CN105481872A - Method for extracting plant active ingredients by constant temperature gradient in-series extraction - Google Patents
Method for extracting plant active ingredients by constant temperature gradient in-series extraction Download PDFInfo
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- CN105481872A CN105481872A CN201510858904.2A CN201510858904A CN105481872A CN 105481872 A CN105481872 A CN 105481872A CN 201510858904 A CN201510858904 A CN 201510858904A CN 105481872 A CN105481872 A CN 105481872A
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- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/02—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains two hetero rings
- C07D493/04—Ortho-condensed systems
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
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- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
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Abstract
A method for extracting plant active ingredients by constant temperature gradient in-series extraction is as follows: 3-5 extraction tanks are taken for in-series connection, a plant material is divided equally according to the number of the extraction tanks, and respectively put into each extraction tank; an extracting agent is added into a first extraction tank for heating thermal-insulation extraction, then an extract of the first extraction tank is pumped into a second extraction tank to be used as an extraction solvent, and is heated to the previous-time extraction temperature for thermal-insulation extraction for the same time, and the rest may be deduced by analogy until the thermal-insulation extraction is performed on the last extraction tank for the same time, and an obtained extract is centrifuged and filtered; an extraction agent is added into a material residue of the first extraction tank for repeated in-series extraction for 1-2 times at the previously-described extraction temperature by the previously-described method, and an obtained extract is centrifuged and filtered, and filtrates of various times are merged. According to the method, extraction devices (extraction tanks) of a conventional solvent extraction method are in-series connection, the more extraction raw materials are, the more the extraction tanks are, and the higher the extraction rate is; compared with the conventional solvent extraction method, at least 30-50% of reagents are saved, and at least 30% of workload of concentration and recovery of a next working procedure can be reduced.
Description
Technical field
The present invention relates to a kind of method extracting activeconstituents from plant, especially relate to the method that active components of plants is extracted in the series connection of a kind of constant temperature gradient.
Background technology
Solvent-extraction process is the most basic, most widely used method in plant extract activeconstituents technology, and it is the character according to effective constituent solubleness various in plant, by a kind of extracting method that required activeconstituents is dissolved out in medicinal material tissue.The method device fabrication cost is low, and technology is very ripe, and the most frequently used is water extraction and organic solvent extraction.As the publication number application that is CN101190258 be a kind of from yulan leaf and/spend middle extraction to be rich in the method for the total sesquiterpene lactone compounds of parithenolide, be first soak with deionized water, then extract with lower alcohol multi-reflow.For another example publication number is the patent of CN103524520A is by Magnoliacea plant material dry, pulverizing, carbon dioxide upercritical fluid extraction.But, solvent-extraction process produce in single tank raw material repeatedly drop into reagent respectively, in heating for multiple times, reagent consumption is large, and extraction time, heat-up time are long, and take the equipment time long, production efficiency is low.
Summary of the invention
Technical problem to be solved by this invention is: for above-mentioned the deficiencies in the prior art, there is provided a kind of constant temperature gradient to connect and extract the method for active components of plants, adopt the method for extractor series connection, extracting solution repeatedly utilizes at a certain temperature, gradient extraction, to improve extraction efficiency, reduce production cost.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is: the method for active components of plants is extracted in a kind of constant temperature gradient series connection, the method gets 3-5 extractor series connection, plant material for carrying out extracting is inserted in each extractor by after tank number decile respectively, extraction agent is added in the first extractor, heating and thermal insulation lixiviate, again the extracting solution of the first extractor is drawn in the second extractor as Extraction solvent, be heated to previous Extracting temperature (extraction temperature in the first extractor) and be incubated lixiviate same time (extraction time in the first extractor), then the extracting solution of the second extractor is drawn in the 3rd extractor as Extraction solvent, be heated to previous Extracting temperature (extraction temperature in the second extractor) and be incubated lixiviate same time (extraction time in the second extractor), the rest may be inferred, until the extracting solution of more than last an extractor extractor is incubated lixiviate same time (extraction time in a upper extractor) under previous Extracting temperature (extraction temperature in a upper extractor), the extracting solution centrifuging obtained, then in the material slag of the first extractor, add extraction agent under aforementioned Extracting temperature and extraction time, repeat series connection extraction 1-2 time by preceding method, the extracting solution centrifuging obtained, merges the filtrate of each time.Wherein, the above-mentioned filtration mentioned adopts tripodia centrifugal cloth bag 200 order to filter.
As, activeconstituents parithenolide is extracted: be first by broken for fresh for southern magnolia leaf making beating from the fresh leaf of southern magnolia, the ratio that 2mL volumetric concentration is the polarity organic reagent of 80%-95% is added in 1g leaf slurry, polarity organic reagent is added in leaf slurry, cold soaking bubble 12-24h under normal temperature, carry out decile by series can number again, join in each series can respectively, for subsequent use; Wherein, polarity organic reagent is methyl alcohol, ethanol or amylalcohol.The extraction agent added in the fresh leaf slurry of the southern magnolia of the first extractor or material slag is the methyl alcohol of 80%-95% volumetric concentration, ethanol or amylalcohol, the add-on of this extraction agent starches/expect in the fresh leaf of 1g southern magnolia the ratio that slag adds 8ml extraction agent to add, Extracting temperature is 65-70 DEG C, and extraction time is 20-30min.
Or, from green tea, extract green tea polyphenol: after green tea etc. is divided into extractor, the extraction agent added in the green tea/material slag of the first extractor is deionized water, and the ratio that deionized water adds 8ml deionized water in 1g green tea/material slag adds, Extracting temperature is 85 DEG C-90 DEG C, and extraction time is 45-50min.
In actual production, material slag can carry out repeating for 4-5 time to extract, and after 2-3 time is repeated extraction, the material slag in the first extractor can be replaced by new raw material, with the second extractor for initial extraction tank, add new extraction agent, lixiviate successively, now, lixiviate order becomes the second extractor and extracts at first, successively until last extractor, and the last lixiviate of the first extractor.Change raw material, extraction agent and lixiviate order by same principle, production can be made to carry out continuously.
The present invention carries out lixiviate under extractor being series at constant temperature, the tank connected is more (can be the extractor series connection of more than 3, but 3 must not be less than), extracting times is more, in extracting solution the concentration of effective constituent step by step gradient increase progressively, finally make the concentration of effective constituent in extracting solution reach highest level.Compared with the traditional technology extracted respectively with each tank, when using equivalent extraction agent, extraction efficiency can effectively improve, and continuous production is good, and the usefulness of subsequent concentration, evaporation recycling design also will improve, and effectively can reduce production cost.Also effectively can improve the concentration of activeconstituents in extracting solution in plant by present method, simplify subsequent purification difficulty, making in subsequent technique without the need to adopting complicated procedures of forming can obtain the higher product of purity.
So, constant temperature gradient series connection of the present invention is extracted extraction equipment (extractor) series connection in Conventional solvents extraction method, and extract raw material more, extractor number is more, and extraction yield is higher; Save reagent at least 30-50% than traditional solvent extraction method, the workload at least 30% of subsequent processing concentration and recovery can be alleviated.
Embodiment
Embodiment 1 extracts parithenolide from the fresh leaf of southern magnolia
Get 4 extractor series connection, take the making beating of 50kg southern magnolia fresh leaf broken, leaf slurry is divided into 4 parts, every part of 12.5kg, is placed in the methyl alcohol that 25L volumetric concentration is 90% respectively, cold soaking bubble 20h under normal temperature.Leaf slurry after these 4 parts of cold soaking bubbles is placed in this 4 extractors respectively, the methyl alcohol that 100L volumetric concentration is 90% is added in the first extractor, heat to 65-70 DEG C and keep this temperature, the extracting solution extracting the first extractor after 30min in the second extractor as extraction agent, heat in second extractor to 65-70 DEG C and keep this temperature, the extracting solution extracting the second extractor after 30min in the 3rd extractor as extraction agent, heat in 3rd extractor to 65-70 DEG C and keep this temperature, the extracting solution of the 3rd extractor is extracted in the 4th extractor as extraction agent after 30min, heat in 4th extractor to 65-70 DEG C and keep this temperature 30min, the extracting solution obtained is through the centrifugal Bag filter of tripodia (200 order), the methyl alcohol that 100L volumetric concentration is 90% is added in material slag remaining in the first extractor again, heat to 65-70 DEG C and keep this temperature, the extracting solution extracting the first extractor after 30min in the second extractor as extraction agent, heat in second extractor to 65-70 DEG C and keep this temperature, the extracting solution extracting the second extractor after 30min in the 3rd extractor as extraction agent, heat in 3rd extractor to 65-70 DEG C and keep this temperature, the extracting solution of the 3rd extractor is extracted in the 4th extractor as Extraction solvent after 30min, heat in 4th extractor to 65-70 DEG C and keep this temperature 30min, the extracting solution obtained is through the centrifugal Bag filter of tripodia (200 order), merge 2 filtrates.Filtrate reclaims methyl alcohol through vacuum-concentrcted, carries out subsequent handling by prior art, and last products obtained therefrom after testing parithenolide content is 95.1%.
Comparison example 1
By adopting deionized water to extract water-soluble portion at present from the fresh leaf of southern magnolia, then undertaken by the method for the mixed solvent extraction parithenolide crude product of first alcohol and water.50kg southern magnolia fresh leaf decile, be loaded in 4 extraction list tanks of not connecting, utilize these 4 to extract single tank and extract parithenolide from the fresh leaf of southern magnolia, extract rear and carry out subsequent handling by the prior art identical with embodiment 1, products obtained therefrom parithenolide content is 81.3%.Than the series connection extraction method of the application, deionized water multiplex 30%, Extraction solvent multiplex 30%, concentration and recovery workload is high by more than 30%.
Embodiment 2 extracts green tea polyphenol from green tea
Get 3 extractor series connection, 300kg green tea materials is divided into 3 equal portions (100kg/ part), is dosed into respectively in these 3 series connection extractors.800kg deionized water is heated to 85 DEG C, is extracted into as extraction agent in the first extractor, extracts 45min in 85 DEG C; The extracting solution of the first extractor is extracted in the second extractor as extraction agent, be heated to previous Extracting temperature 85 DEG C insulation lixiviate 45min, the extracting solution of the second extractor is extracted in the 3rd tank extractor, be heated to 85 DEG C, insulation, lixiviate 45min at such a temperature, the extracting solution obtained is through the centrifugal Bag filter of tripodia (200 order).Then in the material slag of the first extractor, expect that the ratio that slag adds 8ml deionized water adds deionized water in 1g, in 85 DEG C of insulation lixiviate 45min, the extracting solution of the first extractor is drawn in the second extractor as extraction agent, in 85 DEG C of insulation lixiviate 45min, again the extracting solution of the second extractor is extracted in the 3rd extractor as extraction agent, 85 DEG C of insulation lixiviate 45min, the extracting solution obtained is through the centrifugal Bag filter of tripodia (200 order).Then in the material slag of the first extractor, expect that the ratio that slag adds 8ml deionized water adds deionized water in 1g again, lixiviate is again carried out by preceding method, the extracting solution obtained filters through tripodia centrifugal cloth bag 200 order, merges 3 filtrates, carries out subsequent handling by prior art.The raw material leaching yield of present method is 32%, and tea-polyphenol detection level reaches 43%, and extraction solvent (deionized water) is no more than 2000kg and just can reaches extraction effect, and extracting solution solid content reaches 3%.
Comparison example 2
The water extraction technology mainly adopted by current green tea polyphenol is carried out.By 300kg green tea materials trisection, be loaded on respectively in 3 extraction list tanks of not connecting, the ratio adding 8ml deionized water in 1g raw material adds deionized water extraction respectively 3 times in each tank, Extracting temperature 85 DEG C, each 45-60 minute.Extracting solution centrifuging, merging filtrate, carries out subsequent handling by the prior art identical with embodiment 2, and extracting solution solid content is below 1.8%, and raw material leaching yield is 24%, and detecting polyphenol content is 33%.The deionized water added all need be heated to 85 DEG C from normal temperature, and energy consumption is too many, and relative to present method, deionized water consumption at least wants many 30%, and concentration and recovery workload also increases by more than 30%.
Claims (6)
1. a method for active components of plants is extracted in the series connection of constant temperature gradient, it is characterized in that, the method gets 3-5 extractor series connection, by the plant material for carrying out extracting by tank number decile, inserts in each extractor respectively; Extraction agent is added in the first extractor, heating and thermal insulation lixiviate, again the extracting solution of the first extractor is drawn in the second extractor as Extraction solvent, be heated to previous extraction temperature, insulation lixiviate same time, the rest may be inferred, until last extractor is incubated lixiviate same time under aforementioned extraction temperature, and the extracting solution centrifuging obtained; Then in the material slag of the first extractor, add extraction agent under aforementioned extraction temperature, repeat series connection extraction 1-2 time by preceding method, the extracting solution centrifuging obtained, merges the filtrate of each time.
2. the method for active components of plants is extracted in a kind of constant temperature gradient series connection as claimed in claim 1, it is characterized in that, described plant material is the fresh leaf of southern magnolia, activeconstituents is parithenolide, the extraction agent added in first extractor is the methyl alcohol of 80%-95% volumetric concentration, ethanol or amylalcohol, extraction agent is starched/is expected in the fresh leaf of 1g southern magnolia the ratio that slag adds 8ml extraction agent and adds, and Extracting temperature is 65-70 DEG C, and extraction time is 20-30min.
3. the method for active components of plants is extracted in a kind of constant temperature gradient series connection as claimed in claim 2, it is characterized in that, insert again in extractor after the fresh leaf of described southern magnolia is handled as follows: by broken for fresh for southern magnolia leaf making beating, the ratio that 2mL volumetric concentration is the polarity organic reagent of 80%-95% is added in 1g leaf slurry, polarity organic reagent is added, cold soaking bubble 12-24h under normal temperature in leaf slurry.
4. the method for active components of plants is extracted in a kind of constant temperature gradient series connection as claimed in claim 3, and it is characterized in that, described polarity organic reagent is methyl alcohol, ethanol or amylalcohol.
5. the method for active components of plants is extracted in a kind of constant temperature gradient series connection as claimed in claim 1, it is characterized in that, described plant material is green tea, extract component is green tea polyphenol, the extraction agent added in first extractor is deionized water, the ratio that deionized water adds 8ml deionized water in 1g green tea/material slag adds, and Extracting temperature is 85 DEG C-90 DEG C, and extraction time is 45-50min.
6. the method for active components of plants is extracted in a kind of constant temperature gradient series connection as claimed in claim 1, and it is characterized in that, described filtration adopts tripodia centrifugal cloth bag 200 order to filter.
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| CN109609277A (en) * | 2019-01-24 | 2019-04-12 | 河北省农林科学院经济作物研究所 | A kind of continuous extracting device and technique |
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