CN101579585A - Extraction and separation purifier capable of extracting chemical composition in plant corpus - Google Patents
Extraction and separation purifier capable of extracting chemical composition in plant corpus Download PDFInfo
- Publication number
- CN101579585A CN101579585A CNA2009101116659A CN200910111665A CN101579585A CN 101579585 A CN101579585 A CN 101579585A CN A2009101116659 A CNA2009101116659 A CN A2009101116659A CN 200910111665 A CN200910111665 A CN 200910111665A CN 101579585 A CN101579585 A CN 101579585A
- Authority
- CN
- China
- Prior art keywords
- solvent
- separation
- extraction
- chamber
- purification
- 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
Links
Images
Landscapes
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention relates to an extraction and separation purifier capable of respectively extracting, separating and purifying the organic chemical compositions in roots, caudex, leaves, fruits and cores of the plant. The extraction and separation purifier is characterized in that the extraction and separation purifier take the shape of a square tower and consists of the following devices that are arranged from bottom to top: a solvent supply system, a solvent reclaiming chamber, a separation and purification chamber, a composition extraction chamber and a condensation pipe for condensing solvent; control valves are respectively arranged among the solvent supply system, the solvent reclaiming chamber and the separation and purification chamber; the solvent supply system comprises a water bath heating pool, a solvent pool, a magnetic mixer, a water bath temperature-controlling circuit and a solvent stream conveying pipe; the connection position of the solvent reclaiming chamber and the solvent pool is provided with a solvent stream circular conveying side pipe and a solvent reclaiming control valve; and the composition extraction chamber and the separation and purification chamber are arranged in a drawer-type multi-layer structure which is uniformly closed space and has equivalent heights. The extraction and separation purifier is simple and easy, has convenient operation, leads the extraction, separation and purification process to be carried out in the same device, circularly uses the extraction solvent and has low cost for extraction, separation and purification.
Description
Technical field
The present invention relates to a kind of chemical composition that extracts in the plant and extract the separation and purification device, particularly relate to a kind ofly organic chemistry composition in plant roots, stem, Ye Jiguo, the nuclear can be extracted respectively, the extraction separation and purification device of separation and purifying.
Technical background
China's Forest Resources is abundant, and kind is numerous, especially has the One's name is legions such as fruit tree of medical value, and volume of production and marketing is big, is one of pillar industry of agricultural.At present, concentrate the cultivation of fruit and simple deep processing as making cream, wine etc. to the development and use of these fruit trees.Contain various chemical compositions in plant pulp, fruit stone, mesophyll, root and the bark, these active chemical componentses if can be extracted, deep development utilizes, be applied to other industry such as pharmaceuticals industry, health products, cosmetics and skincare product, food additives or the like, with increasing substantially the value of exploiting and utilizing of the pulp, fruit stone, mesophyll, rhizome, skin etc. of fruit tree, bring huge deep processing added value and economic benefit.
Contain multiple biologically active chemical composition in plant pulp, the mesophyll, have very high medicinal value.The loquat, olive, the mango that abound with Fujian are example, Compendium of Material Medica record: " loquat and stomach sending down abnormally ascending, clearing away summerheat poison." modern pharmacology studies show that it has anti-inflammatory, antitussive action, clinically is usually used in treating diseases such as acute and chronic respiratory tract.In recent years research also finds, has antitumor, antiviral, hypoglycemic, hepatic cholagogic, removing oxygen radical, strengthens effect such as body's immunity." function that Chinese pharmacopoeia record olive has heat-clearing, relieve sore throat, promotes the production of body fluid, detoxifies is used for the treatment of abscess of throat, cough, polydipsia, the poisoning of fish crab etc.Mango has that antiasthmatic-antitussive eliminates the phlegm, immunity, anti-inflammatory, analgesia, hepatic cholagogic, and anti peroxidation of lipid, antiviral, antitumor, antibioticly wait effect, central nervous system and disease of cardiovascular system also there are obvious curative effects.
Existing studies show that, the bioactive ingredients in common pulp, fruit stone, the mesophyll mainly are divided into volatile oil, triterpenes, sesquiterpenoids, flavonoids, Polyphenols, amino acid, glucosides class, and organic chemistry composition such as organic acid.To they effectively extract with separation and purification be research focus always.From the extraction separation process of having reported, common separation and purification process is: at first be to select for use certain solvent or mixed solvent to extract, then extract is concentrated and carry out purifying, the purification process of use comprises column chromatography, crystallisation, recrystallization method, and liquid chromatogram etc.Existing extracting method comprises: solvent extraction method, soxhlet extraction, ultrasonic extraction, activated carbon decolorizing method, macroporous absorbent resin separation method, microwave assisting method etc.
These major defects of extracting isolation and purification method are: (1) only extracts separation to wherein a kind of in the fruit tree leaves or an active component, does not have system to extract the multiple biological active component that contains in the fruit tree leaves, and resource is not fully used.(2) adopt earlier extract, the back concentrates, the pattern of separation and purification again, extracts with separation and purification and independently carries out, operation is loaded down with trivial details, consumption worker feed consumption consuming time, extraction cost height.This two big defective has seriously restricted the deep processing development of effective active biotic component.
Summary of the invention
In view of existing plant roots, stem, leaf, bioactive ingredients extracts purifying existing two big defectives in nuclear and the pulp, purpose of the present invention will design a kind of simple exactly, easy to operate, it is low to extract the separation and purification cost, can be systematically successively to pulp, fruit stone, mesophyll, the extraction separation and purification device that multiple main bioactive ingredients extracts respectively in root and the bark, realize that by this extraction separation and purification device main biological active component can systematically be extracted successively, resource is fully used, make simultaneously to extract and in same device, carry out with the separation and purification process, the extraction solvent can be recycled, the time and labour saving material-saving, significantly reduce and extract the separation and purification cost, promote pulp, fruit stone, mesophyll, the industrialization of the extraction separation and purification of biological active component in root and the bark.
The present invention is achieved through the following technical solutions: extracting the separation and purification device is square tower shape, by forming to the condenser pipe of going up down solvent feed system, solvent recovery chamber, separation and purification chamber, the composition extraction chamber that is provided with and being used for solvent condenses, solvent feed system, solvent recovery chamber, separation and purification are respectively equipped with control valve between the chamber.
Described solvent feed system comprises the water-bath heating bath that utilizes supplying heat source heating, is positioned at the upwards solvent vapo(u)r carrier pipe of conveying of water-bath heating bath solvent cell to be heated, the magnetic stirring apparatus that is used to control the solvent temperature balance, water-bath temperature-adjusting circuit and solvent vapo(u)r.
Described solvent recovery chamber is positioned on the solvent cell, and connecting portion therebetween is provided with the solvent vapo(u)r circulation and carries side pipe and solvent recovery control valve.
Setting is presented down in described composition extraction chamber and separation and purification chamber, and be in the unified airtight space, this space segmentation becomes contour drawer type sandwich construction, every drawer layer can insert a drawer, the drawer panel medial surface is provided with sealed film, the base plate of drawer is evenly distributed with fine and closely woven mesh, can and extract the difference adjustment composition extraction chamber of composition and the drawer number of separation and purification chamber according to raw material in the use, the composition extraction chamber is used to hold the plant raw material, and the drawer of separation and purification chamber is used to hold extraction separation and purification post.
Post lower end in the described extraction separation and purification post is equipped with Sha Xin, is equipped with other solid state powder separation and purification agent such as an amount of silica gel or aluminium oxide on the Sha Xin.
The described condenser pipe that is used for solvent condenses is conventional water-cooled condenser pipe.
During use, inject required boiling point in the solvent cell of solvent feed system and be lower than 100 ℃ solvent, in the drawer of composition extraction chamber, place powdered vegetable object raw material through pretreated purifying to be separated, in the drawer of separation and purification chamber, place and extract the separation and purification agent.Utilize supplying heat source such as high-temperature steam that the water-bath heating bath is heated, heating-up temperature is no more than 120 ℃, starts magnetic stirring apparatus, the water-bath temperature-adjusting circuit of solvent cell inner control solvent temperature balance simultaneously.When being heated, solvent reaches boiling point and when evaporating, solvent vapo(u)r upwards carries and enters the composition extraction chamber by the solvent vapo(u)r carrier pipe, this moment, a part of solvent gas fell back in the plant raw material through the water-cooled condensing tube condensation that is arranged at the top, a part directly is subjected to the effect of microtherm body raw material also to be condensed in the plant raw material simultaneously, the plant raw material that formation is extracted is fully immersed in the solvent, solvent extracts the bioactive ingredients in the plant raw material, extraction artifact active component permeates downwards together with solvent and process separation and purification agent, by control valve, further splash in the solvent recovery chamber.
By being arranged at the detection mouth of bottom, solvent recovery chamber, collection is carried out composition detection by the solvent that drips in the separation and purification post, composition as twice collection in front and back is identical, the control valve of then opening the collection container lower end splashes in the solvent cell solvent, enters the cycling extraction process by the solvent vapour carrier pipe again after solvent is heated.As composition is different before and after detecting in the collection container, then changes a new heating container and collects new component.
Extraction separation and purification device of the present invention can also adopt electrically heated mode that the water-bath heating bath is heated, and electrical heating power can adjust accordingly according to different solvents.
Description of drawings
Fig. 1 is the longitudinal profile schematic diagram that can extract the extraction separation and purification device of bioactive ingredients in the plant raw material.
Fig. 2 is the contour drawer schematic diagram that uses in composition extraction chamber and the separation and purification chamber.
Among Fig. 1, the 1st, conventional water-cooled condenser pipe; The 2nd, the low level water inlet of water-cooled condenser pipe 1; The 3rd, the inlet plenum of the solvent vapo(u)r carrier pipe that solvent vapo(u)r is upwards carried; The 4th, the composition extraction chamber, the composition abstraction reaction chamber shown in this figure is made of two drawers; The 5th, drawer supports slide rail; The 6th, the separation and purification chamber, the composition abstraction reaction chamber shown in this figure is made of three drawers; The 7th, the panel of drawer; The 8th, by-pass valve control A; The 9th, the solvent recovery chamber; The 10th, detect sample tap; The 11st, solvent adds pipe; The 12nd, be used to change the water inlet pipe that solvent cell cleans behind the another kind of solvent; The 13rd, the heated water bath pond; The 14th, be positioned at heated water bath pond 13 solvent cell to be heated; The 15th, the solvent discharge pipe; 16 are used to the steam pipe of heated water bath pond supplying heat source; The 17th, the high-order delivery port of water-cooled condenser pipe 1; The 18th, the solvent vapo(u)r carrier pipe that solvent vapo(u)r is upwards carried; The 19th, by-pass valve control B; The 20th, be used to control the magnetic stirring apparatus of solvent temperature balance.
Among Fig. 2, the 7th, the panel of drawer; The 21st, be distributed with the drawer-bottom board of even fine and closely woven mesh; The 22nd, drawer side.
The specific embodiment
For the present invention is further understood, existing in conjunction with the accompanying drawings 1, Fig. 2 makes specific description to it.
Embodiment 1
According to the structure shown in the accompanying drawing 1, adopt stainless steel materials and stainless-steel pipe to process to going up solvent feed system, solvent recovery chamber 9, separation and purification chamber 6, the composition extraction chamber 4 that is provided with down and being used for the extraction separation and purification device of the square tower structure that the water-cooled condenser pipe 1 of solvent condenses forms.Wherein the solvent feed system is 800 * 1000 * 200 (mm), and solvent recovery chamber 9 is 800 * 800 * 300 (mm), and separation and purification chamber 6 and composition extraction chamber 4 length and width are 800 * 800 (mm), and height is 1600 (mm); Drawer individual layer hair high by 250 (mm).
The most following three drawers constitute separation and purification chamber 6, in separation and purification chamber 6, every drawer is filled the high 100-200 order silica of 250mm respectively, go up most two drawer constituent extraction chambers 4, and in two drawers, adding is through olive leaf powder (200 order) 4000g of 60 ℃ of oven dry, and solvent cell 14 adds pipe 11 by solvent and injects the 40000mL benzinum.
Feed steam, water-bath heating bath 13 is heated, start the magnetic stirring apparatus 20 that is used to control the solvent temperature balance, the heating stirring and refluxing, the beginning cycling extraction separates purifies.Detect wherein contained chemical composition from detecting sample tap 10 samplings during collection 1000mL solvent in solvent recovery chamber 9.
Detection in the solvent recovery chamber 9 is shown as the identical solution of branch is transferred to solvent cell 14, continue to make solvent to carry out cycling extraction and separate purification by valve 19.When the solution chemistry composition in detecting discovery solvent recovery chamber 9 changes, temporarily stop solution and shift downwards.At this moment will combine in chemical composition is identical in the solvent cell solution and shift, and add pipe 11 by solvent in addition and add chloroform and in heating container, restart new round cycling extraction and separate and purify from the solvent discharge pipe 15 of lower end.When in the chloroformic solution during chemical composition change,, change and add acetone extract by same program.The solution rotating evaporation and concentration that migrates out obtains corresponding oily mater or pressed powder.
By above-mentioned device, extract and separate is purified and is obtained volatile oil, triterpenes and flavone compound respectively, and yield is respectively 1.5%, 2.9% and 13.5%.Be respectively 86.0%, 81.3% and 78.5% through UV and their purity of HPLC detection.
Embodiment 2
Repeat embodiment 1 described structure and operating process, the most following two drawers in composition extraction chamber and the separation and purification chamber are adjusted to composition from purifying chamber 6, go up three drawers most and be adjusted to composition extraction chamber 4; Earlier with being solvent with acetone behind the chloroform, loguat leaf is the plant raw material, and the extract and separate purification obtains triterpene compound and flavone compound respectively, and its yield is 3.1% and 8.4%.Be respectively 83.5% and 79.7% through UV and their purity of HPLC detection.
Embodiment 3
Repeat embodiment 1 described structure and operating process, the most next drawer in composition extraction chamber and the separation and purification chamber is adjusted to composition from purifying chamber 6, go up four drawers most and be adjusted to composition extraction chamber 4; Successively adopting acetone and ethanol is solvent, and the Loquat-Shaped Cake is the plant raw material, and extract and separate is purified and obtained flavonoids and organic acid substance, and its yield is 21.3% and 18.6%.Be respectively 82.6% and 86.8% through UV and their purity of HPLC detection.
Embodiment 4
Repeat embodiment 1 described structure and operating process, the most following two drawers in composition extraction chamber and the separation and purification chamber are adjusted to composition from purifying chamber 6, go up three drawers most and be adjusted to composition abstraction reaction chamber 4; Successively adopting ethanol and water-ethanol (1: 1) is solvent, and loquat seed is the plant raw material, and extract and separate is purified and obtained amarogentin and tannin, and its yield is 8.5% and 2.6%.Be respectively 78.3% and 80.5% through UV and their purity of HPLC detection.
Embodiment 5
Repeat embodiment 1 described structure and operating process, the most following three drawers in composition extraction chamber and the separation and purification chamber are adjusted to composition from purifying chamber 6, go up two drawers most and be adjusted to composition abstraction reaction chamber 4; Successively adopting acetone and ethanol is solvent, and lichee pericarp is the plant raw material, and extract and separate is purified and obtained flavones and polyphenol, and its yield is 6.2% and 7.9%.Through UV and their purity of HPLC detection is 80.1% and 75.6%.
Embodiment 6
Repeat embodiment 1 described structure and operating process, the most following two drawers in composition extraction chamber and the separation and purification chamber are adjusted to composition from purifying chamber 6, go up three drawers most and be adjusted to composition abstraction reaction chamber 4; Successively adopting benzinum, acetone, ethanol and water-ethanol (1: 1) is solvent, and mango leaf is the plant raw material, and extract and separate is purified and obtained volatile oil, flavonoids, mangiferin and tannin, and its yield is 2.3%, 14.2%, 9.3% and 8.3%.Through UV and their purity of HPLC detection is 69.9%, 86.5%, 78.6% and 81.2%.
Claims (6)
1, a kind of extraction separation and purification device that extracts chemical composition in the plant, it is characterized in that extracting the separation and purification device is square tower shape, by forming to the condenser pipe of going up down solvent feed system, solvent recovery chamber, separation and purification chamber, the composition extraction chamber that is provided with and being used for solvent condenses, solvent feed system, solvent recovery chamber, separation and purification are respectively equipped with control valve between the chamber.
2, solvent feed system according to claim 1 comprises the water-bath heating bath that utilized the supplying heat source heating, is positioned at the upwards solvent vapo(u)r carrier pipe of conveying of water-bath heating bath solvent cell to be heated, the magnetic stirring apparatus that is used to control the solvent temperature balance, water-bath temperature-adjusting circuit and solvent vapo(u)r.
3, the extraction separation and purification device that extracts chemical composition in the plant according to claim 1 is characterized in that the solvent recovery chamber is positioned on the solvent cell, and connecting portion therebetween is provided with the solvent vapo(u)r circulation and carries side pipe and solvent recovery control valve.
4, the extraction separation and purification device that extracts chemical composition in the plant according to claim 1, it is characterized in that described composition extraction chamber and separation and purification chamber present down setting, and be in the unified airtight space, this space segmentation becomes contour drawer type sandwich construction, every drawer layer can insert a drawer, the drawer panel medial surface is provided with sealed film, the base plate of drawer is evenly distributed with fine and closely woven mesh, can and extract the difference adjustment composition extraction chamber of composition and the drawer number of separation and purification chamber according to raw material in the use, the composition extraction chamber is used to hold the plant raw material, and the drawer of separation and purification chamber is used to hold extraction separation and purification post.
5, the extraction separation and purification device that extracts chemical composition in the plant according to claim 4, it is characterized in that the post lower end in the described extraction separation and purification post is equipped with Sha Xin, is equipped with other solid state powder separation and purification agent such as an amount of silica gel or aluminium oxide on the Sha Xin.
6, the extraction separation and purification device that extracts chemical composition in the plant according to claim 1 is characterized in that the described condenser pipe that is used for solvent condenses is conventional water-cooled condenser pipe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009101116659A CN101579585A (en) | 2009-05-06 | 2009-05-06 | Extraction and separation purifier capable of extracting chemical composition in plant corpus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009101116659A CN101579585A (en) | 2009-05-06 | 2009-05-06 | Extraction and separation purifier capable of extracting chemical composition in plant corpus |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101579585A true CN101579585A (en) | 2009-11-18 |
Family
ID=41361985
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2009101116659A Pending CN101579585A (en) | 2009-05-06 | 2009-05-06 | Extraction and separation purifier capable of extracting chemical composition in plant corpus |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101579585A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104906214A (en) * | 2015-05-08 | 2015-09-16 | 福建师范大学 | Method for combined preparation of flavonoid and triterpenic acid substances in loquat leaf |
| CN105617710A (en) * | 2016-01-27 | 2016-06-01 | 福建师范大学 | Circular extraction device and method |
| CN106117279A (en) * | 2016-06-20 | 2016-11-16 | 福建师范大学 | Polyphenol and the continuous extraction method of amygdaloside in a kind of loquat nut |
| CN107537181A (en) * | 2017-10-24 | 2018-01-05 | 湖州展舒生物科技有限公司 | Isolate and purify system |
| CN107961559A (en) * | 2017-10-24 | 2018-04-27 | 湖州展舒生物科技有限公司 | One kind isolates and purifies system |
-
2009
- 2009-05-06 CN CNA2009101116659A patent/CN101579585A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104906214A (en) * | 2015-05-08 | 2015-09-16 | 福建师范大学 | Method for combined preparation of flavonoid and triterpenic acid substances in loquat leaf |
| CN104906214B (en) * | 2015-05-08 | 2018-06-19 | 福建师范大学 | The combined preparation process of flavonoids and triterpene acid in a kind of loguat leaf |
| CN105617710A (en) * | 2016-01-27 | 2016-06-01 | 福建师范大学 | Circular extraction device and method |
| CN105617710B (en) * | 2016-01-27 | 2017-09-26 | 福建师范大学 | A kind of cycling extraction device and cycling extraction method |
| CN106117279A (en) * | 2016-06-20 | 2016-11-16 | 福建师范大学 | Polyphenol and the continuous extraction method of amygdaloside in a kind of loquat nut |
| CN106117279B (en) * | 2016-06-20 | 2019-02-15 | 福建师范大学 | The continuous extraction method of polyphenol and amarogentin in a kind of loquat nut |
| CN107537181A (en) * | 2017-10-24 | 2018-01-05 | 湖州展舒生物科技有限公司 | Isolate and purify system |
| CN107961559A (en) * | 2017-10-24 | 2018-04-27 | 湖州展舒生物科技有限公司 | One kind isolates and purifies system |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101797344B (en) | Method for preparing refined total flavonoids in herba lophatheri | |
| CN102432582A (en) | Preparation method of proanthocyanidin | |
| CN101579585A (en) | Extraction and separation purifier capable of extracting chemical composition in plant corpus | |
| CN101353363A (en) | Method for separating and purifying Momordica grosvenori leaf chromocor compound by high-speed countercurrent chromatography and products thereof | |
| CN100439319C (en) | Method for preparing salviol acid A | |
| CN101463025A (en) | Extracting preparation of hawthorn leaves flavonoids | |
| CN104673486A (en) | Method for simultaneously extracting silybum marianum oil and silymarin from silybum marianum cake | |
| CN102228515B (en) | Separation and enrichment method of total flavones and total alkaloids of Lotus Plumule | |
| CN101348474A (en) | Method for preparing salvianolic acid B and tanshinol from Salvia miltiorrhiza stem | |
| CN101519408A (en) | Method for producing glabridin from glycyrrhiza residue | |
| CN107098942A (en) | A kind of method of kaempferia galamga glycosides in Subcritical Water Extraction radish leaves | |
| CN104926767A (en) | Method of purification preparation of citrus flavones by adopting macroporous adsorption resin | |
| CN101401843B (en) | Extracting method for active principle of traditional Chinese medicine red sage root | |
| CN103554209B (en) | Method for preparing ginsenoside Rg1 from pseudo-ginseng | |
| CN201613040U (en) | Device for extracting main bioactive ingredients from plant | |
| CN101973983A (en) | Method for extracting orientins from Chinese globeflower flowers | |
| CN105106327B (en) | The technique that enzymatic hydrolysis-ultrasound coupling method extracts polygonum flaccidum general flavone | |
| CN101735021A (en) | Method for separating and purifying magnolol and honokiol by HP-20 macroporous resin | |
| CN106749456B (en) | A method of the separating high-purity Hyperoside from lotus leaf | |
| CN102670935B (en) | Method for extracting total saponins from allium chinense | |
| CN104721240B (en) | A kind of technique extracted from leaf of Moringa and separate Moringa flavones and Moringa saponin(e | |
| CN102068630A (en) | Method for extracting flavone from bamboo leaves | |
| CN105616477A (en) | Method for purifying polyphenol in lonicera edulis | |
| CN105646638B (en) | The preparation method of pedunculoside | |
| CN111072736A (en) | A component rich in liquiritin and glycyrrhizic acid in Glycyrrhrizae radix extract and its preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20091118 |