CN101972320B - Method for extracting ferulic acid, chlorogenic acid and other aicd components from coptis chinensis franch - Google Patents
Method for extracting ferulic acid, chlorogenic acid and other aicd components from coptis chinensis franch Download PDFInfo
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Abstract
The invention relates to a method for extracting ferulic acid, chlorogenic acid and other aicd components from coptis chinensis franch, comprising the following process flows: smashing raw materials (coptis chinensis franch, or coptis chinensis franch fibril or coptis chinensis franch byproducts); adding a proper quantity of 0.01-10% sulfuric acid (or sodium bisulfite or sulphurous acid) for dipping; neutralizing, precipitating and decontaminating; decoloring with activated carbon; decompressing for concentration until the obtained product is almost dry; obtaining primary crude; extracting with alcohol or methyl alcohol; recovering solvent; and obtaining the product. The product contains over 30% of acidic components such as ferulic acid, chlorogenic acid and the like in the product. The product has the excellent action of antioxidation lowering blood sugar, lowering blood fat, resisting cancer, beautifying and the like.
Description
Technical field
The invention belongs to a kind of natural product extracting technique, be specifically related to a kind of acid ingredient extraction process technology such as ferulic acid and chlorogenic acid of from Rhizoma Coptidis, extracting.
Background technology
The Rhizoma Coptidis bitter in the mouth, cold in nature, the function of pathogenic fire purging, detoxifcation, heat clearing away, dampness is arranged.Be used for dysphoria with smothery sensation coma, vexed insomnia, damp and hot feeling of fullness, vomiting, stomachache dysentery, conjunctival congestion toxic swelling, aphtha of the mouth and tongue, eczema, scald, haematemesis, epistaxis etc.The Rhizoma Coptidis beginning is stated from Shennong's Herbal, classifies as top grade.The modern Chinese medicine chemical research is the result show, the effective ingredient of Rhizoma Coptidis is Rhizoma Coptidis alkaloid and acid ingredient.At present, the alkaloid of from Rhizoma Coptidis, having separated have berberine (berberine, BBR), tens (Kuang Yanhui, Zhu Jingjing, Wang Zhimin, Peng Xinjun such as palmatine, coptisine, 13-methyl-.psi.-coptisine., jateorhizine, epiberberine, magnoline and berbamine.Coptis plant chemical constituent and Study on Quality Control progress.Chinese Pharmaceutical Journal.43（15）：1121～1125,2008）。The pharmacologically active of Rhizoma Coptidis and Rhizoma Coptidis alkaloid especially hypoglycemic activity obtains broad research (Choi B. H.etcl. Nutrition Research and Practice, 2009,3 (2): 84-88).Rhizoma Coptidis still contains ferulic acid, chlorogenic acid, 3 except that containing the alkaloid activity composition, (acid ingredients such as 4-dihydroxyphenyl ethanol glycosides are rectified gorgeous brightness Zhu Jingjing Wang Zhi people monarch Peng Xin.Coptis medicinal plants chemical constituent and Study on Quality Control progress.Chinese Pharmaceutical Journal, 2,008 43 (15)).The research report of Rhizoma Coptidis acid ingredient is few; But the medical value about ferulic acid and chlorogenic acid etc. but has a large amount of bibliographical informations: ferulic acid has antiplatelet aggregation; Suppress the platelet 5-hydroxy tryptamine and discharge, suppress the generation of the plain A2 of platelet thrombus (TXA2), it is active to strengthen prostaglandin; Analgesia, effects such as alleviating vascular spasm.Be to produce the base stock that is used to treat disease medicines such as cardiovascular and cerebrovascular disease and leukopenia; That chlorogenic acid has is antibiotic, antiinflammatory, detoxifcation, function of gallbladder promoting, blood pressure lowering and leukocyte increasing and significantly increase gastrointestinal peristalsis and promote pharmacological actions such as gastric secretion, is that type of reaching has the active component of medical value very much.
96105233.3,91105606.8) etc. more to the extraction of Rhizoma Coptidis alkaloid research report: Chinese patent document (application number: reported a kind of berberine extraction process technology; Raw material (generally being Radix Berberidis or Cortex Phellodendri or Rhizoma Coptidis) soaks with sulfuric acid solution; Extracting solution neutralizes with Calx; Neutralizer adds sodium chloride deposition (thick level product), and primary product are water-soluble re-refines etc.; Chinese patent document (200510044345.8) has been reported a kind of Rhizoma Coptidis total alkaloids extractive technique, mainly comprises: the Rhizoma Coptidis medical material, and water decocts; Last macroporous resin purifies, washing, aquiferous ethanol eluting; Reclaim ethanol; Concentrate drying obtains processes such as product, and its Rhizoma Coptidis total alkaloids content reaches 25～100%.Extractive technique about chlorogenic acid and ferulic acid also has a large amount of reports: Chinese patent document (application number: 01144170.4) reported " method for extraction and purification of chlorogenic acid in the Flos Lonicerae ": adopt Diluted Alcohol that Flos Lonicerae is carried out secondary back and extract; The preliminary edulcoration purification of concentrated extract reuse flocculence adopts Amberlyst process or acid ethyl acetate extraction method purification refine at last; Chinese patent document (application number: 99115374.X) reported " process for preparing chlorogenic acid from eucommia leaves ": accomplish by steps such as ultrasonic pretreatment and high temperature extraction, ultrafiltration, ethyl acetate extraction, D-140 resin isolation; The Chinese patent document (application number: 200410065240.6) reported " Nicotiana tabacum L. prepares the method for chlorogenic acid as the application of preparation chlorogenic acid raw material and with Nicotiana tabacum L. ": handle down and with organic solvent raw material carried out lixiviate, and gained liquid is rough chlorogenic acid product after solid-liquid separation by microwave or ultrasonic method; (application number: 200510000484.0) reported " production technology of chlorogenic acid extracting from Herba Arctii leaf ": fresh Herba Arctii leaf is after cleaning the defat of roguing chloroform, decolouring for the Chinese patent document; With sour water reflux, extract,, filtration, concentrating under reduced pressure; Reuse ethyl acetate extraction, concentrating under reduced pressure; Then with the absorption of AB-8 resin column, ethanol elution, eluent is concentrated, reuse AB-8 resin absorption, ethanol elution, eluent concentrate, recrystallization and make the pure article of chlorogenic acid; China state patent documentation (application number: 03134575.1) reported " process of chlorogenic acid extracting from leaf of Acer Truncatum Buge ": adopt water cooking and extraction method, decocting in water alcohol deposition method, 70% ethanol reflux extraction usually; Water is put forward the lime precipitation extraction method; But above method all exists product content to hang down general character; Generally between 20%-25%, and extraction cost is high; The present invention is chlorogenic acid extracting from leaf of Acer Truncatum Buge, and adopts extract at low temperature, is adapting to control time and pH value, and under the conditions such as solid-liquid ratio, the soluble solids leaching rate is high, and is effective; Thereby the present invention have simple to operate, cost is low, no toxin, extraction ratio high, be applicable to industrial from leaf of Acer Truncatum Buge chlorogenic acid extracting; Chinese patent document (application number: 200510094347.8) reported the method for chlorogenic acid extracting and purifying " a kind of from sunflower meal ": sunflower meal is extracted with aquiferous ethanol; The chlorogenic acid ethanol water that obtains goes alcohol, acid precipitation to separate sunflower protein through concentrating; The reuse ethyl acetate solvent carries out liquid-liquid extraction, separation, concentrates and go ethyl acetate to obtain the chlorogenic acid bullion; Its purity is significantly improved; Content is brought up to about 70% from 17%, with the D101 macroporous resin chlorogenic acid bullion is further purified at last and obtains high-purity chlorogenic acid, and its purity has reached more than 92%; The Chinese patent document (application number: 200710049141.2) reported " being the method that raw material is produced chlorogenic acid, insecticide, antibacterial and Linesless charcoal with the Eupatorium cannabinum L. (Eupatorium coelestinum L.) ":: (1) is ground into granule with light violet stem Herba Lycopi; (2) the Eupatorium cannabinum L. (Eupatorium coelestinum L.) granule being put into container, to add concentration expressed in percentage by weight be that 95% ethanol soaked 1-3 days fully; (3) Eupatorium cannabinum L. (Eupatorium coelestinum L.) and the soak after will soaking together filters, and gets filtrate and puts into container; (4) the Eupatorium cannabinum L. (Eupatorium coelestinum L.) granule that filters out is put into dewaterer and dewater, reclaim dehydration liquid and mix in container with filtrate in the step (3), the dried slag that dewaters is for use; (5) mixed liquor is added thermal distillation and concentrate, make the moisture 18-22% of concentrated solution, distillate is for use; (6) concentrated solution is added the 10-30% that weight is concentrated solution, concentration expressed in percentage by weight is 99.5% ethyl acetate, at 5-6 hour after-filtration of 30-60 ℃ of insulation; (7) will filtrate distill the chlorogenic acid product; The Chinese patent document (application number: 200810244181.7) reported " method of extraction separation chlorogenic acid from Herba Solidaginis ": this method be with Herba Solidaginis complete handle after; Under ultrasonic or microwave action; With solvent raw material is carried out lixiviate; After solid-liquid separation, promptly get the chlorogenic acid crude extract, after resin absorption separates eluting, obtain the pure article of chlorogenic acid again; (application number: 200910147813.2) reported the industrial technology of rapid extraction high-purity chlorogenic acid " a kind of from Folium Ipomoea ": it is the scarlet potato blade that adopts moisture content about 80% to the Chinese patent document; Handle with hydrochloric acid solution (0.1mol/L HCl without any dry run; 20% ethanol) room temperature is extracted; Cross and filter extracting solution, extracting solution adds decolorizing with activated carbon and KLFC-150 macroporous resin adsorption, and eluent obtains the chlorogenic acid product through concentrating again.The main feature of this operating procedure is that raw material does not need dry directly use, the hydrochloric acid solution lixiviate, and energy consumption is little, and organic solvent uses few, Environmental Safety, production cost is low, and yield is high; The Chinese patent document (application number: 200710059981.7) reported " method of ferulic acid in the supersound extraction Radix Angelicae Sinensis ":: (1) the Radix Angelicae Sinensis rhizome is pulverized or pelletizing after, add adequate amount of ethanol solution; (2) Radix Angelicae Sinensis ultrasound-enhanced extraction under water-bath of step (1) being handled well; (3) extracting liquid filtering that step (2) is obtained, and decompression and solvent recovery are concentrated into the thick paste shape, obtain the ferulic acid extract.The inventive method is simple, extracts convenient, fastly, and extraction time is short, and extraction ratio can reach more than 6%, and the ferulaic acid content in the extract can reach more than 0.9%; Chinese patent document (application number: 200310123676.1) reported " new technique that improves extraction rate of ferulaic acid form in agricultural byproducts and the Chinese medicine ": reported enrichment from raw material of Chinese medicine such as agricultural byproducts such as bran coat, Testa Tritici and Radix Angelicae Sinensis, Rhizoma Chuanxiong, separation, extraction ferulic acid and the Technology that improves extraction rate of ferulaic acid form; The Chinese patent document (application number: 200810163603.8) reported " a kind of method for preparing of natural ferulaic acid ": from Testa oryzae, silverskin, Rice plumule the squeezing or the solvent extraction Testa oryzae oil after; From Testa oryzae oil, produce in the by-product that is commonly called as black foot behind the oryzanol and extract ferulic acid; Utilize soap to be dispersant; Under heating, pressurization, stirring condition, make the natural ferulaic acid bullion, again through centrifugal remove impurity, acid out, refining the pure article of ferulic acid.The explained hereafter cost of improvement is low, and without lower alcohol, according to content of ferulic acid meter in black foot, its yield can reach more than 75%, constant product quality in the technology.
But up to the present, Shang Weijian extracts the research report of Rhizoma Coptidis acid ingredients such as ferulic acid and chlorogenic acid from Rhizoma Coptidis and Rhizoma Coptidis fibrous root.
Summary of the invention
The object of the present invention is to provide a kind of acid ingredients such as ferulic acid and chlorogenic acid that from by-products such as Rhizoma Coptidis and Rhizoma Coptidis fibrous root, extract, it is a raw material with Rhizoma Coptidis or Rhizoma Coptidis or coptis plant, extraction Rhizoma Coptidis acid ingredient.
The present invention is a raw material with Rhizoma Coptidis or Rhizoma Coptidis or coptis plant; Adopt sulphuric acid or sulfurous acid or sodium sulfite solution soaking and extracting Rhizoma Coptidis acid ingredient, its process route is: raw material (Rhizoma Coptidis or Rhizoma Coptidis fibrous root or coptis plant)---pulverizes---adding an amount of 0.01～10% sulphuric acid (or sodium sulfite or sulfurous acid) a soaks---neutralization precipitation remove impurity---activated carbon decolorizing------bullion---ethanol or methanol extracting---the are reclaimed solvent---product that is evaporated near doing.Said method specifically comprises:
1), raw material is prepared
With Rhizoma Coptidis or Rhizoma Coptidis or coptis plant removal silt, pulverize or shredding (as not pulverizing or shredding), as the raw material of processing for Rhizoma Coptidis or coptis plant.
2), soak
Raw material is joined fermentation vat perhaps extract in the still, an amount of (3～20 times of volumes) concentration of adding is 0.01～10% sulphuric acid (or sulfurous acid or sodium sulfite) aqueous solution soaking, and the time is preferably 1～48 hour.
3), extract
After the immersion, be warmed up to 20～100 ℃, insulation was extracted 0.1～5 hour, extracted at least twice, was preferably four times; The used acid concentration lower (being lower than 1%) of last extraction; Heat up time of extracting when low is longer, and the extraction time of heating up when higher is shorter; If leaching process stirs or circulation, extraction effect is better.For the first time be used to produce product with extracting solution for the second time; Extracting solution is used for the soak of next group raw material for the third time, and soak is directly as primary extracting solution; After the 4th the suitable supplemental acid of extracting solution, be used for the extracting solution second time of next group raw material.Because immersion for the first time needs to consume a large amount of acid; What consume during second immersion is sour less; Basically consumption acids not during for the third time with the 4th soaking and extracting; For the third time with the 4th extracting solution in acid concentration do not change basically; Therefore the extracting solution soak (acid solution) that can be directly be used for raw materials such as next group Rhizoma Coptidis raw material or Rhizoma Coptidis fibrous root as " acid solution " uses for the third time, and the 4th time extracting solution can be used as the extracting solution second time (acid solution) use that acid solution is used to repair a collection of Rhizoma Coptidis or Rhizoma Coptidis fibrous root.
4), extracting solution neutralization precipitation
With the first time and extracting solution merging for the second time, using lime cream then is 4～8 to the pH of solution comprehensively, quiescent setting 3～48 hours.It is subsequent use that supernatant is told in filtration.Deposition abandons.
5), activated carbon decolorizing
Supernatant is with 0.1～10% active carbon, in room temperature～70 ℃ but stir decolouring 10～120 minutes down, filter, obtain destaining solution.
6), concentrating under reduced pressure
The destaining solution concentrating under reduced pressure, the extractum oven dry obtains bullion one time.
7), extracting
One time bullion fully stirs (or reflux, extract, or supersound extraction) 3～4 times with 5 times of amount ethanol or methanol, each 30 minutes, filters and obtains extracting solution.
8), production
The alcohol extract decompression and solvent recovery, the extractum oven dry obtains Rhizoma Coptidis acidic extraction thing finished product.Acid ingredient such as ferulic acid and chlorogenic acid total content is more than 30%.
The yield of Rhizoma Coptidis acid ingredient of the present invention is high, and technological process of the present invention is short, can produce the product of 30% above content, is fit to large-scale industrial production.
Product of the present invention (Rhizoma Coptidis acid ingredient) can be used as blood sugar lowering, antioxidation, antibiotic, anticancer.The crude drug of medicines such as beauty treatment also can be used as the usefulness of other products materials.
The present invention has the following advantages:
1., this Technology is raw material with Rhizoma Coptidis or Rhizoma Coptidis or Rhizoma Coptidis lime-ash etc., is raw material with by-products such as Rhizoma Coptidis fibrous root and Rhizoma Coptidis lime-ash especially, belongs to the comprehensive utilization of resources scope, low cost product, the course of processing is simple, is easy to preparation.
2., this Technology can obtain Rhizoma Coptidis acid ingredient products such as ferulic acid and the chlorogenic acid of content more than 30%, shortened the extraction flow process significantly, improved yield, greatly reduces cost.
The specific embodiment
Embodiment 1
1 kilogram of Rhizoma Coptidis is pulverized or section, adds 3 liter 10% sulfuric acid solution, soaks after 1 hour, is warmed up to 100 ℃ of reflux, extract, 0.1 hour, filters; The sulfuric acid solution that the residue reuse is 3 liter 10% is warmed up to 100 ℃ and extracts three times; Merge the first time and second extracting solution (extraction for the third time and the 4th extraction are used for the processing of next group raw material); Amalgamation liquid is with the neutralize pH=4 of solution of lime cream, and static layering 3 hours is filtered; The active carbon (w/v) of adding 10% in the supernatant stirs decolouring 10 minutes down for 70 ℃, filters, and obtains filtrating; Filtrate decompression is concentrated into dried, obtains a bullion (about 0.1 kilogram); Bullion is with the edible ethanol supersound extraction of 5 times of amounts three times, and each 30 minutes, filter, obtain extracting solution; Reclaim under reduced pressure ethanol, 50～70 ℃ of oven dry down of extractum promptly get product.Rhizoma Coptidis such as ferulic acid and chlorogenic acid acid ingredient total content 80%.
Embodiment 2
1 kilogram of Rhizoma Coptidis fibrous root adds 20 liter 0.01% sulfurous acid solution, soaks after 48 hours, filters; The sulfurous acid solution that the residue reuse is 5 liter 0.01% extracts three times; Merge the first time and second extracting solution (extraction for the third time and the 4th extraction are used for the processing of next group raw material); Amalgamation liquid is with the neutralize pH=8 of solution of lime cream, and static layering 12 hours is filtered; Stir decolouring 120 minutes in the supernatant under active carbon (w/v) room temperature of adding 0.1%, filter, obtain filtrating; Filtrate decompression is concentrated into dried, obtains a bullion (about 0.15 kilogram); Bullion is with the edible ethanol supersound extraction of 5 times of amounts three times, and each 30 minutes, filter, obtain extracting solution; Reclaim under reduced pressure ethanol, 50～70 ℃ of oven dry down of extractum promptly get product.Rhizoma Coptidis acid ingredient content 30%.
Embodiment 3
1 kilogram of leaf of Rhizoma Coptidis adds 10 liter 1% sodium sulfite solution, soaks after 12 hours, is warmed up to 50 ℃ of reflux, extract, 0.5 hour, filters; The sodium sulfite solution that the residue reuse is 5 liter 1% is warmed up to 50 ℃ and extracts three times; Merge the first time and second extracting solution (extraction for the third time and the 4th extraction are used for the processing of next group raw material); Amalgamation liquid is with the neutralize pH=6 of solution of lime cream, and static layering 6 hours is filtered; The active carbon (w/v) of adding 1% in the supernatant stirs decolouring 60 minutes down for 50 ℃, filters, and obtains filtrating; Filtrate decompression is concentrated into dried, obtains a bullion (about 0.1 kilogram); Bullion is with the edible ethanol supersound extraction of 5 times of amounts three times, and each 30 minutes, filter, obtain extracting solution; Reclaim under reduced pressure ethanol, 50～70 ℃ of oven dry down of extractum promptly get product.Rhizoma Coptidis acid ingredient content 50%.
Claims (2)
1. method of from Rhizoma Coptidis, extracting ferulic acid and chlorogenic acid acidic materials, it is to be raw material with Rhizoma Coptidis or Rhizoma Coptidis or coptis plant, employing sulphuric acid or sulfurous acid or sodium sulfite solution soaking and extracting Rhizoma Coptidis acid ingredient, said method comprises:
1), raw material is prepared
With Rhizoma Coptidis or Rhizoma Coptidis or coptis plant removal silt, if select for use Rhizoma Coptidis need pulverize or shredding, as the raw material of processing; Said coptis plant refers to leaf of Rhizoma Coptidis, Rhizoma Coptidis lime-ash, American lotus, said Rhizoma Coptidis lime-ash be in the coptis chinensis drying process or the decoction pieces production process in the fritter medical material leftover pieces that fall;
2), soak
The concentration that raw material is added 3～20 times of volumes is that 0.01～10% sulphuric acid or sulfurous acid or aqueous solution of sodium bisulfite soak; Soak time is 1～48 hour;
3), extract
After the immersion, be warmed up to 20～100 ℃, insulation was extracted 0.1～5 hour, extracted more than four times;
4), extracting solution neutralization precipitation
Will be for the first time merge with extracting solution for the second time, using the neutralize pH of solution of lime cream then is 4～8, and quiescent setting filters that to tell supernatant subsequent use, and deposition abandons;
5), activated carbon decolorizing
Supernatant is with 0.1～10% active carbon, ℃ stirs decolouring 10～120 minutes down in room temperature～70, filters, and obtains destaining solution;
6), concentrating under reduced pressure
The destaining solution concentrating under reduced pressure, the extractum oven dry obtains bullion one time;
7), extracting
Bullion filters and obtains extracting solution with ethanol or methanol fully stirring or reflux, extract, or supersound extraction;
8), production
The alcohol extract decompression and solvent recovery, the extractum oven dry obtains Rhizoma Coptidis acidic extraction thing finished product, and wherein ferulic acid and chlorogenic acid acid ingredient total content are more than 30%.
2. the method for from Rhizoma Coptidis, extracting ferulic acid and chlorogenic acid acidic materials according to claim 1, the extraction time that it is characterized in that said step 3) is four times; The used acid concentration of last extraction is lower than 1%; Heat up time of extracting when low is longer, and the extraction time of heating up when higher is shorter; For the first time be used to produce product with extracting solution for the second time; Extracting solution is used for the soak of next group raw material for the third time, and soak is directly as the primary extracting solution of next group raw material; After the 4th the extracting solution supplemental acid, be used for the extracting solution second time of next group raw material.
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| CN101269132A (en) * | 2008-05-14 | 2008-09-24 | 西南大学 | Coptis chinensis total alkaloid extracting technique |
| CN101429197A (en) * | 2008-12-17 | 2009-05-13 | 西南大学 | Extraction method for joint production of coptis chinensis with coptis chinensis fibrous root as raw material |
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| CN101269132A (en) * | 2008-05-14 | 2008-09-24 | 西南大学 | Coptis chinensis total alkaloid extracting technique |
| CN101429197A (en) * | 2008-12-17 | 2009-05-13 | 西南大学 | Extraction method for joint production of coptis chinensis with coptis chinensis fibrous root as raw material |
Non-Patent Citations (1)
| Title |
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| 匡艳辉等.黄连属药用植物化学成分和质量控制的研究进展.《中国药学杂志》.2008,第43卷(第15期),1121-1125. * |
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Application publication date: 20110216 Assignee: HUBEI XIANGLIAN PHARMACEUTICAL CO., LTD. Assignor: Southwest University Contract record no.: 2014420000167 Denomination of invention: Method for extracting ferulic acid, chlorogenic acid and other aicd components from coptis chinensis franch Granted publication date: 20120321 License type: Exclusive License Record date: 20140806 |
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