CN113318134A - Extraction method and application of Korean pine needle polyphenol compounds - Google Patents
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Abstract
The invention belongs to the technical field of biological medicine, and particularly relates to an extraction method and application of Korean pine needle polyphenol compounds, which comprises the following steps: firstly, preprocessing pine needles of the Korean pine, drying, cleaning and sterilizing the pine needles of the Korean pine, and then putting the sterilized pine needles of the Korean pine into a constant-temperature drying box at 40 ℃ until the pine needles of the Korean pine are completely dried; step two: putting the treated pine needles of the Korean pine into a high-speed crusher for crushing, putting the completely dried pine needles of the Korean pine into the high-speed crusher for electric crushing, and then sieving by a sieve of 60 meshes for screening; step three: taking a proper amount of pine needle powder to perform high shear extraction according to a certain material-liquid ratio, performing centrifugal filtration to obtain a pine needle polyphenol extracting solution, selecting pine needle powder and an ethanol solution with the purity of 60% according to the ratio of 1:10, adding the pine needle powder and the ethanol solution into a container, and extracting by a high-shear emulsifying dispersion machine at the temperature of 40 ℃, wherein the high-shear emulsifying dispersion machine has the advantages of reasonable structure, high extraction rate, short extraction time, small solvent consumption and small tool abrasion.
Description
Technical Field
The invention relates to the technical field of biological medicines, in particular to an extraction method and application of Korean pine needle polyphenol compounds.
Background
Pine needles are leaves of the plant of the genus pinus of the family pinaceae of the gymnosperm, and are extremely abundant in our country, and the leaves of the plant of the genus pinus are rarely developed and utilized, thus causing a great deal of waste of resources. The pine needle tea in China is developed later, the process is simple, the tea is mainly drunk by directly making tea with the primarily processed pine needle dry product, and the long-term drinking of the pine needle tea can play a certain health care role in reducing blood pressure and blood sugar. The domestic scholars think that the effective components in the pine needles are phenol acid components and the pine needle polyphenol is the main component. For the extraction process of pine needle polyphenol, domestic literature mostly uses ethanol with a certain volume fraction as an extraction solvent, and the yield is low.
At present, the commonly used extraction methods comprise the traditional organic solvent, microwave, ultrasonic wave auxiliary extraction method, ultrasonic wave complex enzyme extraction method and the like. The optimal extraction conditions for ultrasonic-assisted extraction of the Korean pine scale polyphenol are preferably that the ultrasonic time is 52min, the ultrasonic temperature is 53 ℃, and the ultrasonic power is 300W. The pine polyphenol in the pine bark of the cinnamomum camphora is extracted, and the influence of an organic solvent extraction method, an ultrasonic auxiliary extraction method and an ultrasonic-complex enzyme method on the extraction effect of the pine polyphenol is compared. However, the sound wave-complex enzyme method of the methods has influence on the extraction effect of the pine polyphenol. However, these methods have disadvantages such as large solvent consumption, long extraction time and low extraction yield.
Therefore, the extraction method and the application of the Korean pine needle polyphenol compound are provided for solving the problems.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The invention is provided in view of the problems in the existing extraction method of the polyphenol compounds in the pine needles of the Korean pine.
Therefore, the invention aims to provide an extraction method of Korean pine needle polyphenol compounds and application thereof, which can realize high extraction rate, short extraction time, small solvent consumption and small tool wear.
To solve the above technical problem, according to an aspect of the present invention, the present invention provides the following technical solutions:
a method for extracting polyphenol compounds from pine needles of Korean pine and application thereof comprise the following steps:
the method comprises the following steps: firstly, preprocessing pine needles of the Korean pine, drying, cleaning and sterilizing the pine needles of the Korean pine, and then putting the sterilized pine needles of the Korean pine into a constant-temperature drying box at 40 ℃ until the pine needles of the Korean pine are completely dried;
step two: putting the treated pine needles of the Korean pine into a high-speed crusher for crushing, putting the completely dried pine needles of the Korean pine into the high-speed crusher for electric crushing, and then sieving by a sieve of 60 meshes for screening;
step three: taking a proper amount of pine needle powder, carrying out high shear extraction according to a certain material-liquid ratio, carrying out centrifugal filtration to obtain a pine needle polyphenol extracting solution, selecting pine needle powder and an ethanol solution with the purity of 60% according to the ratio of 1:10, adding the pine needle powder and the ethanol solution into a container, extracting by a high-shear emulsifying and dispersing machine at the temperature of 40 ℃, wherein the shearing time is 150s, and the rotating speed of the high-shear emulsifying and dispersing machine is 18000r/min to obtain the pine needle polyphenol extracting solution;
step four: recovering ionic liquid, purifying pine needle polyphenol of the Korean pine, and concentrating a pine needle polyphenol extracting solution to obtain paste containing the ionic liquid; dissolving with anhydrous ethanol, dripping petroleum ether, completely separating out ionic liquid, centrifuging, and concentrating supernatant to obtain paste without ionic liquid; dissolving with distilled water to obtain folium Pini polyphenol water solution, adjusting pH to 6, adding distilled water, adding into macroporous adsorbent resin material, stirring, standing to completely adsorb polyphenol on resin, vacuum filtering, eluting resin with ethanol, vacuum filtering, and concentrating the eluate to obtain folium Pini polyphenol compound.
As a preferable scheme of the extraction method and the application of the Korean pine needle polyphenol compound, the method comprises the following steps: the centrifuge is TGL-16C desk type centrifuge, the high speed pulverizer is FW177 Chinese herbal medicine pulverizer, the high shear dispersion emulsifier is FA25, and the constant temperature drying oven is DHG-9030A electric heating constant temperature air blast dryer.
As a preferable scheme of the extraction method and the application of the Korean pine needle polyphenol compound, the method comprises the following steps: the Korean pine needle polyphenol compound is prepared into a natural active additive for increasing fragrance, and the mass concentration of the Korean pine needle polyphenol compound in the natural active additive is 100-200 mg/mL.
Compared with the prior art, the invention has the beneficial effects that: through the extraction method of the Korean pine needle polyphenol compounds and the application setting thereof, the structural design is reasonable, the response surface optimization design experiment is applied to further optimize the polyphenol extraction process of the Korean pine needles by a high shear technology on the basis of a single-factor and steepest climbing experiment, the optimal extraction condition of the Korean pine needle polyphenol is determined, the extraction rate is high, the extraction time is short, the solvent consumption is small, and the tool abrasion is small.
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In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the present invention will be described in detail with reference to the accompanying drawings and detailed embodiments, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise. Wherein:
FIG. 1 is a schematic view of the structure of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described herein, and it will be apparent to those of ordinary skill in the art that the present invention may be practiced without departing from the spirit and scope of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Example 1
A method for extracting polyphenol compounds from pine needles of Korean pine and an application thereof are disclosed, which comprise the following steps:
the method comprises the following steps: firstly, preprocessing pine needles of the Korean pine, drying, cleaning and sterilizing the pine needles of the Korean pine, and then putting the sterilized pine needles of the Korean pine into a constant-temperature drying box at 40 ℃ until the pine needles of the Korean pine are completely dried;
step two: putting the treated pine needles of the Korean pine into a high-speed crusher for crushing, putting the completely dried pine needles of the Korean pine into the high-speed crusher for electric crushing, and then sieving by a sieve of 60 meshes for screening;
step three: taking a proper amount of pine needle powder, carrying out high shear extraction according to a certain material-liquid ratio, carrying out centrifugal filtration to obtain a pine needle polyphenol extracting solution, selecting pine needle powder and an ethanol solution with the purity of 60% according to the ratio of 1:10, adding the pine needle powder and the ethanol solution into a container, extracting by a high-shear emulsifying and dispersing machine at the temperature of 40 ℃, wherein the shearing time is 150s, and the rotating speed of the high-shear emulsifying and dispersing machine is 18000r/min to obtain the pine needle polyphenol extracting solution;
step four: recovering ionic liquid, purifying pine needle polyphenol of the Korean pine, and concentrating a pine needle polyphenol extracting solution to obtain paste containing the ionic liquid; dissolving with anhydrous ethanol, dripping petroleum ether, completely separating out ionic liquid, centrifuging, and concentrating supernatant to obtain paste without ionic liquid; dissolving with distilled water to obtain folium Pini polyphenol water solution, adjusting pH to 6, adding distilled water, adding into macroporous adsorbent resin material, stirring, standing to completely adsorb polyphenol on resin, vacuum filtering, eluting resin with ethanol, vacuum filtering, and concentrating the eluate to obtain folium Pini polyphenol compound.
Specifically, the centrifuge is TGL-16C desk type centrifuge, the high speed pulverizer is FW177 Chinese herbal medicine pulverizer, the high shear dispersion emulsifier is FA25, and the constant temperature drying oven is DHG-9030A electric heating constant temperature air blast dryer.
Specifically, the Korean pine needle polyphenol compound is prepared into a natural active additive for increasing fragrance, and the mass concentration of the Korean pine needle polyphenol compound in the natural active additive is 100-200 mg/mL.
While the invention has been described above with reference to an embodiment, various modifications may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. In particular, the various features of the disclosed embodiments of the invention may be used in any combination, provided that no structural conflict exists, and the combinations are not exhaustively described in this specification merely for the sake of brevity and resource conservation. Therefore, it is intended that the invention not be limited to the particular embodiments disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (3)
1. A method for extracting polyphenol compounds from pine needles of Korean pine is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: firstly, preprocessing pine needles of the Korean pine, drying, cleaning and sterilizing the pine needles of the Korean pine, and then putting the sterilized pine needles of the Korean pine into a constant-temperature drying box at 40 ℃ until the pine needles of the Korean pine are completely dried;
step two: putting the treated pine needles of the Korean pine into a high-speed crusher for crushing, putting the completely dried pine needles of the Korean pine into the high-speed crusher for electric crushing, and then sieving by a sieve of 60 meshes for screening;
step three: taking a proper amount of pine needle powder, carrying out high shear extraction according to a certain material-liquid ratio, carrying out centrifugal filtration to obtain a pine needle polyphenol extracting solution, selecting pine needle powder and an ethanol solution with the purity of 60% according to the ratio of 1:10, adding the pine needle powder and the ethanol solution into a container, extracting by a high-shear emulsifying and dispersing machine at the temperature of 40 ℃, wherein the shearing time is 150s, and the rotating speed of the high-shear emulsifying and dispersing machine is 18000r/min to obtain the pine needle polyphenol extracting solution;
step four: recovering ionic liquid, purifying pine needle polyphenol of the Korean pine, and concentrating a pine needle polyphenol extracting solution to obtain paste containing the ionic liquid; dissolving with anhydrous ethanol, dripping petroleum ether, completely separating out ionic liquid, centrifuging, and concentrating supernatant to obtain paste without ionic liquid; dissolving with distilled water to obtain folium Pini polyphenol water solution, adjusting pH to 6, adding distilled water, adding into macroporous adsorbent resin material, stirring, standing to completely adsorb polyphenol on resin, vacuum filtering, eluting resin with ethanol, vacuum filtering, and concentrating the eluate to obtain folium Pini polyphenol compound.
2. The extraction method of the polyphenolic compounds from the Korean pine needles as claimed in claim 1, wherein the polyphenolic compounds comprise the following components in percentage by weight: the centrifuge is TGL-16C desk type centrifuge, the high speed pulverizer is FW177 Chinese herbal medicine pulverizer, the high shear dispersion emulsifier is FA25, and the constant temperature drying oven is DHG-9030A electric heating constant temperature air blast dryer.
3. The application of the Korean pine needle polyphenol compounds obtained by the extraction method of the Korean pine needle polyphenol compounds according to any one of claims 1-2, is characterized in that: the Korean pine needle polyphenol compound is prepared into a natural active additive for increasing fragrance, and the mass concentration of the Korean pine needle polyphenol compound in the natural active additive is 100-200 mg/mL.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113786420A (en) * | 2021-09-10 | 2021-12-14 | 苏州科技大学 | Process for simultaneously extracting polysaccharides and polyphenol from pine needles in grading manner and application of polysaccharide and polyphenol |
| CN115403634A (en) * | 2022-08-30 | 2022-11-29 | 集美大学 | Method for extracting polyphenol from agar industrial waste liquid by using ionic liquid and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108272831A (en) * | 2018-03-15 | 2018-07-13 | 枣庄学院 | The extracting method of Korean Needle polyphenol compound and its application |
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- 2021-06-29 CN CN202110728875.3A patent/CN113318134A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108272831A (en) * | 2018-03-15 | 2018-07-13 | 枣庄学院 | The extracting method of Korean Needle polyphenol compound and its application |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113786420A (en) * | 2021-09-10 | 2021-12-14 | 苏州科技大学 | Process for simultaneously extracting polysaccharides and polyphenol from pine needles in grading manner and application of polysaccharide and polyphenol |
| CN113786420B (en) * | 2021-09-10 | 2022-05-13 | 苏州科技大学 | Process for simultaneously extracting polysaccharides and polyphenol from pine needles in grading manner and application of polysaccharide and polyphenol |
| CN115403634A (en) * | 2022-08-30 | 2022-11-29 | 集美大学 | Method for extracting polyphenol from agar industrial waste liquid by using ionic liquid and application thereof |
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