherein the diameter of a sieve pore of the beater is 0.5 mm.
(3) And (3) naturally drying the slurry obtained in the step (2) at the temperature of 20 ℃.
(4) And (4) grinding the air-dried product in the step (3), and then grinding and discharging the ground product by using a superfine grinding mill to obtain the shine skin papaya powder.
(5) Adding 100 g of shine skin papaya powder into 350 g of water according to the mass ratio of the shine skin papaya powder to the water of 1:3.5, and soaking for 48 hours to obtain an intermediate product A; the total amount of flavonoids in intermediate A was measured to be 2905mg by high performance liquid chromatography of the prior art.
(6) At the temperature of 5-10 ℃, mixing the shine skin papaya powder with a mixed solution of ethyl acetate and cyclopentanol in a mass ratio of 1:3, the volume ratio of ethyl acetate to cyclopentanol in the mixed solution of ethyl acetate and cyclopentanol is 1:3.5, and 300 g of the mixed solution of ethyl acetate and cyclopentanol is added to the intermediate product A, and stirred for 2 hours.
(7) Standing for layering, separating out an organic phase, extracting the water phase twice with the same amount of mixed solution of ethyl acetate and cyclopentanol, and combining the organic phases obtained three times; the total amount of flavonoids in the water phase was 639 mg as determined by high performance liquid chromatography of the prior art, i.e. 2266 mg of flavonoids in the water phase was transferred to the mixed solution of ethyl acetate and cyclopentanol.
(8) To the organic phase was added anhydrous sodium sulfate, dried for 24 hours, and the anhydrous sodium sulfate was removed, and ethyl acetate and cyclopentanol were evaporated under reduced pressure on a rotary evaporator.
(9) Dissolving the product obtained in the step (8) by using ethanol, and then adsorbing and purifying by using D140 macroporous resin; washing with water until the effluent is colorless, eluting with 50% ethanol solution, collecting eluate, and determining total amount of flavonoids in the eluate by high performance liquid chromatography of the prior art to 1994 mg.
The oxidation resistance of the papaya total flavonoids is tested according to the method in the prior art in this example: the reducing capacity before and after the purification of the total flavonoids of the chaenomeles sinensis is respectively measured when the concentration of the total flavonoids is 5 mug/mL by using ascorbic acid as a reference, the A700 value before the purification is 0.55, and the A700 value after the purification is 0.89. With ascorbic acid as a control, the hydroxyl radical scavenging capacity before and after the purification of the chaenomeles sinensis total flavonoids is respectively determined when the total flavonoids concentration is 40 mug/mL, the clearance before the purification is 68%, and the clearance after the purification is 87%. The higher the purity of the total flavonoids of the chaenomeles speciosa is, the higher the reduction capability and the capability of removing hydroxyl free radicals of the total flavonoids of the chaenomeles speciosa are, which shows that the purity of the flavonoids of the chaenomeles speciosa finally obtained by the extraction method of the flavonoids of the chaenomeles speciosa is very high.
Example 4
A process for extracting flavonoids from chaenomeles speciosa comprises the following steps:
(1) picking fresh papaya fruits, cleaning, cutting to remove seeds to obtain pulp, adding the pulp and water into a tissue mashing machine to be mashed, wherein the mass ratio of the pulp to the water is 1: 0.6.
(2) And adding the crushed material into a beater to be beaten, wherein the diameter of a sieve pore of the beater is 0.4 mm.
(3) And (3) naturally drying the slurry obtained in the step (2) at 15 ℃.
(4) And (4) grinding the air-dried product in the step (3), and then grinding and discharging the ground product by using a superfine grinding mill to obtain the shine skin papaya powder.
(5) Adding 100 g of shine skin papaya powder into 400 g of water according to the mass ratio of the shine skin papaya powder to the water of 1:4, and soaking for 24 hours to obtain an intermediate product A; the total amount of flavonoids in intermediate A was 2813mg as determined by high performance liquid chromatography of the prior art.
(6) At the temperature of 15 ℃, according to the mass ratio of the shine skin papaya powder to the mixed solution of ethanol and ethylene glycol diethyl ether of 1: 2, the volume ratio of ethanol to ethylene glycol diethyl ether in the mixed solution of ethanol and ethylene glycol diethyl ether is 1:10, 200 g of the mixed solution of ethanol and ethylene glycol diethyl ether is added into the intermediate product A, and the mixture is stirred for 0.5 hour.
(7) Standing for layering, separating out an organic phase, extracting the water phase twice with the same amount of mixed solution of ethanol and ethylene glycol diethyl ether, and combining the organic phases obtained in three times; the total amount of flavonoids in the water phase is 675 mg measured by high performance liquid chromatography in the prior art, namely 2138 mg of flavonoids in the water phase is transferred into a mixed solution of ethanol and ethylene glycol diethyl ether.
(8) Anhydrous sodium sulfate was added to the organic phase, dried for 24 hours, removed of the anhydrous sodium sulfate, and evaporated under reduced pressure on a rotary evaporator to remove ethanol and ethylene glycol diethyl ether.
(9) Dissolving the product obtained in the step (8) by using ethanol, and then adsorbing and purifying by using D140 macroporous resin; washing with water until the effluent is colorless, eluting with 60% ethanol solution, collecting eluate, and determining total amount of flavonoids in the eluate to 1924 mg by high performance liquid chromatography of the prior art.
The oxidation resistance of the papaya total flavonoids is tested according to the method in the prior art in this example: the reducing capacity before and after the purification of the total flavonoids of the chaenomeles sinensis is respectively measured when the concentration of the total flavonoids is 5 mug/mL by using ascorbic acid as a reference, the A700 value before the purification is 0.65, and the A700 value after the purification is 0.95. With ascorbic acid as a control, the hydroxyl radical scavenging capacity before and after the purification of the chaenomeles sinensis total flavonoids is respectively determined when the total flavonoids concentration is 40 mug/mL, the clearance before the purification is 71%, and the clearance after the purification is 89%. The higher the purity of the total flavonoids of the chaenomeles speciosa is, the higher the reduction capability and the capability of removing hydroxyl free radicals of the total flavonoids of the chaenomeles speciosa are, which shows that the purity of the flavonoids of the chaenomeles speciosa finally obtained by the extraction method of the flavonoids of the chaenomeles speciosa is very high.
Example 5
A process for extracting flavonoids from chaenomeles speciosa comprises the following steps:
(1) picking fresh papaya fruits, cleaning, cutting to remove seeds to obtain pulp, adding the pulp and water into a tissue mashing machine to be mashed, wherein the mass ratio of the pulp to the water is 1: 0.5.
(2) And adding the crushed material into a beater to be beaten, wherein the diameter of a sieve pore of the beater is 0.4 mm.
(3) And (3) naturally drying the slurry obtained in the step (2) at 25 ℃.
(4) And (4) grinding the air-dried product in the step (3), and then grinding and discharging the ground product by using a superfine grinding mill to obtain the shine skin papaya powder.
(5) Adding 100 g of shine skin papaya powder into 300 g of water according to the mass ratio of the shine skin papaya powder to the water of 1:3, and soaking for 24 hours to obtain an intermediate product A; the total amount of flavonoids in intermediate A is 2798mgg by high performance liquid chromatography.
(6) At the temperature of 10 ℃, according to the mass ratio of the shine skin papaya powder to the mixed solution of cyclopentanol and ethylene glycol diethyl ether of 1: 4.5, the volume ratio of the cyclopentanol to the ethylene glycol diethyl ether in the mixed solution of the cyclopentanol and the ethylene glycol diethyl ether is 1:0.8, 450 g of the mixed solution of the cyclopentanol and the ethylene glycol diethyl ether is added to the intermediate product A, and the mixture is stirred for 0.5 hour.
(7) Standing for layering, separating out an organic phase, extracting the water phase twice with the same amount of mixed solution of cyclopentanol and ethylene glycol diethyl ether, and combining the organic phases obtained three times; the total amount of flavonoids in the water phase is 55 mg measured by high performance liquid chromatography in the prior art, namely 2743 mg of flavonoids in the water phase is transferred into the mixed solution of cyclopentanol and ethylene glycol diethyl ether.
(8) Anhydrous sodium sulfate was added to the organic phase, dried for 24 hours, removed, and the cyclopentanol and ethylene glycol diethyl ether were removed by evaporation under reduced pressure on a rotary evaporator.
(9) Dissolving the product obtained in the step (8) by using ethanol, and then adsorbing and purifying by using D140 macroporous resin; washing with water until the effluent is colorless, eluting with 53% ethanol solution, collecting eluate, and determining total amount of flavonoids in the eluate to 2660 mg by high performance liquid chromatography.
The oxidation resistance of the papaya total flavonoids is tested according to the method in the prior art in this example: the reducing capacity before and after the purification of the total flavonoids of the chaenomeles sinensis is respectively measured when the concentration of the total flavonoids is 5 mug/mL by using ascorbic acid as a reference, the A700 value before the purification is 0.7, and the A700 value after the purification is 1.1. And (3) with ascorbic acid as a reference, respectively determining the scavenging capacity of the total flavonoids of the chaenomeles speciosa to hydroxyl free radicals before and after the purification when the concentration of the total flavonoids is 40 mug/mL, wherein the scavenging rate before the purification is 75%, and the scavenging rate after the purification is 92%. The higher the purity of the total flavonoids of the chaenomeles speciosa is, the higher the reduction capability and the capability of removing hydroxyl free radicals of the total flavonoids of the chaenomeles speciosa are, which shows that the purity of the flavonoids of the chaenomeles speciosa finally obtained by the extraction method of the flavonoids of the chaenomeles speciosa is very high.
The above examples are provided for clarity of illustration only and are not intended to limit the invention to the particular embodiments described. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any obvious variations or modifications which come within the spirit and scope of the invention are desired to be protected by the following claims.
Claims (1)
1. The extraction process of the flavonoids of the chaenomeles speciosa is characterized by comprising the following steps:
(1) picking fresh papaya fruits with smooth peel, cleaning, cutting and removing seeds to obtain pulp, adding the pulp and water into a tissue mashing machine for mashing, wherein the mass ratio of the pulp to the water is 1:0.6;
(2) adding the crushed material into a beater to be beaten, wherein the diameter of a sieve pore of the beater is 0.4mm;
(3) naturally drying the slurry obtained in the step (2) at 15 ℃;
(4) grinding the air-dried product in the step (3), and then grinding and discharging the ground product by using a superfine grinding machine to obtain shine skin papaya powder;
(5) adding 100 g of shine skin papaya powder into 400 g of water according to the mass ratio of the shine skin papaya powder to the water of 1:4, and soaking for 24 hours to obtain an intermediate product A; determining the total amount of flavonoids in intermediate product A to be 2813mg by high performance liquid chromatography in the prior art;
(6) at the temperature of 15 ℃, according to the mass ratio of the shine skin papaya powder to the mixed solution of ethanol and ethylene glycol diethyl ether of 1: 2, adding 200 g of mixed solution of ethanol and ethylene glycol diethyl ether into the intermediate product A, and stirring for 0.5 hour, wherein the volume ratio of the ethanol to the ethylene glycol diethyl ether in the mixed solution of the ethanol and the ethylene glycol diethyl ether is 1: 10;
(7) standing for layering, separating out an organic phase, extracting the water phase twice with the same amount of mixed solution of ethanol and ethylene glycol diethyl ether, and combining the organic phases obtained in three times; measuring total amount of flavonoids in water phase to 675 mg by high performance liquid chromatography in the prior art, namely transferring 2138 mg of flavonoids in water phase into mixed solution of ethanol and ethylene glycol diethyl ether;
(8) adding anhydrous sodium sulfate into the organic phase, drying for 24 hr, removing anhydrous sodium sulfate, and removing ethanol and ethylene glycol diethyl ether by reduced pressure evaporation on a rotary evaporator;
(9) dissolving the product obtained in the step (8) by using ethanol, and then adsorbing and purifying by using D140 macroporous resin; washing with water until the effluent is colorless, eluting with 60% ethanol solution, collecting eluate, and determining total amount of flavonoids in the eluate to 1924 mg by high performance liquid chromatography of the prior art.
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Non-Patent Citations (6)
| Title |
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| Antimicrobial and antioxidant activities of unripe papaya;James Akira Osato等;《Life Sciences》;19931231;第53卷(第17期);第1383-1389页 * |
| 光皮木瓜中黄酮类物质提取工艺的研究;徐青梅;《保鲜与加工》;20121231;第12卷(第5期);第23-28页 * |
| 光皮木瓜黄酮和多糖降血脂与抗氧化作用研究;纪学芳等;《中国食品学报》;20130930;第13卷(第9期);第1-7页 * |
| 响应面试验优化超声波提取光皮木瓜黄酮和多糖复合物;纪学芳等;《食品科学》;20131231;第34卷(第6期);第47-51页 * |
| 木瓜黄酮的提取及其紫外光谱特征;胡华平等;《现代食品科技》;20081231;第24卷(第3期);第250-252页 * |
| 木瓜黄酮的提取及抗氧化性研究;周晓丽等;《食品工业科技》;20071231(第8期);第170-172页 * |
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| CN107789406B (en) | 2020-05-19 |
| CN104666483B (en) | 2017-10-20 |
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