CN104490980A - Method for low temperature extraction of eucommia chlorogenic acid by cell wall breaking - Google Patents
Method for low temperature extraction of eucommia chlorogenic acid by cell wall breaking Download PDFInfo
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- CN104490980A CN104490980A CN201310726468.4A CN201310726468A CN104490980A CN 104490980 A CN104490980 A CN 104490980A CN 201310726468 A CN201310726468 A CN 201310726468A CN 104490980 A CN104490980 A CN 104490980A
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Abstract
The invention relates to a natural product extraction method, particularly to a method for extraction of chlorogenic acid from eucommia leaves by a cell wall breaking technology. The method includes: crushing eucommia leaves, destroying the stratum corneum on the leaves by weak base, carrying out low temperature extraction, membrane treatment and reverse osmosis, and combining a resin adsorption and elution process and low temperature continuous band drying. The method provided by the invention adopts the cell wall breaking technology to release chlorogenic acid from eucommia leaves, and the chlorogenic acid dissolution rate is high. By adopting the low temperature extraction and low temperature drying process, the heat loss caused by unstable heating of the heat sensitive component chlorogenic acid is reduced, and also the energy consumption is lowered. Membrane treatment is combined with resin to conduct purification, the impurity removal effect is good, and the chlorogenic acid quality is good.
Description
Technical field
The present invention relates to field of medicinal materials processing, be specially a kind of cell wall breaking extract at low temperature, method that membrane separation technique binding resin technique prepares Cortex Eucommiae chlorogenic acid.
Background technology
Chlorogenic acid (chlorogenic acid) is that one is separated from the leaf and fruit of dicotyledon (as Folium Lonicerae, coffee bean, Helianthi etc.) phenols obtained, also be the main active of many Chinese herbal medicine (as the Cortex Eucommiae, Flos Lonicerae, Herba Artemisiae Scopariae etc.) and compound Chinese medicinal preparation anti-inflammation, heat-clearing and toxic substances removing, become one of leading indicator of Chinese herbal and crude drugs preparations quality control at present.Chinese herbal medicine is the rarity of Chinese nation's civilization in several thousand, is the pride of our descendants of the Yellow.Over the past thousands of years, our ancestors use Chinese herbal medicine and compound preparation thereof in preventing and curing diseases, achieve abnormal abundant clinical experience, leave large quantities of medical masterpiece.In recent years, due to spreading unchecked of Western medicine, the variation of pathogenic microorganism and Drug resistance also achieve considerable " progress ", so people have turned one's attention to Chinese herbal medicine again.Particularly day by day advocate " rear antibiotic " epoch that are natural, pollution-free food people, Chinese herbal medicine is subject to the unprecedented favor of people gradually with its original advantage, in Chinese herbal medicine, the extraction process of effective ingredient, the mechanism of action, applied research also become the focus that the world of medicine chases again, and become a general orientation of Animal nutrition circle research gradually.
Chlorogenic acid is plant a kind of phenylpropanoids through shikimic acid pathway generation in aerobic respiration process.It is a kind of by caffeic acid (caffeic acid) and quinic acid (quinovic acid, quinic acid, i.e. QA) depside of condensation, different name caffeotannic acid, chemical name CA (3-O-caffeoylquinic acid), molecular formula is C
16h
18o
9, molecular weight: 345.30, semihydrate is acicular crystal, becomes anhydrous compound when 110 DEG C, and soluble in water, ethanol, acetone, be slightly soluble in ethyl acetate, in faint yellow solid under room temperature.
The biosynthesis of plant Content of Chlorogenic Acid includes a series of enzymatic reaction.Under the catalysis of enzyme, conversion of glucose becomes shikimic acid (shikimic acid), and the latter changes into phenylalanine again, obtains chlorogenic acid finally by synzyme effect.Its possible biosynthesis pathway is as follows: chlorogenic acid is widely distributed in plant, all report is had to pteridophyta from high dicotyledon, but the plant that content is higher is few, mainly be present in Caprifoliaceae Lonicera (Lonicera), Compositae artemisia (Artemisia) plant, comprising the Cortex Eucommiae, Flos Lonicerae, Helianthi, coffee.
Because chlorogenic acid is the organic acid that polarity is stronger, be soluble in alcohol, water, be insoluble in chloroform, ether, therefore the extracting method of chlorogenic acid is more, has alcohol (methanol, ethanol) molten method, water extract-alcohol precipitation, alcohol extraction lead heavy method and Thin-layer chromatography etc.
The molten method of alcohol: it is colourless for being first extracted into effluent continuously with chloroform, then use 95% industrial alcohol extraction instead, carry most chlorogenic acid; Gained ethanol extract concentrating under reduced pressure is become extractum, after clean fine sand mix, with hot water extraction several, makes chlorogenic acid turn soluble in water, discard residue; Obtained aqueous solution extracted with diethyl ether, removes oil-soluble impurities further; In the aqueous solution after defat, add saturated inorganic salt solution, to precipitation completely, and slightly excessive till.Now, the chlorogenic acid in water is combined with metal ion and generates insoluble salt; Isolate by centrifugal separation and to precipitate and after the metal ion removed in precipitation, by gained filtrate with organic solvent extraction for several times, recycling design, obtains chlorogenic acid crude product, and refine through the method such as fractional crystallization and recrystallization, obtain chlorogenic acid pure product, yield is about 0.5%.The drawback of the molten method of alcohol: solvent loss amount adds production cost greatly, seriously.
Decoction and alcohol sedimentation technique: employing water is solvent, heated and boiled is extracted, but correspondingly increases other water soluble ingredients as impurity such as protein, polysaccharide, tannins, available traditional alcohol deposition method removing.With absorption with sandwich in precipitate with ethanol process, chlorogenic acid is caused to have loss in various degree.When extracting Aqueous extracts Content of Chlorogenic Acid, gradation precipitate with ethanol is higher than a precipitate with ethanol products obtained therefrom purity; When concentration of alcohol is finally 90%, the loss rate of a precipitate with ethanol is larger than gradation precipitate with ethanol.
Also exist in above extraction scheme that extraction ratio is not high, product purity is low, energy-intensive problem, seriously constrain the development of Cortex Eucommiae industry.
Summary of the invention
Object of the present invention: in order to overcome above-mentioned Problems existing and defect, the invention provides a kind of method of cell wall breaking extract at low temperature Cortex Eucommiae chlorogenic acid.The method is after being pulverized by Folium Eucommiae, adopts the horny layer on weak base destruction blade, by extract at low temperature, film process, reverse osmosis, adsorption and desorption by resin technique, concentrated and low temperature continuous band drying preparation Cortex Eucommiae chlorogenic acid.
The technical solution adopted for the present invention to solve the technical problems is: adopt a kind of method step of cell wall breaking extract at low temperature Cortex Eucommiae chlorogenic acid to comprise:
1, extract: for the first time: be the alkaline soak (3 times of water yields of Folium Eucommiae weight) 20 minutes of 9 with pH value, then aqueous alkali is put back in storage tank and soak aqueous alkali for subsequent use for the first time as next group raw material; For the second time: the 7 times of pH value adding Folium Eucommiae weight are the dynamic extract at room temperature of pure water 2 hours of 2, blowing liquid; For the third time: the pure water room temperature dynamic extraction 2 hours adding 6 times of pH value 4 of Folium Eucommiae weight, blowing liquid; 4th time: the pure water adding Folium Eucommiae weight 8 times, is warmed to 60 DEG C, dynamic extraction 1 hour, blowing liquid, is cooled to less than 30 DEG C with sheet frame during fluid, and this feed liquid is as the second time Extraction solvent of next group raw material;
2, centrifugal: the feed liquid after extracting with high speed tubular type centrifuge, remove suspended impurity, flow velocity is no more than 1t/h;
3, membrance separation: go out the protein in Folium Eucommiae, polysaccharide, tannin with the ceramic membrane separation of 0.5 micron;
4, reverse osmosis concentration: use reverse osmosis membrane recycle-water, is concentrated to 4 times of volumes of Folium Eucommiae raw material weight;
5, upper resin column: resin model is NKA-9 macroporous adsorbent resin, upper column flow rate is that 0.6 times amount of column volume is per hour;
6, eluting: with 50% ethanol elution of column volume 3 times amount, flow speed control is per hour in 0.6 times amount of column volume, collects eluent;
7, reclaim eluent: concentration and recovery ethanol, being concentrated to relative density is 1.08 fluids;
8, dry: continuous low temperature belt drying, pulverizing, temperature controls at 45 DEG C-60 DEG C.
In the present invention, described resin regeneration method is: new resin 90% soak with ethanol 12 hours, 90% ethanol consumption is as the criterion for can all be dipped into resin, again with the 5%NaOH process of column volume doubling dose, being washed till pH value with pure water is 8.0, again with the 3%HCl process of column volume doubling dose, being washed till pH value with pure water is 6.
The beneficial effect that the present invention has:
1, the present invention adopts cell wall technology of breaking to be discharged from Folium Eucommiae by chlorogenic acid, and chlorogenic acid dissolution rate is high;
2, the present invention adopts extract at low temperature, low temperature drying technology, decreases heat-sensitive ingredients chlorogenic acid because of by the thermogenetic loss of thermally labile, reduces energy consumption simultaneously;
3, the present invention adopts film process binding resin to carry out purification, and Impurity removal is effective, chlorogenic acid quality better.
Accompanying drawing explanation
Fig. 1 represents present invention process flow chart.
Detailed description of the invention
The technological means realized to make the present invention, creation characteristic, reaching object and effect is easy to understand, setting forth the present invention further below in conjunction with specific embodiment.
Embodiment 1: the Folium Eucommiae taking 1Kg, extracts and divides four times.For the first time: with pH value be 9 aqueous alkali 3 kilograms soak 20 minutes, then using aqueous alkali put back in storage tank as next group raw material first time soak aqueous alkali for subsequent use; For the second time: add the dynamic extract at room temperature of pure water 2 hours that 7Kg pH value is 2, blowing liquid; For the third time: add pure water room temperature dynamic extraction 2 hours blowings that 6Kg pH value is 4; 4th time: add 8Kg pure water, be warmed to 60 DEG C, dynamic extraction 1 hour, blowing liquid, be cooled to less than 30 DEG C during fluid with sheet frame, this feed liquid is as the second time Extraction solvent of next group raw material; Centrifugal: the Cortex Eucommiae mother solution after extracting with high speed tubular type centrifuge, remove suspended impurity, flow velocity is no more than 1t/h; Membrance separation: go out the protein in Folium Eucommiae, polysaccharide, tannin with the ceramic membrane separation of 0.5 micron; Reverse osmosis membrane: use reverse osmosis membrane recycle-water, being concentrated to volume is 4L; Upper resin column: resin model is NKA-9 macroporous absorption, upper column flow rate is that 0.6 times amount of column volume is per hour; Eluting: with 50% ethanol elution of column volume 3 times amount, flow speed control is per hour in 0.6 times amount of column volume, collects eluent; Reclaim eluent: being concentrated to relative density with outer circulation concentration and recovery ethanol is 1.08 fluids; Dry: continuous low temperature belt drying, pulverizing, temperature controls at 45 DEG C-60 DEG C, obtains the chlorogenic acid that 16.2g purity is 65.6%.
Embodiment 2: the Folium Eucommiae taking 1Kg, extracts and divides four times.For the first time: the aqueous alkali reclaimed after soaking with embodiment 1 first time also complements to 3 kilograms with the aqueous alkali that the pH value of new configuration is 9 and soaks 20 minutes, then aqueous alkali is put back in storage tank and soak aqueous alkali for subsequent use for the first time as next group raw material; For the second time: add the dynamic extract at room temperature of pure water 2 hours that 7Kg pH value is 2, blowing liquid; For the third time: add pure water room temperature dynamic extraction 2 hours blowings that 6Kg pH value is 4; 4th time: add embodiment 1 and extract the feed liquid of gained and complement to 8Kg with pure water for the 4th time, be warmed to 60 DEG C, dynamic extraction 1 hour, blowing liquid, be cooled to less than 30 DEG C during fluid with sheet frame, this feed liquid is as the second time Extraction solvent of next group raw material; Centrifugal: the Cortex Eucommiae mother solution after extracting with high speed tubular type centrifuge, remove suspended impurity, flow velocity is no more than 1t/h; Membrance separation: go out the protein in Folium Eucommiae, polysaccharide, tannin with the ceramic membrane separation of 0.5 micron; Reverse osmosis membrane: use reverse osmosis membrane recycle-water, being concentrated to volume is 4L; Upper resin column: resin model is NKA-9 macroporous absorption, upper column flow rate is that 0.6 times amount of column volume is per hour; Eluting: with 50% ethanol elution of column volume 3 times amount, flow speed control is per hour in 0.6 times amount of column volume, collects eluent; Reclaim eluent: being concentrated to relative density with outer circulation concentration and recovery ethanol is 1.08 fluids; Dry: continuous low temperature belt drying, pulverizing, temperature controls at 45 DEG C-60 DEG C, obtains the chlorogenic acid that 16.5g purity is 65.0%.
Embodiment 3: the Folium Eucommiae taking 1Kg, extracts and divides four times.For the first time: the aqueous alkali reclaimed after soaking with embodiment 2 first time also complements to 3 kilograms with the aqueous alkali that the pH value of new configuration is 9 and soaks 20 minutes, then aqueous alkali is put back in storage tank and soak aqueous alkali for subsequent use for the first time as next group raw material; For the second time: add the dynamic extract at room temperature of pure water 2 hours that 7Kg pH value is 2, blowing liquid; For the third time: add pure water room temperature dynamic extraction 2 hours blowings that 6Kg pH value is 4; 4th time: add 8Kg embodiment 2 and extract the feed liquid of gained and complement to 8Kg with pure water for the 4th time, be warmed to 60 DEG C, dynamic extraction 1 hour, blowing liquid, be cooled to less than 30 DEG C during fluid with sheet frame, this feed liquid is as the second time Extraction solvent of next group raw material; Centrifugal: the Cortex Eucommiae mother solution after extracting with high speed tubular type centrifuge, remove suspended impurity, flow velocity is no more than 1t/h; Membrance separation: go out the protein in Folium Eucommiae, polysaccharide, tannin with the ceramic membrane separation of 0.5 micron; Reverse osmosis membrane: use reverse osmosis membrane recycle-water, being concentrated to volume is 4L; Upper resin column: resin model is NKA-9 macroporous absorption, upper column flow rate is that 0.6 times amount of column volume is per hour; Eluting: with 50% ethanol elution of column volume 3 times amount, flow speed control is per hour in 0.6 times amount of column volume, collects eluent; Reclaim eluent: being concentrated to relative density with outer circulation concentration and recovery ethanol is 1.08 fluids; Dry: continuous low temperature belt drying, pulverizing, temperature controls at 45 DEG C-60 DEG C, obtains the chlorogenic acid that 16.0g purity is 66.4%.
More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention; the technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and description just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications; these changes and improvements all fall in the claimed scope of the invention, and application claims protection domain is defined by appending claims and equivalent thereof.
Claims (1)
1. a method for cell wall breaking extract at low temperature Cortex Eucommiae chlorogenic acid, is characterized in that, comprise the following steps:
(1) extract: for the first time: be the alkaline soak (3 times of water yields of Folium Eucommiae weight) 20 minutes of 9 with pH value, then aqueous alkali is put back in storage tank and soak aqueous alkali for subsequent use for the first time as next group raw material; For the second time: the 7 times of pH value adding Folium Eucommiae weight are the dynamic extract at room temperature of pure water 2 hours of 2, blowing liquid; For the third time: the 6 times of pH value adding Folium Eucommiae weight are the pure water room temperature dynamic extraction 2 hours of 4, blowing liquid; 4th time: the pure water adding Folium Eucommiae weight 8 times, is warmed to 60 DEG C, dynamic extraction 1 hour, blowing liquid, is cooled to less than 30 DEG C with sheet frame during fluid, and this feed liquid is as the second time Extraction solvent of next group raw material;
(2) centrifugal: the feed liquid after extracting with high speed tubular type centrifuge, remove suspended impurity, flow velocity is no more than 1t/h;
(3) membrance separation: go out the protein in Folium Eucommiae, polysaccharide, tannin with the ceramic membrane separation of 0.5 micron;
(4) reverse osmosis concentration: use reverse osmosis membrane recycle-water, is concentrated to 4 times of volumes of Folium Eucommiae raw material weight;
(5) upper resin column: resin model is NKA-9 macroporous adsorbent resin, and upper column flow rate is that 0.6 times amount of column volume is per hour;
(6) eluting: with 50% ethanol elution of column volume 3 times amount, flow speed control is per hour in 0.6 times amount of column volume, collects eluent;
(7) reclaim eluent: concentration and recovery ethanol, being concentrated to relative density is 1.08 fluids;
(8) dry: continuous low temperature belt drying, pulverizing, temperature controls at 45 DEG C-60 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110934216A (en) * | 2018-09-21 | 2020-03-31 | 黄钰庭 | Method for processing coffee beans |
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| CN101157827A (en) * | 2007-09-27 | 2008-04-09 | 贵州大学 | Method for extracting filament gutta-percha from eucommia leaf and skin |
| CN102267906A (en) * | 2011-06-23 | 2011-12-07 | 湖南长沙远航生物制品有限公司 | Extraction method for chlorogenic acid |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101157827A (en) * | 2007-09-27 | 2008-04-09 | 贵州大学 | Method for extracting filament gutta-percha from eucommia leaf and skin |
| CN102267906A (en) * | 2011-06-23 | 2011-12-07 | 湖南长沙远航生物制品有限公司 | Extraction method for chlorogenic acid |
Non-Patent Citations (2)
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| 张吉波等: "杜仲叶中绿原酸水提工艺的优化及其防腐效果研究", 《食品科技》, vol. 38, no. 4, 30 April 2013 (2013-04-30), pages 232 - 236 * |
| 李玉山: "绿原酸在天然植物中的分布和提取纯化工艺研究进展", 《解放军药学学报》, vol. 28, no. 4, 31 August 2012 (2012-08-31), pages 355 - 359 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110934216A (en) * | 2018-09-21 | 2020-03-31 | 黄钰庭 | Method for processing coffee beans |
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Application publication date: 20150408 |