CN102697849B - Method for extracting total polyphenol from pecan peels - Google Patents
Method for extracting total polyphenol from pecan peels Download PDFInfo
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- CN102697849B CN102697849B CN201210145991.3A CN201210145991A CN102697849B CN 102697849 B CN102697849 B CN 102697849B CN 201210145991 A CN201210145991 A CN 201210145991A CN 102697849 B CN102697849 B CN 102697849B
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Abstract
The invention belongs to the field of extracting functional components of plants and specifically relates to a method for extracting total polyphenol from pecan peels. The method includes: adding ethanol water solution serving as the solvent into dry powder of pecan peels, wherein the proportion of the quality of the dry powder and the volume of the solvent is 1: (5-10); performing ultrasonic extracting at the temperature of 30-60 DEG C for 30-60 minutes, and filtering the extracting liquid; and performing rotary evaporation concentration and freezing drying on the obtained filtrate to obtain products of total polyphenol of the pecan peels. The method adopts the ultrasonic extracting technology, greatly improves extracting rate of active constituents, reduces waste of plant resources and solves the problem of pollution caused by waste pecan peels, and biological activity of the extractive is intact.
Description
Technical field
The invention belongs to plant function composition and extract field, be specifically related to a kind of extracting method of Semen Caryae Cathayensis Pu shell total polyphenols.
Background technology
Semen Caryae Cathayensis Juglans Mandshurica Maxim, is Juglandaceae Juglandaceae, hickory Carya plant, and main product is in Linan, Zhejiang, Chunan and Anji and other places.When Semen Caryae Cathayensis immaturity, there is the thick green Pu shell of one deck core outside, along with Semen Caryae Cathayensis gradually ripe and plucked and peeled off after, this Pu shell color can become reddish brown gradually.Semen Caryae Cathayensis Pu shell amount after peeling off is very large, and the weight ratio of fruit and Pu shell is almost 1:3.A large amount of discarded Semen Caryae Cathayensis Pu shells, have seriously polluted local environment, have affected local ecology, are thorny the difficult problem of environmental protections always.
According to the literature, Hickory Leaves, bark and Pu shell all can be used as medicine, and Semen Caryae Cathayensis bark bitter in the mouth is pungent, cold in nature can heat clearing away, dampness, bowel relieving, parasite killing.It is applied to treatment digestive system, tumor in recent years, especially evident in efficacy to esophageal carcinoma, gastric cancer.Its property of Semen Caryae Cathayensis Pu shell is light, and bitter and puckery flavor has the effects such as antitumor, easing pain and diminishing inflammation, bacteriostasis and sterilization, repellent antipruritic, clearing away heat and promoting diuresis, improving eyesight removing toxic substances.Therefore, how making good use of Semen Caryae Cathayensis Pu shell, turn waste into wealth, is a problem in the urgent need to address.
Plant polyphenol refers to the glucose by gallic acid or its polymer and the polymer of polyhydric alcohol, flavonol and derivant thereof and the plant polyhydric phenols that the mixing of the two forms jointly in plant.In recent years, along with the continuous intensification of people to plant polyphenol and structure and chemical property understanding, the research of plant polyphenol physiologically active and application thereof has become one of focus of its research in recent years.
Modern medicine study shows, human body is in metabolic process, and the various diseases that the superfluous free radical producing because of various environmental factorss can cause people is as atherosclerosis, hypertension, cataract, cancer etc.Plant polyphenol has the ability of removing free radical, and the biomacromolecule that free radical is brought out damage plays a protective role.
Non-oxidizability is also a critical nature of plant polyphenol, ortho position phenolic hydroxyl group in phenolic hydroxyl structure catechol or pyrogallol in polyphenol is easy to be oxidized to quinones structure, the free radicals such as active oxygen are had to very strong capturing ability, the ability that this makes polyphenol have stronger non-oxidizability and remove free radical simultaneously.In addition, plant polyphenol has stronger absorbability in ultraviolet and far-ultraviolet region, and therefore plant polyphenol can reduce the sickness rate of cancer, cardiovascular disease, arthritis chronic diseases.
Ultrasound wave is a kind of elastic mechanical vibration wave, and the extraction that it is applied to pharmaceutical analysis and chemical composition as a kind of extractive technique has had the research history of two more than ten years.Ultrasound assisted extraction technique is to utilize the multiple main second order effects such as ultrasonic cavitation effect, mechanical vibration, heat effect, in fluid, produce the High Temperature High Pressure field of moment, the surface of solids in convection cell produces powerful shearing force, accelerate stripping and the strengthening mass transport process of active skull cap components, so also claim ultrasound-enhanced extraction.
The extracting method that plant polyphenol adopts at present mainly contains water extraction, organic solvent extractionprocess, using microwave-assisted and ultrasonic extraction etc.Water extraction cost is low, safely, be suitable for suitability for industrialized production, but aqueous polar is large, the compositions such as albumen, sugar, inorganic salt also easily extract simultaneously, product purity is low.Organic solvent extractionprocess have extraction efficiency high, be easy to realize the advantages such as suitability for industrialized production, be the extracting method of extensive use, but its needed time is long, consumption of organic solvent is larger.Microwave extraction method has advantages of that extraction time is short and consumption of organic solvent is few, but microwave extracting also exists some problems in theory and practice.Ultrasonic secondary solvent extraction extraction time is short, and solvent use amount is few, and extraction process temperature is low, is conducive to keep the biological activity of polyphenol, meets environment protection requirement.
At present, the comprehensive utilization of Semen Caryae Cathayensis Pu shell is at the early-stage, is mainly used in firing charcoal, and added value of product is not high.And polyphenol component is wherein extracted, provide concrete technology parameter, process and the step extracted in separating there are no report.
Summary of the invention
The object of this invention is to provide a kind of technique simple, extraction ratio is high, cost is low, the extracting method of pollution-free, the Semen Caryae Cathayensis Pu shell total polyphenols of turning waste into wealth.
Particularly, inventor provides following technical scheme:
An extracting method for Semen Caryae Cathayensis Pu shell total polyphenols, comprising:
In Semen Caryae Cathayensis Pu shell dry powder, add ethanol water solvent, dry powder quality and solvent volume are than being 1:5-10, then at 30 ℃ of-60 ℃ of temperature, carry out ultrasonic extraction, extraction time is 30min-60min, extracting liquid filtering, the filtrate obtaining again and lyophilization concentrated through rotary evaporation obtains Semen Caryae Cathayensis Pu shell total polyphenols product.
As preferably, according to the extracting method of a kind of Semen Caryae Cathayensis Pu shell total polyphenols of the present invention, wherein, described Semen Caryae Cathayensis Pu shell dry powder is processed rear use as follows: after the Semen Caryae Cathayensis Pu shell that contains polyphenol compound is cleaned, at 40 ℃～60 ℃ temperature, being dried to moisture is 5%～10%, then pulverize and cross 30 mesh sieves, obtaining the Pu shell dry powder that contains polyphenol compound.
As preferably, according to the extracting method of a kind of Semen Caryae Cathayensis Pu shell total polyphenols of the present invention, wherein, described ethanol water concentration is 50%～80% V/V.
As preferably, according to the extracting method of a kind of Semen Caryae Cathayensis Pu shell total polyphenols of the present invention, wherein, the hyperacoustic power bracket in described ultrasonic extraction is 50w～200w.
As preferably, according to the extracting method of a kind of Semen Caryae Cathayensis Pu shell total polyphenols of the present invention, wherein, the temperature of described rotary evaporation is 30 ℃～50 ℃, concentrates and removes organic solvent and most of moisture, obtains concentrated solution.
As preferably, according to the extracting method of a kind of Semen Caryae Cathayensis Pu shell total polyphenols of the present invention, wherein, in described lyophilization: temperature is that-45 ℃～-60 ℃, vacuum are 2Pa-10Pa.Concentrated solution is dried to quality in vacuum freeze drier no longer to be changed.
Compared with prior art, the present invention has the following advantages:
1. the present invention has adopted ultrasonic wave extraction, and the extraction ratio of effective ingredient is improved greatly, has reduced the waste of plant resources.
2. owing to adopting ultrasound wave auxiliary extraction technology, the use amount of organic solvent greatly reduces, and cost is lowered, and pollute and reduce, and concentration process also shortens greatly.
3. traditional extracting method is wanted 24 hours as extracted in Soxhlet.Cold-maceration needs 48 hours even for more time, and the ultrasonic extraction time obviously reduces, and extraction efficiency improves.
4. ultrasound assisted extraction technique is a kind of low-temperature physics leaching process, so the biological activity of extract is intact.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of the extracting method of a kind of Semen Caryae Cathayensis Pu of the present invention shell total polyphenols.
Fig. 2 is the comparison diagram of the embodiment of the present invention 1 and comparative example Semen Caryae Cathayensis Pu shell total polyphenols extraction ratio.
The specific embodiment
Below in conjunction with embodiment, be described more specifically content of the present invention.Should be appreciated that enforcement of the present invention is not limited to the following examples, any pro forma accommodation that the present invention is made and/or change all will fall into protection domain of the present invention.
In the present invention, if not refer in particular to, all part, percentage ratios are unit of weight, and all equipment and raw materials etc. all can be buied from market or the industry is conventional.Method in following embodiment, if no special instructions, is the conventional method of this area.
The capital equipment that the embodiment of the present invention is used:
Ultrasonic extractor: Kunshan Ultrasonic Instruments Co., Ltd.,
Vacuum freeze drier: LABCONCO company of the U.S.,
Rotary evaporator: Shanghai Yarong Biochemical Instrument Plant.
Semen Caryae Cathayensis Pu shell dry powder described in embodiment is processed rear use as follows: the Semen Caryae Cathayensis Pu shell that contains polyphenol compound is cleaned, then at 40 ℃～60 ℃ temperature, is dried to moisture is 5%～10%, pulverize again and cross 30 mesh sieves, obtaining the Semen Caryae Cathayensis Pu shell dry powder that contains polyphenol compound.
embodiment 1
Get the beaker that Semen Caryae Cathayensis Pu shell powder that 50g pulverized 30 mesh sieves is placed in 1000ml, add in the ethanol water of 500ml 50% and soak 4h, then ultrasonic extraction 40min, hyperacoustic power is 150w, extracting temperature is 30 ℃, collection extracting solution after extraction completes, 40 ℃ of rotary evaporation in vacuo are concentrated, concentrated organic solvent and the most of moisture of removing, the concentrated solution obtaining carries out vacuum lyophilization, temperature is-45 ℃, vacuum is 2Pa, concentrated solution is dried to quality in vacuum freeze drier no longer to be changed, obtain Semen Caryae Cathayensis Pu shell total polyphenols product-brownish red pressed powder 11.04g.Measuring Determination of Polyphenols in extract is 38.25%.Assay method: the mensuration of total polyphenols adopts Folin-Ciocalteus method.
comparative example
Get the beaker that Semen Caryae Cathayensis Pu shell powder that 50g pulverized 30 mesh sieves is placed in 1000ml, add in the ethanol water of 500ml 50% and soak 4h, collection extracting solution after extraction completes, 40 ℃ of rotary evaporation in vacuo are concentrated, and vacuum lyophilization concentrated solution, the temperature of vacuum lyophilization, for-45 ℃, vacuum are 2Pa, obtains brownish red pressed powder 8.24g.Measuring Determination of Polyphenols in extract is 32.18%.Assay method: the mensuration of total polyphenols adopts Folin-Ciocalteus method.
embodiment 2
Get the beaker that Semen Caryae Cathayensis Pu shell powder that 50g pulverized 30 mesh sieves is placed in 1000ml, add in the ethanol water of 500ml 60% and soak 2h, then ultrasonic extraction 30min, ultrasonic power is 100w, extracting temperature is 40 ℃, collection extracting solution after extraction completes, 40 ℃ of rotary evaporation in vacuo are concentrated, concentrated organic solvent and the most of moisture of removing, the concentrated solution obtaining carries out vacuum lyophilization, temperature is-45 ℃, vacuum is 8Pa, concentrated solution is dried to quality in vacuum freeze drier no longer to be changed, obtain Semen Caryae Cathayensis Pu shell total polyphenols product-brownish red pressed powder 10.36g.Measuring Determination of Polyphenols in extract through Folin-Ciocalteus method is 39.13%.
embodiment 3
Get the beaker that Semen Caryae Cathayensis Pu shell powder that 50g pulverized 30 mesh sieves is placed in 1000ml, add in the ethanol water of 400ml 70% and soak 2h, then ultrasonic extraction 60min, ultrasonic power is 200w, extracting temperature is 30 ℃, collection extracting solution after extraction completes, 30 ℃ of rotary evaporation in vacuo are concentrated, concentrated organic solvent and the most of moisture of removing, the concentrated solution obtaining carries out vacuum lyophilization, temperature is-50 ℃, vacuum is 5Pa, concentrated solution is dried to quality in vacuum freeze drier no longer to be changed, obtain Semen Caryae Cathayensis Pu shell total polyphenols product-brownish red pressed powder 12.46g.Measuring Determination of Polyphenols in extract through Folin-Ciocalteus method is 37.34%.
Get the beaker that Semen Caryae Cathayensis Pu shell powder that 50g pulverized 30 mesh sieves is placed in 1000ml, add in the ethanol water of 250ml 80% and soak 3h, then ultrasonic extraction 50min, hyperacoustic power is 50w, extracting temperature is 60 ℃, collection extracting solution after extraction completes, 50 ℃ of rotary evaporation in vacuo are concentrated, concentrated organic solvent and the most of moisture of removing, the concentrated solution obtaining carries out vacuum lyophilization, temperature is-60 ℃, vacuum is 10Pa, concentrated solution is dried to quality in vacuum freeze drier no longer to be changed, obtain Semen Caryae Cathayensis Pu shell total polyphenols product-brownish red pressed powder 12.44g.Measuring Determination of Polyphenols in extract is 38.75%.Assay method: the mensuration of total polyphenols adopts Folin-Ciocalteus method.
Above preferred embodiment, just for description and interpretation content of the present invention, does not form the restriction to content of the present invention.Although inventor has done in more detail and has enumerated the present invention, but, the content that those skilled in the art discloses according to summary of the invention part and embodiment, can make various modifications or/and supplement or to adopt similar mode to substitute be obvious to described specific embodiment, and can realize technique effect of the present invention, therefore, repeat no longer one by one herein.The term occurring in the present invention, for the elaboration to technical solution of the present invention and understanding, is not construed as limiting the invention.
Claims (1)
1. an extracting method for Semen Caryae Cathayensis Pu shell total polyphenols, is characterized in that comprising:
In Semen Caryae Cathayensis Pu shell dry powder, add ethanol water solvent, the ratio of dry powder quality and solvent volume is 1:5～10, then at 30 ℃～60 ℃ temperature, carry out ultrasonic extraction, extraction time is 30min～60min, extracting liquid filtering, the filtrate obtaining again and lyophilization concentrated through rotary evaporation obtains Semen Caryae Cathayensis Pu shell total polyphenols product
Described Semen Caryae Cathayensis Pu shell dry powder is processed rear use as follows: it is 5%～10% that Semen Caryae Cathayensis Pu shell is dried to moisture at 40 ℃～60 ℃ temperature, then pulverizes and crosses 30 mesh sieves, obtains Pu shell dry powder,
Described ethanol water concentration is 50%～80% V/V,
Hyperacoustic power bracket in described ultrasonic extraction is 50w～200w,
The temperature of described rotary evaporation is 30 ℃～50 ℃,
In described lyophilization: temperature is that-45 ℃～-60 ℃, vacuum are 2Pa-10Pa.
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| CN102973645A (en) * | 2012-12-11 | 2013-03-20 | 青岛海洋新材料科技有限公司 | Extracting method for pecan shell polyphenol |
| CN104208138B (en) * | 2014-10-08 | 2018-06-15 | 大理大学 | Steep walnut shell extract application in preparation of anti-tumor drugs |
| CN105418693B (en) * | 2015-10-31 | 2018-03-02 | 中北大学 | The application of the extracting method of tannin and its gained tannin in a kind of walnut shell |
| 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 |
| CN107298695A (en) * | 2017-08-09 | 2017-10-27 | 浙江大学 | A kind of method for extracting pecan shell sterol |
| CN107751527A (en) * | 2017-10-24 | 2018-03-06 | 江南大学 | The preparation method and Chinese herbal medicine candy of a kind of pharynx-clearing throat-benefiting Chinese herbal medicine candy |
| CN110302240A (en) * | 2018-10-24 | 2019-10-08 | 河北科技大学 | The method for extracting polyphenol in walnut Diaphragma juglandis |
| CN115644302A (en) * | 2022-05-31 | 2023-01-31 | 中国计量大学 | Method for improving emulsification property of whey protein isolate |
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Inventor after: Fang Xiangjun Inventor after: Gao Haiyan Inventor after: Chen Hangjun Inventor after: Chen Wenhui Inventor after: Tao Fei Inventor after: Mao Jinlin Inventor before: Gao Haiyan Inventor before: Fang Xiangjun Inventor before: Chen Hangjun Inventor before: Chen Wenhui Inventor before: Tao Fei Inventor before: Mao Jinlin |
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