CN101804077B - Pretreatment method of propolis effective component raw material by supercritical extraction - Google Patents
Pretreatment method of propolis effective component raw material by supercritical extraction Download PDFInfo
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- CN101804077B CN101804077B CN2009100583428A CN200910058342A CN101804077B CN 101804077 B CN101804077 B CN 101804077B CN 2009100583428 A CN2009100583428 A CN 2009100583428A CN 200910058342 A CN200910058342 A CN 200910058342A CN 101804077 B CN101804077 B CN 101804077B
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- propolis
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- effective component
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Abstract
The invention belongs to the chemical technology field of natural product, particularly relating to a pretreatment method of a propolis effective component raw material by supercritical extraction. The invention is realized by the following mode: freezing raw material rough propolis at the temperature of -18 DEG C for 6-24 hours; after being smashed, processing with 5-20 times of pretreatment solution; after standing, separating impurities on the upper layer, filtering other parts, and carrying out supercritical CO2 extraction after filter residues are dried. The pretreatment solution is one of the solutions or the mixture of a plurality of solutions of ethanol, glycol and water. The propolis raw material processed by the invention dose not block, does not adhere to extraction kettle wall and is easy to clean in the supercritical CO2 extraction process. The invention has simple operation and cheap solution, does not generate any side effect on products, reduces equipment cleaning time, energy consumption cost and the like and improves extraction efficiency.
Description
Technical field
The invention belongs to the natural product chemistry technical field, be specifically related to a kind of pretreatment method of propolis effective component raw material by supercritical extraction.
Background technology
The propolis armaticity jelly that to be Apis process from the secretions of sneaking into bodies of gland such as its mandibular gland after the tissues such as newborn branch, leaf, bud or bark of plant collect resin-like secretions and Cera Flava etc. contains the mass efficient composition similar with the collagen plant.Because it is propolis has effects such as antiviral, blood fat reducing, antioxidation, raising immunity, more and more to its extraction of effective components research in recent years.Supercritical CO
2The method of bee glue extracting effective ingredient obtains people's attention.But the thick propolis of pulverizing is soft in room temperature matter, toughness, directly puts it into and carries out supercritical extraction in the extraction kettle, is easy to lump and be bonded on the extraction kettle wall, is unfavorable for the cleaning of further extraction and extraction kettle, has a strong impact on extraction efficiency.
Summary of the invention
The objective of the invention is: overcome raw material serious sticking glutinous shortcoming in still in the effective bee glue components supercritical extraction process, a kind of pretreatment of raw material technology and technology of effective bee glue components supercritical extraction is provided.
The present invention realizes in the following manner:
The thick propolis of raw material was pulverized after under-18 ℃ freezing 6～24 hours again, and the preprocessing solution that adds 5-20 times of volume carries out stir process, after leaving standstill, upper strata impurity is told, and remainder filters, and filtering residue carries out supercritical CO again after drying
2Extraction.Preprocessing solution is pure ethanol, ethylene glycol, water or several solns mixture, alcoholic solution as 15% even pure water, and perhaps 15% ethylene glycol solution even pure water, preprocessing solution is-10 ℃-15 ℃ coolings more than 1 hour down.
The propolis raw material of handling through the present invention is at supercritical CO
2Do not lump in the extraction process, do not glue the extraction kettle wall, be easy to clean.That the present invention has is simple to operate, solution is cheap, can not produce any side effect, reduce expenses such as equipment cleaning time and energy consumption product, improves extraction efficiency.
The specific embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1
Thick propolis was pulverized after under-18 ℃ freezing 6～24 hours, added 10 times pretreatment fluid, stirred five minutes, left standstill one hour, upper strata impurity is told after-filtration lower floor sample, filtering residue carries out supercritical CO again after drying
2Extraction.Pretreatment fluid is 8% alcoholic solution.
Embodiment 2
Thick propolis is pulverized after freezing, added 14 times pretreatment fluid, stirred five minutes, left standstill one hour, upper strata impurity is told after-filtration lower floor sample, filtering residue carries out supercritical CO again after drying
2Extraction.Pretreatment fluid is 10% ethylene glycol solution.
Embodiment 3
Thick propolis is pulverized after freezing, added 12 times pretreatment fluid, stirred five minutes, left standstill one hour, upper strata impurity is told after-filtration lower floor sample, filtering residue carries out supercritical CO again after drying
2Extraction.Pretreatment fluid is 15% ethylene glycol solution.
Embodiment 4
Thick propolis is pulverized after freezing, added 20 times pretreatment fluid, stirred five minutes, left standstill one hour, upper strata impurity is told after-filtration lower floor sample, filtering residue carries out supercritical CO again after drying
2Extraction.Pretreatment fluid is 15% alcoholic solution.
Embodiment 5
Thick propolis is pulverized after freezing, added 10 times pretreatment fluid, stirred five minutes, left standstill one hour, upper strata impurity is told after-filtration lower floor sample, filtering residue carries out supercritical CO again after drying
2Extraction.Pretreatment fluid is 5% alcoholic solution.
Claims (2)
1. pretreatment method of propolis effective component raw material by supercritical extraction; It is characterized in that: freezing 6～24 hours thick propolis of raw material under-18 ℃; Pulverize the back and handle, after leaving standstill, upper strata impurity is told with 5-20 preprocessing solution doubly; Remainder filters, and filtering residue carries out supercritical CO again after drying
2Extraction; Preprocessing solution is the aqueous solution of alcoholic acid aqueous solution or ethylene glycol.
2. pretreatment method of propolis effective component raw material by supercritical extraction according to claim 1 is characterized in that: described preprocessing solution-10-15 ℃ down cooling re-use after more than 1 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100583428A CN101804077B (en) | 2009-02-17 | 2009-02-17 | Pretreatment method of propolis effective component raw material by supercritical extraction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100583428A CN101804077B (en) | 2009-02-17 | 2009-02-17 | Pretreatment method of propolis effective component raw material by supercritical extraction |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101804077A CN101804077A (en) | 2010-08-18 |
| CN101804077B true CN101804077B (en) | 2012-06-27 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2009100583428A Expired - Fee Related CN101804077B (en) | 2009-02-17 | 2009-02-17 | Pretreatment method of propolis effective component raw material by supercritical extraction |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102188455A (en) * | 2011-05-13 | 2011-09-21 | 扬州三邦生物工程有限公司 | Method for extracting totipotent propolis |
| CN102441010B (en) * | 2011-12-12 | 2013-04-03 | 南京中科集团股份有限公司 | Preparation method of deleaded refined propolis |
| CN114271462B (en) * | 2021-12-28 | 2024-02-20 | 南昌蜂芝缘健康科技有限公司 | Preparation method of supercritical carbon dioxide extracted propolis |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1493304A (en) * | 2003-07-25 | 2004-05-05 | 吴晓闻 | Method of extracting mixed propolis using supercritical fluid separation |
| CN100348203C (en) * | 2004-04-30 | 2007-11-14 | 无锡尚宝生物科技有限公司 | Hypercritical soluble propolis prescription and its preparing method |
| CN101244086A (en) * | 2008-02-01 | 2008-08-20 | 南昌大学 | Method for improving supercritical CO2 abstraction propolis obtaining ratio |
-
2009
- 2009-02-17 CN CN2009100583428A patent/CN101804077B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1493304A (en) * | 2003-07-25 | 2004-05-05 | 吴晓闻 | Method of extracting mixed propolis using supercritical fluid separation |
| CN100348203C (en) * | 2004-04-30 | 2007-11-14 | 无锡尚宝生物科技有限公司 | Hypercritical soluble propolis prescription and its preparing method |
| CN101244086A (en) * | 2008-02-01 | 2008-08-20 | 南昌大学 | Method for improving supercritical CO2 abstraction propolis obtaining ratio |
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| CN101804077A (en) | 2010-08-18 |
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