CN105497116A - Method for extracting polyphenol compounds from walnut shells - Google Patents
Method for extracting polyphenol compounds from walnut shells Download PDFInfo
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- CN105497116A CN105497116A CN201510886669.XA CN201510886669A CN105497116A CN 105497116 A CN105497116 A CN 105497116A CN 201510886669 A CN201510886669 A CN 201510886669A CN 105497116 A CN105497116 A CN 105497116A
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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)
- A61K36/52—Juglandaceae (Walnut family)
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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
- A61K2236/13—Preparation or pretreatment of starting material involving cleaning, e.g. washing or peeling
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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
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/17—Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
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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, 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
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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Abstract
The invention discloses a method for extracting polyphenol compounds from walnut shells. The method for extracting the polyphenol compounds from the walnut shells comprises steps as follows: 1), the walnut shells without kernels are cleaned, dried and smashed, a product is sieved and mixed with water, and a material-liquid ratio of the product to the water is 1%-5% (w/v); 2), a mixed liquid in the step 1) is placed into a conventional temperature-control pressure resisting device and is extracted at the temperature of 120-220 DEG C for 5-20 min; 3), heating is stopped, a sample is cooled, filtered and centrifuged, and the polyphenol compounds in the walnut shells are obtained. Compared with other conventional technologies for extracting natural polyphenol compounds, the method has the advantages as follows: (1), the cost is low, and only water is taken as a solvent; (2), the method is environment-friendly, an organic solvent is not used, so that the defect that the organic solvent is discharged as liquid waste and damages the environment is overcome, and the problem about liquid waste treatment is solved; (3), the extraction time is shorter, and the method is more efficient compared with a traditional extraction method.
Description
Technical field
The present invention relates to a kind of method utilizing green environmental protection technique to extract aldehydes matter in walnut shell.
Background technology
Semen Juglandis has another name called Semen Juglandis, and be one of large dry fruit in the world four, Semen Juglandis extensively distributes in the whole world.According to the data that United Nations Food and Agricultural Organization is announced, world's Semen Juglandis output about 3.4 × 10 in 2013
6ton, wherein the output of China is 1.7 × 10
6ton.Walnut shell is the garbage after Semen Juglandis gets Semen Juglandis, and walnut shell accounts for Semen Juglandis gross weight 67%, and the annual whole world about has 2 × 10
6ton walnut shell.Current most of walnut shell is burned, only has sub-fraction to be utilized, and is mainly used in filtering material, decontamination material etc.Utilization for walnut shell is scarcely out of swaddling-clothes, and mainly make use of its physical property, height indissolubility and adsorptivity etc.Relevant research for the deep processing of walnut shell chemical composition and utilization is less.Walnut shell main component is the biomass resource of lignin, cellulose, hemicellulose, simultaneously containing some phenols and quinones, has certain non-oxidizability and biocidal property, if can utilize a large amount of discarded walnut shell, can be a valuable wealth.
Phenolic ingredients in walnut shell is divided three classes, and is respectively phenolic acids, flavonoid, procyanidin class, specifically comprises phenolic acid, chlorogenic acid, gallic acid, P-coumaric acid, naphthoquinone nucin, flavone Quercetin, phenolic acid syringic acid, vanillin etc.In walnut shell, the anti-oxidation characteristics of aldehydes matter is mainly due to its redox property.They play reducing agent, hydrogen donor, metal-chelator, singlet oxygen quencher.Phenols can the activity of multiple enzyme in control agent, thus interferes the signaling mechanism of multiple cell processes.Therefore the natural components in Semen Juglandis can stop body oxidized, also can stop the destruction of radical pair human body simultaneously.
Mainly use organic solvent extraction for extracting phenol from natural product, but there is extraction ratio effect, extraction time is long, and energy resource consumption is large, has the problems such as pollution.
Summary of the invention
The object of the invention is to make full use of agricultural waste-walnut shell, and then the extracting method of polyphenolic substance in a kind of walnut shell is provided.
The object of the invention is to be achieved through the following technical solutions:
In walnut shell, an extracting method for polyphenolic substance, comprises the steps:
1) de-young walnut shell is cleaned, dries, is pulverized, sieve (40 order) and with water with 1 ~ 5%(w/v) solid-liquid ratio mix.
2) mixed liquor of step 1) being put into existing temperature control pressure-resistant apparatus, is extraction time 5 ~ 20min under the condition of 120 ~ 220 DEG C in temperature.
3) heating is stopped, cooling sample, overanxious, and centrifugal, obtain polyphenolic substance in walnut shell.
The present invention extracts the phenols in walnut shell and uses green, environmental protection, energy-conservation, extraction ratio is high, short Subcritical water chromotagraphy method consuming time.
Subcritical water is also referred to as pressure hot water, high-pressure water heating or superheated water.The critical point of water is temperature 374 DEG C, pressure 22.4Mpa, and when temperature is higher than 100 DEG C, during lower than critical temperature 374 DEG C, under pressure, water still keeps liquid condition.Along with the change of the temperature and pressure of water, the character of water itself also changes.When water temperature raises, its physicochemical property changes, especially its dielectric constant and ionic product.Relative dielectric constant can raise along with temperature and decline, and drops to 250 DEG C 27 from 25 DEG C 80, with methanol and ethanol 25 DEG C dielectric constant closely.The ionic product of water equals the product of hydrion and hydroxyl ion concentration, and ionic product also constantly increases along with the rising of temperature, and namely hydrion and hydroxide ion concentration increase.Therefore subcritical water and alternative organic solvent are as extractant, also can serve as acid base catalysator.It can dissolve or extract Semi-polarity product as the polarity in phenol, polycyclic aromatic hydrocarbon, quintessence oil and apolar substance.
The present invention, compared to the extractive technique of other natural polyphenol compounds existing, has the following advantages:
(1) low cost, just uses water as solvent.
(2) environmental protection, not with an organic solvent, then avoids organic solvent as this drawback of discharging of waste liquid welding, does not have the problem of liquid waste processing simultaneously.
(3) extraction time is shorter, and comparatively traditional extraction process is more efficient.
Detailed description of the invention
Illustrate below and technical scheme of the present invention is further described; but be not limited thereto; everyly technical solution of the present invention modified or equivalent to replace, and not departing from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
Detailed description of the invention one: the extracting method that present embodiments provide for polyphenolic substance in a kind of walnut shell, utilize free of contamination water as Extraction solvent, use controllable temperature pressure-resistant apparatus, with certain solid-liquid ratio, walnut shell powder is mixed with solvent, extract certain hour at a certain temperature, make polyphenol compound extraction rate reached in extracting solution to maximum.Concrete implementation step is as follows:
1, technological process
Walnut shell pulverizing → walnut shell fully mixes → is heated in pressure-resistant apparatus the certain reaction of design temperature → maintain during with water → stopping heats and cools → filter and centrifugal.
2, main technique key points for operation
1) setting of Extracting temperature
The polarity (dielectric constant) of Extraction solvent water is closely related with the temperature of system, considers the polarity then depending on solvent, so the selection of Extracting temperature is directly connected to the height of extraction ratio to the extraction of aldehydes matter in sample.
Setting extraction time and solid-liquid ratio are preset parameter, are respectively 5min and 2%.When Extracting temperature scope is 120 ~ 220 DEG C, the polyphenols extraction ratio in its extracting solution can reach 0.025 ~ 0.16mg/g.
2)
the setting of extraction time
The temperature of subcritical water is higher, and at high temperature the polarity of water weakens, and the viscosity of solvent also declines to some extent, be conducive to the stripping of the material of some low poles like this, but at a certain temperature, if extraction time is long, then can there is degradation reaction at polyphenols, reduce extraction ratio.
Extracting temperature be 180 DEG C, solid-liquid ratio be 2% time, extraction time, (reaching design temperature to count) was from 5 ~ 20min, and the polyphenols extraction ratio in its extracting solution can reach 0.025 ~ 0.10mg/g.
3) selection of solid-liquid ratio
Solid-liquid ratio is excessive, reduces extraction ratio, and solid-liquid ratio is too low, and production efficiency can reduce, and comprehensive extraction ratio and production efficiency should select the feed liquid be suitable for.
Extracting temperature be 180 DEG C, extraction time, when being 10min, its solid-liquid ratio was 1 ~ 5%(w/v), the polyphenols extraction ratio in extracting solution can reach 0.85 ~ 0.11mg/g.
Detailed description of the invention two: present embodiment provides the extracting method of polyphenolic substance in a kind of walnut shell, and concrete steps are as follows:
1) de-young walnut shell is cleaned, dries, is pulverized, sieve (40 order) and with water with 2%(w/v) solid-liquid ratio mix.
2) mixed liquor of step 1) being put into existing temperature control pressure-resistant apparatus, is extraction time 10min under the condition of 180 DEG C in temperature.
3) heating is stopped, cooling sample, overanxious, and it is centrifugal, get the content that extracting solution measures total phenolic compound and can reach 0.16mg/g, and extract in vitro antioxidation experiment (DPPH, FRAP) in show good antioxidant effect, result of the test is respectively 0.1134mg-VC/mg-sample, 0.3087mmolFeSO4/mL-extract.
Claims (5)
1. the extracting method of polyphenolic substance in walnut shell, is characterized in that described extracting method step is as follows:
1) de-young walnut shell is cleaned, dries, is pulverized, sieve and with water with 1 ~ 5%(w/v) solid-liquid ratio mix;
2) mixed liquor of step 1) being put into existing temperature control pressure-resistant apparatus, is extraction time 5 ~ 20min under the condition of 120 ~ 220 DEG C in temperature;
3) heating is stopped, cooling sample, overanxious, and centrifugal, obtain polyphenolic substance in walnut shell.
2. the extracting method of polyphenolic substance in walnut shell according to claim 1, is characterized in that described liquid ratio is 2%(w/v).
3. the extracting method of polyphenolic substance in walnut shell according to claim 1, is characterized in that described temperature is 180 DEG C.
4. the extracting method of polyphenolic substance in walnut shell according to claim 1, is characterized in that described extraction time is 10min.
5. the extracting method of polyphenolic substance in walnut shell according to claim 1, is characterized in that described to cross grit number be 40 orders.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510886669.XA CN105497116A (en) | 2015-12-07 | 2015-12-07 | Method for extracting polyphenol compounds from walnut shells |
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| CN201510886669.XA CN105497116A (en) | 2015-12-07 | 2015-12-07 | Method for extracting polyphenol compounds from walnut shells |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106805180A (en) * | 2017-01-13 | 2017-06-09 | 江南大学 | A kind of method that polyphenol substance is extracted in desmoenzyme and the ultrasonically treated endotesta walnut kernel by band |
| CN107674753A (en) * | 2017-09-30 | 2018-02-09 | 衢州刘家香食品有限公司 | A kind of processing method of walnut oil |
| CN111514097A (en) * | 2020-05-14 | 2020-08-11 | 燕山大学 | Preparation method of pH-responsive nano hydrogel of walnut shell polyphenol |
| RU2800829C1 (en) * | 2022-12-26 | 2023-07-28 | федеральное государственное автономное образовательное учреждение высшего образования "Санкт-Петербургский политехнический университет Петра Великого" (ФГАОУ ВО "СПбПУ") | Method for obtaining polyphenolic substances from walnut partitions |
-
2015
- 2015-12-07 CN CN201510886669.XA patent/CN105497116A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 金海涛等: "亚临界水法提取稻糠中酚类活性物质及其组分鉴定", 《粮食加工》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106805180A (en) * | 2017-01-13 | 2017-06-09 | 江南大学 | A kind of method that polyphenol substance is extracted in desmoenzyme and the ultrasonically treated endotesta walnut kernel by band |
| CN106805180B (en) * | 2017-01-13 | 2020-08-07 | 江南大学 | Method for extracting polyphenol substance from walnut kernel with inner seed coat by combining enzyme and ultrasonic treatment |
| CN107674753A (en) * | 2017-09-30 | 2018-02-09 | 衢州刘家香食品有限公司 | A kind of processing method of walnut oil |
| CN111514097A (en) * | 2020-05-14 | 2020-08-11 | 燕山大学 | Preparation method of pH-responsive nano hydrogel of walnut shell polyphenol |
| CN111514097B (en) * | 2020-05-14 | 2022-02-11 | 燕山大学 | Preparation method of pH-responsive nano hydrogel of walnut shell polyphenol |
| RU2800829C1 (en) * | 2022-12-26 | 2023-07-28 | федеральное государственное автономное образовательное учреждение высшего образования "Санкт-Петербургский политехнический университет Петра Великого" (ФГАОУ ВО "СПбПУ") | Method for obtaining polyphenolic substances from walnut partitions |
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