CN106188322B - The extracting method of wolfberry fruit extract - Google Patents
The extracting method of wolfberry fruit extract Download PDFInfo
- Publication number
- CN106188322B CN106188322B CN201610542203.2A CN201610542203A CN106188322B CN 106188322 B CN106188322 B CN 106188322B CN 201610542203 A CN201610542203 A CN 201610542203A CN 106188322 B CN106188322 B CN 106188322B
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- matrimony vine
- mixture
- filtrate
- obtains
- filters
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- 244000241838 Lycium barbarum Species 0.000 title claims abstract description 51
- 235000015459 Lycium barbarum Nutrition 0.000 title claims abstract description 51
- 239000000284 extract Substances 0.000 title claims abstract description 18
- 235000015468 Lycium chinense Nutrition 0.000 title claims abstract description 16
- 235000013399 edible fruits Nutrition 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 24
- 239000000706 filtrate Substances 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010894 electron beam technology Methods 0.000 claims abstract description 8
- 235000019441 ethanol Nutrition 0.000 claims abstract description 8
- 239000003960 organic solvent Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000009835 boiling Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 125000005909 ethyl alcohol group Chemical group 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 239000003643 water by type Substances 0.000 claims abstract description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 4
- 239000003208 petroleum Substances 0.000 claims description 4
- 235000002710 Ilex cornuta Nutrition 0.000 claims 1
- 241001310146 Ilex cornuta Species 0.000 claims 1
- 235000010326 Osmanthus heterophyllus Nutrition 0.000 claims 1
- 238000000605 extraction Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- VYLQGYLYRQKMFU-UHFFFAOYSA-N Ochratoxin A Natural products CC1Cc2c(Cl)cc(CNC(Cc3ccccc3)C(=O)O)cc2C(=O)O1 VYLQGYLYRQKMFU-UHFFFAOYSA-N 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- RWQKHEORZBHNRI-BMIGLBTASA-N ochratoxin A Chemical compound C([C@H](NC(=O)C1=CC(Cl)=C2C[C@H](OC(=O)C2=C1O)C)C(O)=O)C1=CC=CC=C1 RWQKHEORZBHNRI-BMIGLBTASA-N 0.000 description 1
- DAEYIVCTQUFNTM-UHFFFAOYSA-N ochratoxin B Natural products OC1=C2C(=O)OC(C)CC2=CC=C1C(=O)NC(C(O)=O)CC1=CC=CC=C1 DAEYIVCTQUFNTM-UHFFFAOYSA-N 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Sustainable Development (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of extracting methods of wolfberry fruit extract, including:1 portion of matrimony vine is placed in drying box, water content≤5% of matrimony vine is dried to, is ground;Intensity is used to be irradiated for the electron beam of 10kGy;To a concentration of 70%, for pH value for matrimony vine powder is added in 5 ethyl alcohol, water bath sonicator 5min stirs 1h, filters, and obtains the first filtrate and the first filter residue, rotates the first filtrate, obtains mixture A;First filter residue is placed in 8 parts of organic solvents, water bath sonicator 5min, stirs 30min, filtered, obtain the second filtrate, rotated the second filtrate, obtain mixture B;50 parts of deionized waters are added in second filter residue, and boiling 10min is cooled to 30 DEG C, it filters, obtains third filtrate, be evaporated under reduced pressure, mixture C is obtained, mixture A, mixture B and mixture C are placed in 15 parts of absolute ethyl alcohols, is placed in the water-bath that temperature is 50 DEG C, 20min is stirred, is placed in refrigerator, in the case where temperature is 5 DEG C, stand 10h, it filters, filters out liquid to get to wolfberry fruit extract.The present invention realizes the extraction to nutriment highly effective and safe in matrimony vine.
Description
Technical field
The present invention relates to a kind of extracting methods of wolfberry fruit extract.
Background technology
With the expanding economy in China and the continuous improvement of living standards of the people, people to the health of itself also increasingly
Pay attention to, health product is that people are usually used in one of food of health care day, and in health food, most of health products are plant extract
Class product, type is varied, but many plants extraction product needs to expend a large amount of raw material, causes price height
It is high.
Invention content
It is an object of the invention to solve at least the above, and provide the advantages of at least will be described later.
It is a still further object of the present invention to provide a kind of extracting methods of wolfberry fruit extract, can efficiently extract in matrimony vine
Contained nutriment.
In order to realize these purposes and other advantages according to the present invention, a kind of extracting method of wolfberry fruit extract is provided,
Including:
According to the mass fraction,
Step 1: 1 portion of matrimony vine is placed in drying box, at 70 DEG C, it is dried to water content≤5% of matrimony vine, grinds, obtains
To matrimony vine powder;
Step 2: intensity is used to irradiate matrimony vine powder for the electron beam of 10kGy;
Step 3: with citric acid solution, the pH value of 10 parts a concentration of 70% of ethyl alcohol is adjusted to 5, matrimony vine powder is added,
Bath temperature be 40 DEG C at, water bath sonicator 5min, bath temperature be 50 DEG C at, stir 1h, filter, obtain the first filtrate and
First filter residue rotates the first filtrate, obtains mixture A;
Step 4: the first filter residue is placed in 8 parts of organic solvents, in the case where bath temperature is 30 DEG C, water bath sonicator 5min,
At 40 DEG C, 30min is stirred, is filtered, the second filtrate and the second filter residue are obtained, the second filtrate is rotated, obtains mixture B;
Step 5: 50 parts of deionized waters are added in the second filter residue, at 3MPa, at 150 DEG C, boiling 10min is cooled to 30
DEG C, it filters, obtains third filtrate, be evaporated under reduced pressure, obtain mixture C;
Step 6: mixture A, mixture B and mixture C are placed in 15 parts of absolute ethyl alcohols, it is 50 DEG C to be placed in temperature
In water-bath, 20min is stirred, is placed in refrigerator, in the case where temperature is 5 DEG C, stood 10h, filter, filter out liquid and carried to get to matrimony vine
Take object.
Preferably, in the extracting method of the wolfberry fruit extract, in the step 1,1 portion of matrimony vine is placed in drying
In case, at 70 DEG C, it is dried to water content≤5% of matrimony vine, the particle that grain size is 20 μm is ground into, obtains matrimony vine powder.
Preferably, in the extracting method of the wolfberry fruit extract, in the step 2, use intensity for 10kGy's
Electron beam irradiates matrimony vine powder 3min.
Preferably, in the extracting method of the wolfberry fruit extract, in the step 4, organic solvent includes following matter
Measure the component of score:55% dichloromethane and 45% petroleum ether.
The present invention includes at least following advantageous effect:The first, matrimony vine is ground into the particle that grain size is 20 μm in the present invention,
Recovery rate is greatly increased, while its internal structure will not be destroyed again;The second, the present invention uses mixed organic solvents, solves
The halfway problem that single solvent extracts nutritional ingredient, while the dichloromethane and petroleum ether low boiling point selected, are easy
It removes, is not easy to remain, the effective safety for ensureing extract;The method that water bath sonicator is used in third, the present invention, increases battalion
The dissolving of foster substance in a solvent;4th, matrimony vine powder is irradiated using electron beam in the present invention, life powder can be effectively removed
Contained in Ochratoxin A;5th, boiling is carried out to matrimony vine using the method for thermophilic digestion in the present invention, improves extraction
Efficiency.
Part is illustrated to embody by further advantage, target and the feature of the present invention by following, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail, to enable those skilled in the art with reference to specification
Word can be implemented according to this.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or more
The presence or addition of a other elements or combinations thereof.
The present invention provides a kind of extracting method of wolfberry fruit extract, including:
Step 1: 1g matrimony vines are placed in drying box, at 70 DEG C, it is dried to water content≤5% of matrimony vine, grinds, obtains
To matrimony vine powder;
Step 2: intensity is used to irradiate matrimony vine powder for the electron beam of 10KGy;
Step 3: with citric acid solution, the pH value of the ethyl alcohol of 10g a concentration of 70% is adjusted to 5, matrimony vine powder is added,
Bath temperature be 40 DEG C at, water bath sonicator 5min, bath temperature be 50 DEG C at, stir 1h, filter, obtain the first filtrate and
First filter residue rotates the first filtrate, obtains mixture A;
Step 4: the first filter residue is placed in 8g organic solvents, in the case where bath temperature is 30 DEG C, water bath sonicator 5min,
At 40 DEG C, 30min is stirred, is filtered, the second filtrate and the second filter residue are obtained, the second filtrate is rotated, obtains mixture B;
Step 5: 50g deionized waters are added in the second filter residue, at 3MPa, at 150 DEG C, boiling 10min is cooled to 30
DEG C, it filters, obtains third filtrate, be evaporated under reduced pressure, obtain mixture C;
Step 6: mixture A, mixture B and mixture C are placed in 15g absolute ethyl alcohols, it is placed in the water that temperature is 50 DEG C
In bath, 20min is stirred, is placed in refrigerator, in the case where temperature is 5 DEG C, stood 10h, filter, filter out liquid and extracted to get to matrimony vine
Object.
In one embodiment, in step 1,1g matrimony vines are placed in drying box, at 70 DEG C, are dried to matrimony vine
Water content≤5% is ground into the particle that grain size is 20 μm, obtains matrimony vine powder.
In one embodiment, in step 1, in step 2, intensity is used to irradiate wolfberry fruit powder for the electron beam of 10kGy
Last 3min.
In one embodiment, in step 1, in step 4, organic solvent includes the component of following mass fraction:
55% dichloromethane and 45% petroleum ether.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details.
Claims (3)
1. a kind of extracting method of wolfberry fruit extract, which is characterized in that including:
According to the mass fraction,
Step 1: 1 portion of matrimony vine is placed in drying box, at 70 DEG C, it is dried to water content≤5% of matrimony vine, grinds, obtains Chinese holly
Qi powder;
Step 2: intensity is used to irradiate matrimony vine powder for the electron beam of 10kGy;
Step 3: with citric acid solution, the pH value of 10 parts a concentration of 70% of ethyl alcohol is adjusted to 5, matrimony vine powder is added, in water
Bath temperature is that water bath sonicator 5min at 40 DEG C stirs 1h in the case where bath temperature is 50 DEG C, filters, obtains the first filtrate and first
Filter residue rotates the first filtrate, obtains mixture A;
Step 4: the first filter residue is placed in 8 parts of organic solvents, in the case where bath temperature is 30 DEG C, water bath sonicator 5min, at 40 DEG C
Under, 30min is stirred, is filtered, the second filtrate and the second filter residue are obtained, the second filtrate is rotated, obtains mixture B;
Step 5: 50 parts of deionized waters are added in the second filter residue, at 3MPa, at 150 DEG C, boiling 10min is cooled to 30 DEG C,
It filters, obtains third filtrate, be evaporated under reduced pressure, obtain mixture C;
Step 6: mixture A, mixture B and mixture C are placed in 15 parts of absolute ethyl alcohols, it is placed in the water-bath that temperature is 50 DEG C
In, 20min is stirred, is placed in refrigerator, in the case where temperature is 5 DEG C, 10h is stood, filters, filters out liquid to get to wolfberry fruit extract;
In the step 4, organic solvent includes the component of following mass fraction:55% dichloromethane and 45% petroleum ether.
2. the extracting method of wolfberry fruit extract as described in claim 1, which is characterized in that in the step 1, by 1 portion of matrimony vine
It is placed in drying box, at 70 DEG C, is dried to water content≤5% of matrimony vine, be ground into the particle that grain size is 20 μm, obtain matrimony vine
Powder.
3. the extracting method of wolfberry fruit extract as described in claim 1, which is characterized in that in the step 2, using intensity
Matrimony vine powder 3min is irradiated for the electron beam of 10kGy.
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Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101348529A (en) * | 2008-09-08 | 2009-01-21 | 北京联合大学生物化学工程学院 | Extraction and separation method of medlar polysaccharide |
CN101817749A (en) * | 2009-11-18 | 2010-09-01 | 青海青美生物资源研究开发有限公司 | Method for extracting chlorogenic acid from Chinese wolfberry |
CN102000208A (en) * | 2010-11-09 | 2011-04-06 | 中国科学院西北高原生物研究所 | Method for extracting and preparing medlar leaf flavone |
CN102659741A (en) * | 2012-04-27 | 2012-09-12 | 宁夏大学 | Method for extracting and preparing active ingredients of Ningxia wolfberries |
CN103772526A (en) * | 2014-02-21 | 2014-05-07 | 香港理工大学深圳研究院 | Method for efficiently extracting polysaccharide active ingredients in lycium barbarum by using ultrasound enhanced subcritical water |
CN104447470A (en) * | 2014-12-19 | 2015-03-25 | 宁夏农林科学院 | Method for preparing lycium barbarum lutein by HSCCC (high-speed countercurrent chromatography) separation |
CN105218694A (en) * | 2015-10-28 | 2016-01-06 | 青海尤尼克生物技术有限公司 | A kind of Lycium barbarum polysaccharide extract and preparation method thereof |
-
2016
- 2016-07-11 CN CN201610542203.2A patent/CN106188322B/en active Active
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101348529A (en) * | 2008-09-08 | 2009-01-21 | 北京联合大学生物化学工程学院 | Extraction and separation method of medlar polysaccharide |
CN101817749A (en) * | 2009-11-18 | 2010-09-01 | 青海青美生物资源研究开发有限公司 | Method for extracting chlorogenic acid from Chinese wolfberry |
CN102000208A (en) * | 2010-11-09 | 2011-04-06 | 中国科学院西北高原生物研究所 | Method for extracting and preparing medlar leaf flavone |
CN102659741A (en) * | 2012-04-27 | 2012-09-12 | 宁夏大学 | Method for extracting and preparing active ingredients of Ningxia wolfberries |
CN103772526A (en) * | 2014-02-21 | 2014-05-07 | 香港理工大学深圳研究院 | Method for efficiently extracting polysaccharide active ingredients in lycium barbarum by using ultrasound enhanced subcritical water |
CN104447470A (en) * | 2014-12-19 | 2015-03-25 | 宁夏农林科学院 | Method for preparing lycium barbarum lutein by HSCCC (high-speed countercurrent chromatography) separation |
CN105218694A (en) * | 2015-10-28 | 2016-01-06 | 青海尤尼克生物技术有限公司 | A kind of Lycium barbarum polysaccharide extract and preparation method thereof |
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Effective date of registration: 20220323 Address after: 710018 room 1904, block B, baihualin international, No. 16, Wenjing Road, economic development zone, Xi'an, Shaanxi Province Patentee after: Shaanxi Huaze Biotechnology Co.,Ltd. Address before: 530500 No. 13, Gongxun Zhuang, Dashan Village, Xiangxian Town, Shanglin County, Nanning City, Guangxi Zhuang Autonomous Region Patentee before: Zhou Hansheng |