CN114748512A - Method for rapidly extracting propolis - Google Patents

Method for rapidly extracting propolis Download PDF

Info

Publication number
CN114748512A
CN114748512A CN202210354507.1A CN202210354507A CN114748512A CN 114748512 A CN114748512 A CN 114748512A CN 202210354507 A CN202210354507 A CN 202210354507A CN 114748512 A CN114748512 A CN 114748512A
Authority
CN
China
Prior art keywords
propolis
ethanol solution
purified
extraction
extracting
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202210354507.1A
Other languages
Chinese (zh)
Inventor
张勇
王海燕
王莉
范国纲
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangsu Feng Ao Biological Technology Co ltd
Original Assignee
Jiangsu Feng Ao Biological Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jiangsu Feng Ao Biological Technology Co ltd filed Critical Jiangsu Feng Ao Biological Technology Co ltd
Priority to CN202210354507.1A priority Critical patent/CN114748512A/en
Publication of CN114748512A publication Critical patent/CN114748512A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K35/00Medicinal preparations containing materials or reaction products thereof with undetermined constitution
    • A61K35/56Materials from animals other than mammals
    • A61K35/63Arthropods
    • A61K35/64Insects, e.g. bees, wasps or fleas
    • A61K35/644Beeswax; Propolis; Royal jelly; Honey
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0261Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
    • B01D11/0265Applying ultrasound
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0288Applications, solvents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/04Solvent extraction of solutions which are liquid

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Insects & Arthropods (AREA)
  • Physics & Mathematics (AREA)
  • Acoustics & Sound (AREA)
  • Mechanical Engineering (AREA)
  • Animal Husbandry (AREA)
  • Zoology (AREA)
  • Engineering & Computer Science (AREA)
  • Medicinal Chemistry (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Jellies, Jams, And Syrups (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

The invention discloses a rapid extraction method of propolis, which relates to the field of propolis processing and comprises the following steps of S10, percolating and extracting the original propolis at room temperature, and storing primary percolate; step S20, stirring and cooling the primary percolate, standing for layering, taking a middle layer of the filtrate, concentrating and drying to form purified propolis; step S30, freezing the purified propolis at low temperature, pulverizing and sieving; step S40, dissolving the purified propolis in ethanol solution, and extracting by ultrasonic oscillation. Purifying the original propolis by a percolation method to form purified propolis, then carrying out secondary extraction on the basis of the purified propolis, wherein impurities and interferents in the propolis extracted by the percolation method are fully removed, and the propolis can be fully dissolved after being dissolved in an alkaline ethanol solution, so that the extraction is finished; compared with the existing propolis extraction method, the extraction method has good effect and high efficiency.

Description

Method for rapidly extracting propolis
Technical Field
The invention relates to the field of propolis processing, in particular to a rapid extraction method of propolis.
Background
Propolis is a viscous substance formed by mixing secretions such as branches, leaf buds and callus of bees collected from plants, secretions such as jawbone and wax gland, and a small amount of pollen, is a very rare natural resource and is known as purple gold. In recent years, researches of scholars at home and abroad show that the propolis has important physiological effects of treating cardiovascular diseases, diabetes, skin diseases, gastrointestinal diseases, resisting cancers, enhancing immunity, resisting bacteria and diminishing inflammation and the like, is a hot spot in the field of health food research at present, has complex chemical components and contains phenol, acid, alcohol, ester, phenol, ether, alkene and various trace elements. The total flavone is one of the main active components of propolis for enhancing body immunity, softening blood vessel, reducing blood lipid and scavenging free radicals.
The modern propolis industrialized extraction method mainly comprises ethanol extraction and ultrasonic extraction, and most of components extracted by the two extraction methods are flavonoid compounds. The ultrasonic extraction mode is gradually reduced along with the equipment cost, is easier to scale and industrialize, and is gradually popularized.
However, in the existing ultrasonic extraction method, because the original propolis is not pretreated, the content of flavonoid compounds in the extract is low, the content of impurities similar to lead is high, and the extraction effect is poor.
Disclosure of Invention
In order to realize the purpose, the technical scheme adopted by the invention is as follows: a rapid extraction method of propolis comprises step S10, percolating and extracting raw propolis at room temperature, and storing primary percolate; step S20, stirring and cooling the primary percolate, standing for layering, taking a middle layer of filtrate, concentrating and drying to form purified propolis; step S30, freezing the purified propolis at low temperature, pulverizing and sieving; step S40, dissolving the purified propolis in ethanol solution, and extracting by ultrasonic oscillation.
Further, step S30 is included after step S20, wherein the propolis ethanol solution is subjected to a filtration treatment to remove insoluble substances therein.
Further, in step S30, the propolis ethanol solution is filtered with a 200 mesh sieve.
Further, in step S30, the raw propolis is frozen in an environment of-20 to-40 degrees for 24 to 48 hours.
Further, in step S40, the method further includes step S41 of preparing an ethanol solution with a mass concentration ratio of 75% to 90%; step S42, heating the configured ethanol solution by using heating equipment, and keeping the constant temperature of 80 ℃; in step S43, a sodium hydroxide solution is added to the ethanol solution to adjust the pH of the ethanol solution to between 11 and 13.
Further, in step S40, when the original propolis piece is dissolved and ultrasonically vibrated, the original propolis piece is soaked in the ethanol solution for 15 to 20 minutes.
Further, in step S40, the frequency of the ultrasonic wave is between 25khz and 40khz, and the extraction time is 30 minutes.
Further, step S10 includes step S11 of percolating the vibrated mixed solution through a percolating device, and collecting a percolate; step S12, vacuum decompression concentration is carried out on the collected percolate, the extract is transferred into a settling tank, and stirring and cooling are carried out through stirring equipment; and step S13, standing and layering the cooling liquid, removing beeswax on the upper layer of the precipitation tank, concentrating the solution on the middle layer for later use, and discharging extract on the bottom layer to form purified propolis.
Further, step S13 is followed by step S14 of drying the extract at 105 degrees to constant weight by vacuum microwave drying.
Further, in step S13, the drying time was 30 minutes.
Compared with the prior art, the invention has the following beneficial effects:
firstly, purifying the original propolis by a percolation method to form purified propolis, then carrying out secondary extraction on the basis of the purified propolis, wherein impurities and interferents in the propolis extracted by the percolation method are fully removed, and the propolis can be fully dissolved after being dissolved in an alkaline ethanol solution, so that the extraction is finished; compared with the existing propolis extraction method, the extraction method has good effect and high efficiency.
Drawings
Fig. 1 is a schematic diagram of the working flow of propolis extraction in the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present.
Examples
As shown in fig. 1, the rapid extraction method of propolis in this embodiment includes the following steps,
step S10, percolating and extracting the original propolis at room temperature, and storing primary percolate;
step S20, stirring and cooling the primary percolate, standing for layering, taking a middle layer of the filtrate, concentrating and drying to form purified propolis;
Step S30, freezing the purified propolis at low temperature, pulverizing and sieving;
step S40, dissolving the purified propolis in ethanol solution, and extracting by ultrasonic oscillation.
The modern propolis industrialized extraction method mainly comprises ethanol extraction and ultrasonic extraction, and most of components extracted by the two extraction methods are flavonoid compounds. The ultrasonic extraction mode is gradually reduced along with the equipment cost, is easier to scale and industrialize, and is gradually popularized.
However, in the existing ultrasonic extraction method, because the original propolis is not pretreated, the content of flavonoid compounds in the extract is low, the content of impurities similar to lead is high, and the extraction effect is poor.
In the scheme, the original propolis is purified by a percolation method to form purified propolis, and then secondary extraction is carried out on the basis of the purified propolis, because impurities and interferents in the propolis extracted by the percolation method are fully removed, the propolis can be fully dissolved after being dissolved in an alkaline ethanol solution, so that the extraction is finished; compared with the existing propolis extraction method, although the propolis extraction method is complex, the extraction effect is better and the efficiency is high.
Propolis is insoluble in water, slightly soluble in turpentine, partially soluble in ethanol, and soluble in 95% ethanol to give transparent chestnut color and granular precipitate. It is very soluble in ether, acetone and chloroform, and also in sodium hydroxide. Among the chemical substances, substances except ethanol are not common substances, and countries have strict regulations and limits on the application of the substances; the antibacterial property of propolis liquid extracted by ethanol is the strongest in all propolis extracting liquid at present. Thus, to date, ethanol has been the primary extraction solvent.
Referring to fig. 1, after step S20, step S30 is further included, wherein the propolis ethanol solution is subjected to a filtration treatment to remove insoluble substances therein;
particularly, can accomplish through centrifuge or the reciprocating sieve of aperture and filter, if the screen cloth that adopts in time filters, can select for use 200 meshes sieve, during the use, through getting rid of the insoluble substance in the propolis ethanol solution, firstly can prevent the pollution and the interference of insoluble substance to the propolis extract product, secondly also be convenient for retrieve the reuse to former propolis insoluble substance to avoid the waste on the material.
In step S30, the raw propolis is frozen in an environment of-20 to-40 degrees for 24h to 48h, preferably 36 h.
When in use, the original propolis can be quickly embrittled by cooling at low temperature, and the original propolis blocks can be frozen inside and outside after 36h of freezing.
Referring to fig. 1, in step S40, further includes the following,
step S41, preparing an ethanol solution with the mass concentration ratio of 75% to 90%; preferably, 75% ethanol is used as the extraction solvent of propolis;
step S42, heating the configured ethanol solution by using heating equipment, and keeping the constant temperature of 80 ℃; or carrying out water bath treatment at 80 ℃;
step S53, adding sodium hydroxide solution into the ethanol solution to adjust the pH value of the ethanol solution to between 11 and 13, preferably 12.5;
when the propolis tablet is used, the ethanol solution is adjusted to be alkaline and is subjected to constant-temperature water bath, and the organic extract in the original propolis block is more easily dissolved in the alkaline organic solution, so that the difficulty of subsequent extraction is reduced.
In step S40, when the original propolis block is subjected to ultrasonic wave vibration for dissolution, the original propolis block is soaked in an ethanol solution for 15 to 20 minutes; so as to dissolve the original propolis blocks as much as possible.
Furthermore, when the frequency of the ultrasonic wave is selected, the frequency can be selected from 25khz to 40khz, such as 25khz, 28khz and 40khz, and the ultrasonic wave is selected to vibrate the ethanol solution in which the original propolis blocks are dissolved, so that organic matters in the propolis can be crushed, and chemical bonds in the propolis can be broken to increase the dissolution of the propolis; further, the duration of ultrasonic extraction is about 30 minutes.
Referring to fig. 1, the following is included in step S10;
step S11, percolating and extracting the vibrated mixed solution through percolating equipment, and collecting percolate;
step S12, vacuum decompression concentration is carried out on the collected percolate, the extract is transferred into a settling tank, and stirring and cooling are carried out through stirring equipment;
and step S13, standing and layering the cooling liquid, removing beeswax on the upper layer of the precipitation tank, concentrating the solution on the middle layer for later use, and discharging extract on the bottom layer to form purified propolis.
After step S13, step S14 is included, wherein the extract is dried at 105 degrees by vacuum microwave drying to constant weight for approximately 30 minutes.
When the method is used, the primary extraction is carried out on the propolis by adopting a percolation method, and the purified propolis is primarily formed, so that impurities and insoluble substances in the propolis are reduced as much as possible during secondary purification, the purity of the propolis extract can be improved, and the difficulty of secondary purification can be reduced.
It is noted that, in this document, relational terms such as first and second, and the like, if any, are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
The technical problems to be solved are still consistent with the present invention and should be included in the scope of the present invention.

Claims (10)

1. A rapid extraction method of propolis is characterized by comprising the following steps of S10, percolating and extracting raw propolis at room temperature, and storing primary percolate; step S20, stirring and cooling the primary percolate, standing for layering, taking a middle layer of filtrate, concentrating and drying to form purified propolis; step S30, freezing the purified propolis at low temperature, pulverizing and sieving; step S40, dissolving the purified propolis in ethanol solution, and extracting by ultrasonic oscillation.
2. The method as claimed in claim 1, further comprising a step S30 after the step S20, wherein the ethanol solution of propolis is filtered to remove insoluble substances.
3. The method for rapidly extracting propolis according to claim 2, wherein in step S30, the propolis ethanol solution is filtered by a 200-mesh sieve.
4. The method for rapidly extracting propolis according to claim 3, wherein in step S30, the raw propolis is frozen in an environment of-20 to-40 degrees for a period of time ranging from 24h to 48 h.
5. The method for rapidly extracting propolis according to claim 1, wherein in step S40, the method further comprises step S41 of preparing an ethanol solution with a mass concentration ratio of 75% to 90%; step S42, heating the configured ethanol solution by using heating equipment, and keeping the constant temperature of 80 ℃; in step S43, a sodium hydroxide solution is added to the ethanol solution to adjust the pH of the ethanol solution to between 11 and 13.
6. The method as claimed in claim 5, wherein the step S40 comprises immersing the propolis block in the ethanol solution for 15-20 minutes while subjecting the propolis block to ultrasonic wave for dissolution.
7. The method as claimed in claim 6, wherein in step S40, the frequency of the ultrasonic wave is between 25khz and 40khz, and the extraction time is 30 minutes.
8. The method for rapidly extracting propolis according to claim 1, wherein the step S10 includes a step S11 of percolating the mixed solution after shaking through a percolating device, and collecting a percolate; step S12, vacuum decompression concentration is carried out on the collected percolate, the extract is transferred into a settling tank, and stirring and cooling are carried out through stirring equipment; and step S13, standing and layering the cooling liquid, removing beeswax on the upper layer of the precipitation tank, concentrating the solution on the middle layer for later use, and discharging extract on the bottom layer to form purified propolis.
9. The method as claimed in claim 8, further comprising a step S14 after the step S13, drying the extract to constant weight at 105 degrees by vacuum microwave drying.
10. The method for rapidly extracting propolis according to claim 8, wherein in step S13, the drying time is 30 minutes.
CN202210354507.1A 2022-04-06 2022-04-06 Method for rapidly extracting propolis Pending CN114748512A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210354507.1A CN114748512A (en) 2022-04-06 2022-04-06 Method for rapidly extracting propolis

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210354507.1A CN114748512A (en) 2022-04-06 2022-04-06 Method for rapidly extracting propolis

Publications (1)

Publication Number Publication Date
CN114748512A true CN114748512A (en) 2022-07-15

Family

ID=82329389

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210354507.1A Pending CN114748512A (en) 2022-04-06 2022-04-06 Method for rapidly extracting propolis

Country Status (1)

Country Link
CN (1) CN114748512A (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060040226A (en) * 2004-11-04 2006-05-10 한국식품연구원 A method for preparing water-soluble propolis extract and powder
CN102283866A (en) * 2011-06-16 2011-12-21 张大辉 Method for extracting propolis containing high-purity flavones
CN106074617A (en) * 2016-08-24 2016-11-09 深圳市荣格保健品有限公司 A kind of propolis extract and extraction process thereof
CN110538128A (en) * 2019-09-24 2019-12-06 江苏蜂奥生物科技有限公司 Method for recovering and extracting propolis effective components from beeswax
CN110638837A (en) * 2019-10-31 2020-01-03 广东国源国药制药有限公司 Propolis extract and preparation method and application thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060040226A (en) * 2004-11-04 2006-05-10 한국식품연구원 A method for preparing water-soluble propolis extract and powder
CN102283866A (en) * 2011-06-16 2011-12-21 张大辉 Method for extracting propolis containing high-purity flavones
CN106074617A (en) * 2016-08-24 2016-11-09 深圳市荣格保健品有限公司 A kind of propolis extract and extraction process thereof
CN110538128A (en) * 2019-09-24 2019-12-06 江苏蜂奥生物科技有限公司 Method for recovering and extracting propolis effective components from beeswax
CN110638837A (en) * 2019-10-31 2020-01-03 广东国源国药制药有限公司 Propolis extract and preparation method and application thereof

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
周多刚等: "蜂胶制成品中总黄酮含量的测定", 《安徽机电学院学报》, vol. 15, no. 1, pages 67 *
李朝强: "蜂胶提取工艺探讨", 《临床合理用药杂志》, vol. 6, no. 6, pages 88 *
林贤统等: "不同溶剂提取蜂胶的得率及其提取物的抗氧化性", 《蜜蜂杂志》, no. 7 *
潘秋月;李英华;周晓红;杨凤杰;: "蜂胶黄酮的超声波提取工艺研究", 蜜蜂杂志, no. 12 *
郭相华, 王福志, 许磊, 姚崇舜: "蜂胶醇制剂的制备及临床应用", 辽宁药物与临床, no. 03 *

Similar Documents

Publication Publication Date Title
CN106361633B (en) It is a kind of using citrus peel residue as moisture saver mask of raw material and preparation method thereof
CN107266609B (en) Method for extracting pomegranate peel residue pectin by electrolytic water
CN101914170B (en) Preparation method for producing sodium heparin by using small sheep intestines
CN102212144B (en) Method for preparing pure polysaccharose from alfalfa hay
CN102746412A (en) Method for extracting momordica charantiap polysaccharide
CN113278088A (en) Sargassum fusiforme polysaccharide with obvious intestinal mucosa repair activity and preparation method and application thereof
RU2339395C1 (en) Method of pectin substances extraction from plant materials
CN106674370A (en) Bletilla striata gelatin and preparation method thereof
CN108203566A (en) The technique that a kind of alkaline process prepares pharmagel
CN114748512A (en) Method for rapidly extracting propolis
CN1342714A (en) Process for extracting heparin sodium by integrated biologic method
CN103483403A (en) Circulating extraction method for extracting and purifying hesperidin from orange residues
CN115322241B (en) Method for extracting tea saponin from oil tea meal
CN115820778B (en) Industrial production method of sea cucumber polypeptide rich in sea cucumber polysaccharide
CN105985430A (en) Low-temperature macromolecular collagen extracting method
CN112457431A (en) Production method of dry and wet raw material blended pectin
CN107903334B (en) Process for extracting green algae proteoglycan from fresh green algae
RU2373956C1 (en) Method of preparing polysaccharide complex of tillet blossom
CN110643052A (en) Method for extracting gutta-percha by treating eucommia ulmoides shells with sodium hydroxide/urea aqueous solution
CN104137996A (en) Holothurian internal organ processing method
CN114989320A (en) Method for extracting natural vegetable gum from basil seeds
CN1654670A (en) Preparation method of chondroitin sulfate
CN106977613B (en) Method for extracting artemisia desertorum polysaccharide from artemisia desertorum seeds
CN114588181A (en) Propolis extract and production process thereof
CN103341481A (en) Method and equipment for processing egg shell powder

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20220715