CN106913639A - A method for preparing ellagic acid concentrate from branches and leaves of Rubi fructus - Google Patents
A method for preparing ellagic acid concentrate from branches and leaves of Rubi fructus Download PDFInfo
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- CN106913639A CN106913639A CN201510994593.2A CN201510994593A CN106913639A CN 106913639 A CN106913639 A CN 106913639A CN 201510994593 A CN201510994593 A CN 201510994593A CN 106913639 A CN106913639 A CN 106913639A
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- ellagic acid
- raspberry
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- ATJXMQHAMYVHRX-CPCISQLKSA-N Ellagic acid Natural products OC1=C(O)[C@H]2OC(=O)c3cc(O)c(O)c4OC(=O)C(=C1)[C@H]2c34 ATJXMQHAMYVHRX-CPCISQLKSA-N 0.000 title claims abstract description 47
- 229920002079 Ellagic acid Polymers 0.000 title claims abstract description 47
- 229960002852 ellagic acid Drugs 0.000 title claims abstract description 47
- 235000004132 ellagic acid Nutrition 0.000 title claims abstract description 47
- FAARLWTXUUQFSN-UHFFFAOYSA-N methylellagic acid Natural products O1C(=O)C2=CC(O)=C(O)C3=C2C2=C1C(OC)=C(O)C=C2C(=O)O3 FAARLWTXUUQFSN-UHFFFAOYSA-N 0.000 title claims abstract description 47
- AFSDNFLWKVMVRB-UHFFFAOYSA-N Ellagic acid Chemical compound OC1=C(O)C(OC2=O)=C3C4=C2C=C(O)C(O)=C4OC(=O)C3=C1 AFSDNFLWKVMVRB-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000012141 concentrate Substances 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title claims abstract description 7
- 240000007651 Rubus glaucus Species 0.000 claims abstract description 47
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000001556 precipitation Methods 0.000 claims abstract description 4
- 235000011034 Rubus glaucus Nutrition 0.000 claims description 49
- 235000009122 Rubus idaeus Nutrition 0.000 claims description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000012153 distilled water Substances 0.000 claims description 12
- 239000000287 crude extract Substances 0.000 claims description 9
- 239000000284 extract Substances 0.000 claims description 7
- 238000000605 extraction Methods 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 2
- 238000012360 testing method Methods 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 235000021013 raspberries Nutrition 0.000 abstract description 11
- 235000013305 food Nutrition 0.000 abstract description 5
- 238000010992 reflux Methods 0.000 abstract description 2
- 206010028980 Neoplasm Diseases 0.000 abstract 2
- 201000011510 cancer Diseases 0.000 abstract 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 230000000711 cancerogenic effect Effects 0.000 abstract 1
- 231100000315 carcinogenic Toxicity 0.000 abstract 1
- -1 ellagic acid compound Chemical class 0.000 abstract 1
- 230000004060 metabolic process Effects 0.000 abstract 1
- 235000015097 nutrients Nutrition 0.000 abstract 1
- 238000001035 drying Methods 0.000 description 21
- 239000000843 powder Substances 0.000 description 21
- 239000000243 solution Substances 0.000 description 16
- 244000235659 Rubus idaeus Species 0.000 description 13
- 239000013049 sediment Substances 0.000 description 12
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 10
- 206010013786 Dry skin Diseases 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- 239000007787 solid Substances 0.000 description 10
- 239000003814 drug Substances 0.000 description 7
- 238000011160 research Methods 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 201000010099 disease Diseases 0.000 description 4
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 4
- 229940079593 drug Drugs 0.000 description 4
- 235000013399 edible fruits Nutrition 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 241001116389 Aloe Species 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 235000011399 aloe vera Nutrition 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229930003935 flavonoid Natural products 0.000 description 2
- 150000002215 flavonoids Chemical class 0.000 description 2
- 235000017173 flavonoids Nutrition 0.000 description 2
- 210000003734 kidney Anatomy 0.000 description 2
- 210000004185 liver Anatomy 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 206010001928 Amenorrhoea Diseases 0.000 description 1
- 208000008035 Back Pain Diseases 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 206010013935 Dysmenorrhoea Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 208000008930 Low Back Pain Diseases 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
- 206010059013 Nocturnal emission Diseases 0.000 description 1
- 241000123889 Rubus chingii Species 0.000 description 1
- 240000005255 Rubus parvifolius Species 0.000 description 1
- 235000018803 Rubus parvifolius Nutrition 0.000 description 1
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 1
- 241000607142 Salmonella Species 0.000 description 1
- 241000270295 Serpentes Species 0.000 description 1
- 241000607768 Shigella Species 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 244000228451 Stevia rebaudiana Species 0.000 description 1
- 235000006092 Stevia rebaudiana Nutrition 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 244000269722 Thea sinensis Species 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229930014669 anthocyanidin Natural products 0.000 description 1
- 150000001452 anthocyanidin derivatives Chemical class 0.000 description 1
- 235000008758 anthocyanidins Nutrition 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000021028 berry Nutrition 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004438 eyesight Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000019990 fruit wine Nutrition 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 201000001881 impotence Diseases 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 239000003182 parenteral nutrition solution Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 238000000926 separation method 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
- 239000005720 sucrose Substances 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 235000013618 yogurt Nutrition 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/02—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains two hetero rings
- C07D493/06—Peri-condensed systems
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- 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
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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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
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Medicinal Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Biochemistry (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
A method for preparing ellagic acid concentrate from branches and leaves of Rubi fructus is provided. The natural extracted ellagic acid compound only destroys the bad cells in the body (the products of daily metabolism of the human body comprise thousands to tens of thousands of carcinogenic cells), and does not damage the good cells in the body. Therefore, the normal intake of the nutrient can prevent the formation of cancer cells and is the best natural supplementary food for resisting cancer. The method comprises the steps of utilizing residual branches and leaves after stumping of raspberries as raw materials, refluxing for 120-180 min at 80-90 ℃ for 1.2-2.0 mol/L of hydrochloric acid, 45-55% of ethanol and 1: 50-60 (m/v) of material-liquid ratio, and then carrying out vacuum concentration, cooling and precipitation to obtain the ellagic acid concentrate with the ellagic acid content of more than 16%.
Description
Technical field
The invention belongs to agricultural product byproduct high-efficiency comprehensive utilization technical field, and in particular to by removing solvent after the ellagic acid in solvent extraction raspberry branch and extracting auxiliary agent method.
Background technology
Early there is the record of raspberry medication in China,《A thousand pieces of gold food therapy》Described in raspberry " sweet, put down, nontoxic ", " enter liver, kidney two warp " has filling liver kidney, reduces just, and impotence is controlled in supporing yang, controlling nocturnal emission with astringent drugs, improving eyesight, seminal emission, loses weak, consumptive disease, and the dark effect of mesh is the Traditional Folk medication of Miao ethnic group.Its root, lotus, leaf can all be used as medicine, root nature and flavor slightly bitter, hold back and drag effect with expelling wind and activating blood flow, removing toxic substances, cure mainly copper disease, snake sting, the disease such as amenorrhoea dysmenorrhoea, wet epidemic disease, lumbago due to wind-wetness evil.By having reached 180,000 mu to the cultivated area of China raspberry in 2012, and nearly 3 years raspberry cultivated areas increase sharply.Raspberry branches and leaves according to being discarded after the annual raspberry stump of raspberry cultivated area in 2012 reach more than 30,000 tons, and cumulative year after year, up to the present only having a small amount of raspberry leaf is used for the making of raspberry tea by purchase, and major part to go out of use and cause the pollution of environment in field or burning.Find that raspberry contains several functions composition according to the research of this seminar, mainly there are the aldehydes matters such as anthocyanidin, ellagic acid and flavonoids, salicylic acid, ascorbic acid and raspberry glycosides etc., these functional components have special physiological function and BA, and the content of ellagic acid is more than 50 times in fruit wherein in branch.Therefore, raspberry branches and leaves are carried out with the extraction of functional components, the economic benefit planted for improving raspberry has very important significance.
At present, the raspberry processed goods whole dependence on import of China, only can just buy in metropolitan supermarket, and the product entirely imported goods such as Raspberry Drink, jam, Yoghourt that for example Beijing Yansha, Saite are sold is expensive, is referred to as " noble's consumption " product.The external report on raspberry processing has done substantial amounts of basic research work nor many but more active to the research of the functional component in raspberry, is that the deep level development of raspberry is laid a good foundation.The Chinese Central Television (CCTV) reports that Japan extracts raspberry flavonoids from raspberry seed, makees to disappear fat agent for substituting capsicim, and the fat-reducing fat effect that disappears is ten times of capsicim.Japan is using raspberry for development of raw materials goes out the senior skincare product of All Pure Nature.China is that, in recent years, the provinces and cities such as Heilungkiang, Jilin, Tianjin, Jiangsu, Guangdong have successively carried out the research of fruit wine, beverage, inspissated juice, jam, can and quick-frozen food and utilized；Cooperate to have extracted much sweeter than sucrose 300 times of stirrup acid anhydride from sweetleaf stirrup with Japan in Guangdong.Also had made some progress in terms of medical utilization in addition, the research in terms of pharmacology, medicine and composition such as has been carried out to Rubus parvifolius, Rubus chingii, have developed the Chinese patent drug of certain curative effect, Zhongshan University and Guangzhou Chinese medicine head factory cooperation research and development have " ' Zhixueling " parenteral solution of good therapeutic effect.Carry out the separation of active component in raspberry branch fruit leaf, extract and concentrate the development for being beneficial to China's raspberry deep processed product.
The content of the invention
In order to realize that raspberry branches and leaves are fully used, the economic benefit of raspberry industry is improved, present invention solves the technical problem that being achieved by the following scheme.
（ 1 ）TreeThe treatment of certain kind of berries branch：After raspberry branch after stump air-dries treatment, after moisture is controlled more than 7%, dry raspberry branch is crushed with high speed Universal pulverizer, be contained in plastic packaging bag and be placed at shady and cool drying, it is standby.
（ 2 ）The extraction of ellagic acid：To step（1）The raspberry branch for the treatment of, in concentration of hydrochloric acid 1.2-2.0mol/L, concentration of alcohol is 50%, solid-liquid ratio 1:55-60（m/v）, return time 120-160min under the conditions of 85 DEG C, acquisition ellagic acid crude extract.
（ 3 ）Concentrating and precipitating：By step（2）Crude extract is obtained in 0.1Mpa, after 75-90 DEG C is concentrated in vacuo to extract solution 1/3, it is zero to measure the alcohol content in extract solution, and a large amount of precipitations are produced normal temperature is put into 3.5-4.5 DEG C of refrigeration 12 hours after being cooled to 20-25 DEG C after, then filter paper filtering, obtains raspberry branch and extracts sediment.
（ 4 ）It is washed to neutrality：To step（3）Obtain raspberry branch and extract sediment and washed with distilled water, be washed till water in being dried to moisture below 6% after neutrality, as raspberry branch extracts the ellagic acid concentrate for obtaining.
The measure of ellagic acid：
Liquid phase chromatogram condition.Chromatographic column is Symmetry C18Post (4.6 × 250mm, 5 μm)；Mobile phase is CH3CN-0.1% phosphoric acid (volume ratio 21：79)；Flow velocity is 1 ml/min；Column temperature is 35 DEG C；Detection wavelength is 253 nm；
The preparation of standard solution.Accurately weigh 5.00mg ellagic acid standard items, as 50ml volumetric flasks in, be settled to graduation mark with dmso solution, obtain concentration be 100ppm ellagic acid standard liquid.Again with this solution as mother liquor, the standard liquid for being made into that concentration is 80ppm, 60ppm, 40ppm, 20ppm, 5ppm is diluted respectively with dimethyl sulfoxide (DMSO), it is standby through 0.45 μm of filtering with microporous membrane；
Standard curve is set up.By liquid chromatograph on the ellagic acid standard items of the various concentrations of above-mentioned preparation, corresponding chromatogram is obtained（See accompanying drawing 1）, with concentration x（ppm）It is abscissa, peak area y is ordinate, makees standard curve, obtains ellagic acid standard curve regression equation for y=151.69x-1003（R2=0.9998）.The curvilinear equation shows that ellagic acid concentration of standard solution linear relationship in the range of 0.005 ~ 0.3mg/ml is good, can be used to analyze the ellagic acid content in sample；
The preparation of need testing solution.Accurately weigh 0.5g steps（4）Ellagic acid concentrate dmso solution be settled to 50ml, with syringe draw 1 ~ 2ml cross 0.45 μm of miillpore filter, upper hplc determination（See accompanying drawing 2）.
The content of ellagic acid concentrate：Through liquid phase measurement raspberry branch ellagic acid concentrate content between 16.9% ~ 20.7%.
Advantage of the invention is that：
（1）Existing document invention report it is main with fruit of raspberry be raw material extraction ellagic acid based on product, and the present invention is with raspberry branches and leaves as raw material, low cost, and is conducive to the utilization of agricultural product castoff；
（2）Preliminary purification after prepared by ellagic acid concentrate obtains pulverulent product of the ellagic acid content more than 16% by the way of precipitation cleaning the most original, and simple production process, cost of investment is low, it is easy to large-scale production；
（3）Made ellagic acid concentrate reference QB/T2489-2007 raw-food materials aloe products related sanitary standard, through checking arsenic, lead, BHC, DDT, total plate count, Escherichia coli, yeast and mold, pathogenic bacteria（Salmonella, Shigella and staphylococcus aureus）Inspection is below aloe powder.Therefore, the product can be as a kind of alternative and medical material of raw material for food.
Brief description of the drawings
Figure
1
The liquid chromatogram of ellagic acid standard items under experiment condition of the present invention.
Figure
2
The liquid phase measurement figure of the ellagic acid concentrate of present invention system.
Specific embodiment
Invention is described in detail with reference to specific example：
Raspberry branch used of the invention is special hereby for two season of summer and autumn result type raspberry kind Haier（Heritage）Stump branches and leaves, the kind Liaoning Prov. Fruit Tree Science Inst. introduces for 2003 from the Chinese Academy of Forestry, originates in the U.S..
Unless otherwise specified, material therefor of the present invention is commercially available.Food grade hydrochloric acid, is purchased from up to Chemical Co., Ltd. of Zhongshan city；Edible alcohol, is purchased from Henan Tianguan Enterprise Group Co；Ellagic acid standard items, are purchased from Chengdu Man Site bio tech ltd, lot number：MUST-14110807；Dimethyl sulfoxide (DMSO)（Analysis is pure）, Tianjin Fu Qi Chemical Co., Ltd.s；Acetonitrile（Chromatographically pure, purchase xingmake chemicals；Phosphoric acid, is purchased from Tianjin Jin Feng Chemical Co., Ltd.s；Heartily pure water is purchased from Hangzhou Wahaha Group Co., Ltd；
Instrument and equipment：The high performance liquid chromatographs of Agilent- 1100, Agilent company of the U.S.；Rotary Evaporators, Shanghai Yarong Biochemical Instrument Plant, model RE-52A；Electric-heated thermostatic water bath, mayor of Beijing bearing instruments and meters company, model HW SY11-K；Electronic balance, Yuyao City Jin Nuo balance equipments Co., Ltd, model JF1004；High speed Universal pulverizer, Beijing Zhong Xing great achievements Instrument Ltd., model FW100；Refluxing extraction device.
Embodiment 1
It is 6.8% by the raspberry branches and leaves drying of stump to moisture, is crushed to 40 mesh, take 20g raspberries branch powder, adds 50% ethanol of 1000ml（Hydrochloric 1.2mol）Solution, after 150min being extracted in 85 DEG C, 0.1MPa, 75 DEG C are concentrated into 350ml, after cooling being put into 4.8 DEG C of cold compartment of refrigerator after being cooled to 23 DEG C 14 hours, the sediment after being filtered with 200 mesh is cleaned in neutrality in six times with 30ml distilled water, is 6.8% in 53 DEG C of dryings to moisture, 1.28g solid powders are obtained, it is 16.9% to measure ellagic acid content.
Embodiment 2
It is 7.0% by the raspberry branches and leaves drying of stump to moisture, is crushed to 40 mesh, take 10g raspberries branch powder, adds 50% ethanol of 550ml（Hydrochloric 0.82mol）Solution, after 140min being extracted in 85 DEG C, 0.1MPa, 70 DEG C are concentrated into 170ml, after cooling being put into 4.3 DEG C of cold compartment of refrigerator after being cooled to 20 DEG C 15 hours, the sediment after being filtered with 200 mesh is cleaned in neutrality in six times with 18ml distilled water, is 7.2% in 53 DEG C of dryings to moisture, 0.65g solid powders are obtained, it is 17.2% to measure ellagic acid content.
Embodiment 3
It is 7.0% by the raspberry branches and leaves drying of stump to moisture, is crushed to 40 mesh, take 20g raspberries branch powder, adds 50% ethanol of 1200ml（Hydrochloric 2.2mol）Solution, after 140min being extracted in 84 DEG C, 0.1MPa, 70 DEG C are concentrated into 380ml, after cooling being put into 3.8 DEG C of cold compartment of refrigerator after being cooled to 25 DEG C 16 hours, the sediment after being filtered with 200 mesh is cleaned in neutrality in six times with 36ml distilled water, is 7.8% in 58 DEG C of dryings to moisture, 1.4g solid powders are obtained, it is 18.7% to measure ellagic acid content.
Embodiment 4
It is 7.0% by the raspberry branches and leaves drying of stump to moisture, is crushed to 40 mesh, take 15g raspberries branch powder, adds 50% ethanol of 800ml（Hydrochloric 1.5mol）Solution, after 160min being extracted in 83 DEG C, 0.1MPa, 78 DEG C are concentrated into 270ml, after cooling being put into 4.2 DEG C of cold compartment of refrigerator after being cooled to 23 DEG C 18 hours, the sediment after being filtered with 200 mesh is cleaned in neutrality in six times with 30ml distilled water, is 7.1% in 55 DEG C of dryings to moisture, 0.94g solid powders are obtained, it is 18.3% to measure ellagic acid content.
Embodiment 5
It is 6.6% by the raspberry branches and leaves drying of stump to moisture, is crushed to 40 mesh, take 10g raspberries branch powder, adds 50% ethanol of 570ml（Hydrochloric 1.09mol）Solution, return time 150min under the conditions of 85 DEG C, obtains the 24ml distilled water of the sediment after 200 mesh of ellagic acid crude extract are filtered and cleans in six times in neutrality, is 7.2% in 52 DEG C of dryings to moisture, 0.64g solid powders are obtained, it is 20.1% to measure ellagic acid content.
Embodiment 6
It is 6.6% by the raspberry branches and leaves drying of stump to moisture, is crushed to 40 mesh, take 5g raspberries branch powder, adds 50% ethanol of 280ml（Hydrochloric 0.5mol）Solution, return time 150min under the conditions of 87 DEG C, obtains the 12ml distilled water of the sediment after 200 mesh of ellagic acid crude extract are filtered and cleans in six times in neutrality, is 7.8% in 50 DEG C of dryings to moisture, 0.31g solid powders are obtained, it is 19.8% to measure ellagic acid content.
Embodiment 7
It is 6.6% by the raspberry branches and leaves drying of stump to moisture, is crushed to 40 mesh, take 30g raspberries branch powder, adds 50% ethanol of 1800ml（Hydrochloric 2.7mol）Solution, return time 160min under the conditions of 85 DEG C, obtains the 72ml distilled water of the sediment after 200 mesh of ellagic acid crude extract are filtered and cleans in six times in neutrality, is 6.8% in 65 DEG C of dryings to moisture, 1.72g solid powders are obtained, it is 19.5% to measure ellagic acid content.
Embodiment 8
It is 6.6% by the raspberry branches and leaves drying of stump to moisture, is crushed to 40 mesh, take 30g raspberries branch powder, adds 50% ethanol of 1800ml（Hydrochloric 2.7mol）Solution, return time 150min under the conditions of 85 DEG C, obtains the 72ml distilled water of the sediment after 200 mesh of ellagic acid crude extract are filtered and cleans in six times in neutrality, is 6.8% in 65 DEG C of dryings to moisture, 1.72g solid powders are obtained, it is 19.5% to measure ellagic acid content.
Embodiment 9
It is 7.1 % by the raspberry branches and leaves drying of stump to moisture, is crushed to 40 mesh, take 10g raspberries branch powder, adds 50% ethanol of 570ml（Hydrochloric 1.03mol）Solution, return time 150min under the conditions of 86 DEG C, obtains the 24ml distilled water of the sediment after 200 mesh of ellagic acid crude extract are filtered and cleans in six times in neutrality, is 6.5% in 55 DEG C of dryings to moisture, 0.62g solid powders are obtained, it is 18.9% to measure ellagic acid content.
Embodiment 10
It is 7.1 % by the raspberry branches and leaves drying of stump to moisture, is crushed to 40 mesh, take 20g raspberries branch powder, adds 50% ethanol of 1200ml（Hydrochloric 1.7mol）Solution, return time 150min under the conditions of 83 DEG C, obtains the 24ml distilled water of the sediment after 200 mesh of ellagic acid crude extract are filtered and cleans in six times in neutrality, is 6.8% in 55 DEG C of dryings to moisture, 1.3g solid powders are obtained, it is 18.7% to measure ellagic acid content.
Claims (4)
1., according to seminar's result of the test, the present invention extracts ellagic acid concentrate as processing raw material from raspberry branches and leaves.
2. the extraction conditions of the concentrate of pair right 1 are：, concentration of hydrochloric acid 1.2-2.0mol/L, concentration of alcohol is 50%, solid-liquid ratio 1:55-60（m/v）, return time 120-160min under the conditions of 85 DEG C, acquisition ellagic acid crude extract.
3. the product of right 1 is obtained using vacuum concentration, the method for cooling precipitation to the product of claim 2.
4. the products therefrom of pair right 3 removes residual salt acid group in the product using the method that distilled water is cleaned repeatedly.
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Cited By (7)
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| CN107417696A (en) * | 2017-07-17 | 2017-12-01 | 长沙爱扬医药科技有限公司 | A kind of method that raspberry glycosides and ellagic acid are extracted from raspberry |
| CN109497235A (en) * | 2018-12-27 | 2019-03-22 | 青海师范大学 | A kind of giving off a strong fragrance bush cinqefoil tea and its preparation method |
| CN110950882A (en) * | 2019-12-09 | 2020-04-03 | 上海焕生生物科技有限公司 | Method for extracting ellagic acid from blackberry seeds and blackberry leaves |
| CN113092650A (en) * | 2021-04-16 | 2021-07-09 | 云南中烟工业有限责任公司 | Detection method of raspberry glycoside in cigarette paper |
| CN113358765A (en) * | 2021-04-16 | 2021-09-07 | 云南省中医中药研究院 | Method for detecting raspberry glycoside content in plant |
| CN114605427A (en) * | 2022-03-25 | 2022-06-10 | 大连理工大学盘锦产业技术研究院 | Method for extracting and preparing raspberry ellagic acid |
| WO2024009260A1 (en) | 2022-07-07 | 2024-01-11 | Universidade De Aveiro | Method for the recovery of ellagic acid from industrial pulp mill streams |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107417696A (en) * | 2017-07-17 | 2017-12-01 | 长沙爱扬医药科技有限公司 | A kind of method that raspberry glycosides and ellagic acid are extracted from raspberry |
| CN109497235A (en) * | 2018-12-27 | 2019-03-22 | 青海师范大学 | A kind of giving off a strong fragrance bush cinqefoil tea and its preparation method |
| CN110950882A (en) * | 2019-12-09 | 2020-04-03 | 上海焕生生物科技有限公司 | Method for extracting ellagic acid from blackberry seeds and blackberry leaves |
| CN113092650A (en) * | 2021-04-16 | 2021-07-09 | 云南中烟工业有限责任公司 | Detection method of raspberry glycoside in cigarette paper |
| CN113358765A (en) * | 2021-04-16 | 2021-09-07 | 云南省中医中药研究院 | Method for detecting raspberry glycoside content in plant |
| CN114605427A (en) * | 2022-03-25 | 2022-06-10 | 大连理工大学盘锦产业技术研究院 | Method for extracting and preparing raspberry ellagic acid |
| WO2024009260A1 (en) | 2022-07-07 | 2024-01-11 | Universidade De Aveiro | Method for the recovery of ellagic acid from industrial pulp mill streams |
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