CN101073590A - Muxiang total lactone extract and its production - Google Patents
Muxiang total lactone extract and its production Download PDFInfo
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- CN101073590A CN101073590A CN 200710111228 CN200710111228A CN101073590A CN 101073590 A CN101073590 A CN 101073590A CN 200710111228 CN200710111228 CN 200710111228 CN 200710111228 A CN200710111228 A CN 200710111228A CN 101073590 A CN101073590 A CN 101073590A
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Abstract
The invention is concerned with the method of preparation of the lactone extract that distills from the Chinese tranditional medicine banksian rose. The extract mainly includes: bandsian roses hydrocarbon lactone, hydrogen removed banksian roses lactone, Effects vary dehydrogenase costas, dihydrodithiins banksian roses lactone, banksian roses olefin lactone, alpha-ring banksian roses olefin lactone, beta-ring banksian roses olefin lactone and other ramification. The method of extracting can be any one of the mehod as follow: solvent distilling, solvent extraction, and macropore polymeric adsorbent method, exceed critical flow extraction, column chromatography, and liquid-liquid countercurrent flow partition chromatography. The final banksian roses the lactone contents banksian roses hydrocarbon lactone and hydrogen removed banksian roses lactone with total assay value of 5-100% (w/w).
Description
Technical field
The invention belongs to medical technical field, be specifically related to a kind of total lactone extract of the Chinese medicine Radix Aucklandiae and preparation method, method of quality control and in the application of medicine and field of health care food.
Background technology
The Radix Aucklandiae is a conventional Chinese medicine, derives from the dry root of feverfew Radix Aucklandiae Aucklandia lappa Decne plant.Traditional Chinese medicine theory is thought Radix Aucklandiae nature and flavor suffering, hardship, temperature.Have the warming middle-JIAO to promote flow of QI pain relieving, the effect of strengthening the spleen to promote digestion intestinal stasis relieving cures mainly feeling of stuffiness in chest hypochondriac pain, abdominal distention, heavy after the dysentery, accumulation of food in the stomach and intes tine due to indigestion, vomiting is had loose bowels, colic of cold type stomachache, edema, cards such as beriberi, modern pharmacological research show that the Radix Aucklandiae has adjusting gastrointestinal tract, blood vessel dilating, blood pressure lowering, expansion bronchus, resisting pathogenic microbes, multiple efficacies such as blood sugar lowering.Wide clinical application is in treatment flatulence, infantile dyspepsia, acute gastroenteritis, chronic gastritis, gastrointestinal neurosis, cholecystitis, cholelithiasis, diseases such as acute lumbar muscle sprain.The Radix Aucklandiae mainly contains compositions such as lactone, volatile oil and alkaloids, and pharmacological research shows that total lactone composition is its main active.
Radix Aucklandiae total lactones is the lactone composition that extraction separation obtains from the Chinese medicine Radix Aucklandiae, and wherein main component is costunolide and dehydrocostuslactone etc.The pharmacologically active of relevant Radix Aucklandiae chemical constituent, application and preparation method, the invention disclosed patent has " extract of a kind of Radix Aucklandiae total lactones and its production and application " (application number 200410014854.1) at present, relates to the preparation method of total lactone composition in the Radix Aucklandiae.But the method for this patent disclosure system adopts alcohols solvent to extract, and the method for ethers, hydro carbons or esters organic solvent extraction prepares Radix Aucklandiae total lactones, is difficult to realize suitability for industrialized production.
Summary of the invention
The object of the present invention is to provide a kind of Muxiang total lactone extract.
Another object of the present invention is to provide a kind of preparation method of Muxiang total lactone extract.This method can the selective enrichment effective ingredient, removes impurity.This method has advantages such as good reproducibility, good stability, yield height, environmental protection, suitable suitability for industrialized production simultaneously.
A further object of the present invention is to provide the purposes of Radix Aucklandiae total lactones class extract health care aspect.
The Radix Aucklandiae of the present invention is whole plant or any position of feverfew Radix Aucklandiae Aucklandia lappa Decne and any one mutation plant thereof, RUGEN, rhizome, stem, leaf, spica, fruit etc., or commercially available Radix Aucklandiae decoction pieces.Wherein preferred medical material position is the dry root of these plants.The above-mentioned Radix Aucklandiae comprises crude drug and the decoction pieces of handling without any process of preparing Chinese medicine, also comprises various process of preparing Chinese medicine converted productss, as Radix Aucklandiae (roasted) etc.
Muxiang total lactone extract of the present invention, being meant that root after the drying peeling from the Radix Aucklandiae extracts obtains, comprise multiple lactone composition of active components, these lactone compositions mainly comprise costunolide, dehydrocostuslactone, different dehydrocostuslactone, dihydrocostulactone, costunolide, α-ring costunolide, β-ring costunolide and derivant thereof etc.
Among the various lactone active component that Muxiang total lactone extract of the present invention is contained, compositions such as costunolide, dehydrocostuslactone, dihydrocostulactone, costunolide most importantly.As Muxiang total lactone extract, the content of costunolide and two kinds of compositions of dehydrocostuslactone accounts for all 5～100% (w/w) of total lactone contents, wherein 50～100% (w/w) preferably.
Muxiang total lactone extract of the present invention, can with slaine such as some alkali such as sodium hydroxide, potassium hydroxide etc. and sodium salt, potassium salt, calcium salt, zinc salt such as sodium carbonate, potassium carbonate, calcium carbonate, sodium acetate, zinc acetate etc., form the metallic salt derivant.These derivants have pharmacologically active and the purposes identical or close with above-mentioned Muxiang total lactone extract.
Muxiang total lactone extract of the present invention can also form metal complex with metal ions such as ferrum, aluminum, zinc, copper, barium, chromium, strontiums.These metal complexs not only have pharmacologically active or the purposes identical or close with above-mentioned Muxiang total lactone extract, and have some new purposes.
The invention allows for the preparation technology of described Muxiang total lactone extract, it can adopt following any one method, or the combination in any of these methods is prepared: (1) solvent extraction method; (2) solvent extraction; (3) macroporous adsorbent resin method; (4) supercritical fluid extraction; (5) column chromatography; (6) liquid-liquid adverse current partography.Wherein preferable methods is the macroporous adsorbent resin method.
When these methods of use are prepared, generally comprise following step:
(1) extract: solvent for use can be water or any one alcohols, ketone and esters solvent, or the mixed solvent formed by a certain percentage of these solvents, or the acidity or the basic solvent that are made into by these solvents and acid, alkali, salt.Extracting method can be decoction, reflux, supersound extraction, merceration, percolation, microwave extraction, high pressure extract etc.
Preferred extraction process is: Radix Aucklandiae medical material adds 30～90% ethanol, and reflux, extract, 2～3 times was extracted 1～2 hour at every turn, and solvent load is 5～15 times of amounts (L/kg).
(2) filter: comprise methods such as centrifugal, sucking filtration, ultrafiltration, filter pressing, use or do not use following any one clarifier or its combination: the precipitate with ethanol agent, gelatin, Kaolin, various resins, Polyethylene Glycol, poly-second triol, chitosan and natural clarifying agent finished product are as 101 fruit juice clarifiers, ZTC+1 natural clarifying agent etc.
(3) concentrate: comprise thin film evaporation, rotary evaporation and decocting and concentrating etc. under normal pressure or the reduced pressure.
(4) drying: comprise vacuum drying, spray drying, lyophilization etc.
When adopting the macroporous adsorbent resin method to be prepared, used macroporous resin can be any one types such as nonpolar, low pole, middle polarity, alkalescence or faintly acid, as D101, D4020, HPD400, AB-8, S-8, HZ-806 etc., the resin of low pole or middle polarity preferably wherein is as AB-8, HPD400, D101 etc.Used eluant is water and aqueous ethanol, methanol, acetone etc., wherein 0～100% ethanol preferably.
Preferred Radix Aucklandiae extract resin purification technology is: select AB-8 for use, middle polarity such as HPD400 or low pole macroporous adsorbent resin are as the purification resin, Radix Aucklandiae ethanol extraction sample solution concentration 2～10mg/mL (in costunolide and dehydrocostuslactone total amount), absorption flow velocity 3～9BV/h, resin column blade diameter length ratio 1: 5～1: 10, applied sample amount is 30～80mg/mL (in costunolide and a dehydrocostuslactone total amount), 1～4 times of resin volume of 0～20% ethanol elution carries out remove impurity, the remove impurity flow velocity is 3～8BV/h, with 3～6 times of resin volumes of 40～90% ethanol elutions, elution flow rate is 5～9BV/h.
When adopting supercritical fluid extraction to be prepared, can directly extract Radix Aucklandiae raw material, also can the product that above-mentioned arbitrary method and step obtained be extracted.Can use or not use following any kind solvent and solvent mixture during extraction: water, alcohols, ketone and esters solvent.
When adopting column chromatography to be prepared, the object of its processing can be the product that the said extracted step is obtained, and also can be the product behind above-mentioned solvent extraction, macroporous adsorbent resin method or supercritical fluid extraction preliminary purification.Used immobile phase can be silica gel, polyamide, aluminium oxide, glucosan (Sephadex series or Sephadex LH-20 series), C-8, C-18, active carbon, cellulose etc., used eluent is different because of the difference of immobile phase, generally the mixed solvent of being made up of water, methanol, ethanol, acetone, chloroform, ethyl acetate, petroleum ether etc.
Liquid-when the liquid counter-current extraction was prepared, the object of its processing can be the product of said extracted step when adopting, and also can be the product behind above-mentioned solvent extraction, macroporous adsorbent resin method or supercritical fluid extraction preliminary purification.General earlier extract mixture being suspended from the water, then with low polar esters, alkanes or ether solvent (as petroleum ether, ether, hexane, gasoline, ethyl acetate etc.) extraction weeding of grease solubility impurity, use the solvent of suitable polarity then, as chloroform, ethyl acetate, acetone, n-butyl alcohol etc., or the mixture of these solvents, extraction obtains total lactone composition wherein, gets total lactone extract.
This extract can be pressed the arbitrary proportion compatibility separately or with other any Chinese and western drugs or food, be used to prepare medicine or functional food, prepared medicine or functional food can be capsule, tablet, pill, granule, oral liquid, syrup, electuary, medicated wine, injection, unguentum, powder, beverage etc.
Method of quality control of the present invention comprises the HPLC content assaying method of costunolide and dehydrocostuslactone:
Chromatographic condition: chromatographic column: Agilent Zorbax C
18Post (4.6mm * 150mm, 5 μ m); Mobile phase: water-acetonitrile (6: 4), flow velocity: 1.0mL/min; Detect wavelength: 225nm; Column temperature: room temperature.
Standard curve is drawn: accurate respectively absorption costunolide reference substance solution (concentration is 0.068 μ g/ μ L), dehydrocostuslactone reference substance solution (concentration is 0.055 μ g/ μ L) 0,2,4,6,8,10 μ L inject chromatograph of liquid, measure each chromatograph peak-to-peak area, (μ g) is abscissa with the reference substance sample size, the chromatographic peak peak area is a vertical coordinate, the drawing standard curve.
Assay: precision takes by weighing each 3 parts in 3 batches of Muxiang total lactone extract samples, and every part of about 13mg puts in the 10mL measuring bottle, adds 70% ethanol ultrasonic dissolution, and is diluted to scale, shakes up, as need testing solution.The above-mentioned need testing solution 10 μ L of accurate absorption inject chromatograph of liquid, measure each chromatograph peak-to-peak area, calculate content.
The specific embodiment
Embodiment 1: Muxiang total lactone extract preparation technology
Get Radix Aucklandiae decoction pieces 10kg, 70% ethanol 8L reflux, extract, 3 times, the each extraction 1 hour, decompression and solvent recovery, get extract, add the aqueous dispersion dissolving, making concentration of aqueous solution is 10mg/mL (in costunolide and dehydrocostuslactone total amount), with the centrifugal 30min of 3000 rev/mins rotating speed, get supernatant, by 5L AB-8 macroporous adsorbent resin, absorption flow velocity 2BV/h, the resin column blade diameter length ratio is 1: 8, applied sample amount is 75mg/mL (in costunolide and a dehydrocostuslactone total amount), and 3 times of resin volumes of 30% ethanol elution carry out remove impurity, and the remove impurity flow velocity is 2BV/h, 5 times of resin volumes of 90% ethanol elution, elution flow rate is 3.0BV/h, collects 90% ethanol elution, reclaims solvent, drying under reduced pressure is Muxiang total lactone extract.The content sum of costunolide and two kinds of compositions of dehydrocostuslactone is 68% in the mensuration Muxiang total lactone extract.
Embodiment 2: Muxiang total lactone extract preparation technology
Radix Aucklandiae decoction pieces 10kg, 50% ethanol 15L, reflux, extract, 3 times, the each extraction 1.5 hours, reclaim solvent, extract adds the aqueous dispersion dissolving, and making concentration of aqueous solution is 8.00mg/mL (in costunolide and dehydrocostuslactone amount), with the centrifugal 30min of 3000 rev/mins rotating speed, get supernatant, by 6L AB-8 macroporous adsorbent resin, absorption flow velocity 1.0mL/min, the resin column blade diameter length ratio is 1: 7, applied sample amount is 67.00mg/mL (in costunolide and a dehydrocostuslactone total amount), and 2 times of resin volumes of 10% ethanol elution carry out remove impurity, and the remove impurity flow velocity is 1.0mL/min, 4 times of resin volumes of 50% ethanol elution, elution flow rate is 2.0mL/min, collects 50% ethanol elution, reclaims solvent, drying under reduced pressure is Muxiang total lactone extract.The content sum of costunolide and two kinds of compositions of dehydrocostuslactone is 60% in the mensuration Muxiang total lactone extract.
Embodiment 3: Muxiang total lactone extract preparation technology
Radix Aucklandiae decoction pieces 10kg, 70% ethanol 12L reflux, extract, 2 times, the each extraction 2 hours, reclaim solvent, extract adds the aqueous dispersion dissolving, making concentration of aqueous solution is 9.00mg/mL (in costunolide and dehydrocostuslactone total amount), with the centrifugal 30min of 3000 rev/mins rotating speed, gets supernatant, by 7L AB-8 macroporous adsorbent resin, absorption flow velocity 1.0mL/min, the resin column blade diameter length ratio is 1: 9, applied sample amount is 65.00mg/mL (in costunolide and a dehydrocostuslactone total amount), 4 times of resin volumes of water elution carry out remove impurity, the remove impurity flow velocity is 1.0mL/min, 4 times of resin volumes of 90% ethanol elution, and elution flow rate is 2.0mL/min, collect 90% ethanol elution, reclaim solvent, drying under reduced pressure is Muxiang total lactone extract.The content sum of costunolide and two kinds of compositions of dehydrocostuslactone is 58% in the mensuration Muxiang total lactone extract.
Embodiment 4: Muxiang total lactone extract preparation technology
Radix Aucklandiae decoction pieces 10kg, 70% ethanol 12L reflux, extract, 2 times, the each extraction 2 hours reclaimed solvent, drying under reduced pressure, extract adds methanol and is extracted into colourless repeatedly, merge methanol extract liquid, decompression and solvent recovery gets the methanol extraction dry extract, add the aqueous dispersion dissolving, making sample solution concentration is 7.00mg/mL (in costunolide and dehydrocostuslactone total amount), by 7L AB-8 macroporous adsorbent resin, and absorption flow velocity 1.0mL/min, the resin column blade diameter length ratio is 1: 9, applied sample amount is 70mg/mL (in costunolide and a dehydrocostuslactone total amount), and 4 times of resin volumes of water elution carry out remove impurity, and the remove impurity flow velocity is 1.0mL/min, 4 times of resin volumes of 90% ethanol elution, elution flow rate is 2.0mL/min, collects 90% ethanol elution, reclaims solvent, drying under reduced pressure is Muxiang total lactone extract.The content sum of costunolide and two kinds of compositions of dehydrocostuslactone is 80% in the mensuration Muxiang total lactone extract.
Embodiment 5: the preparation of Radix Aucklandiae total lactones sheet
Muxiang total lactone extract 100g
Starch 100g
The said components mix homogeneously, it is an amount of to add Pulvis Talci, is pressed into 1000.
Embodiment 6: the preparation of Radix Aucklandiae total lactones compound preparation
Muxiang total lactone extract 50g
Rhizoma Coptidis alkaloid extract 50g
The said components mix homogeneously, in the hard gelatin capsule of packing into, totally 1000 capsules.
Claims (9)
1, a kind of Muxiang total lactone extract, it is characterized in that this extract obtains by extracting in the Chinese medicine Radix Aucklandiae, and contain following lactone composition: costunolide, dehydrocostuslactone, different dehydrocostuslactone, dihydrocostulactone, costunolide, a-ring costunolide, β-ring costunolide and derivant thereof etc.
2, Muxiang total lactone extract as claimed in claim 1, it is characterized in that the Radix Aucklandiae is whole plant or any position of feverfew Radix Aucklandiae Aucklandia lappa Decne and any one mutation plant thereof, RUGEN, rhizome, stem, leaf, spica, fruit etc., or commercially available Radix Aucklandiae decoction pieces, the above-mentioned Radix Aucklandiae comprises crude drug and the decoction pieces of handling without any process of preparing Chinese medicine, also comprise various process of preparing Chinese medicine converted productss, as Radix Aucklandiae (roasted) etc.
3, Muxiang total lactone extract as claimed in claim 1, the content sum that it is characterized in that costunolide, two kinds of compositions of dehydrocostuslactone is 5～100% by weight.
4, Muxiang total lactone extract as claimed in claim 1, it is characterized in that above-mentioned each lactone composition, also comprise metallic salt derivant that forms with slaines such as sodium salt, potassium salt, calcium salt, zinc salts and the metal complex that forms with metal ions such as ferrum, aluminum, zinc, copper, barium, chromium, strontiums.
5, as the described Muxiang total lactone extract of claim 1～4, it is characterized in that adopting solvent extraction method, solvent extraction, macroporous adsorbent resin method, supercritical extraction, column chromatography, liquid-any one methods such as liquid adverse current partography, or the combination in any of these methods is prepared.
6, Muxiang total lactone extract preparation method as claimed in claim 5 is characterized in that, when these methods of use are prepared, comprises following one or several step:
Extract: solvent for use can be water or any one alcohols, ketone and lipid solvent, or the mixed solvent formed by a certain percentage of these solvents, or the acidity or the basic solvent that are made into by these solvents and acid, alkali, salt; Extracting method can be decoction, reflux, supersound extraction, merceration, percolation, microwave extraction, high pressure extract etc.;
Filter: comprise methods such as centrifugal, sucking filtration, ultrafiltration, filter pressing, use or do not use following any clarifier or its combination: the precipitate with ethanol agent, gelatin, Kaolin, various resins, Polyethylene Glycol, poly-second triol, chitosan and natural clarifying agent finished product are as 101 fruit juice clarifiers, ZTC+1 natural clarifying agent etc.;
Concentrate: comprise thin film evaporation, rotary evaporation and decocting and concentrating etc. under normal pressure or the reduced pressure;
Dry: as to comprise vacuum drying, spray drying, lyophilization etc.
7, Muxiang total lactone extract preparation method as claimed in claim 5, it is characterized in that when using the macroporous adsorbent resin method, used macroporous resin can be any types such as nonpolar, low pole, middle polarity, alkalescence or faintly acid, as D101, D4020, HPD400, AB-8, S-8, HZ-806 etc., the resin of low pole or middle polarity preferably wherein, as AB-8, HPD400, D101 etc., used eluant is water and aqueous ethanol, methanol, acetone etc.
8, Muxiang total lactone extract preparation method as claimed in claim 7, it is characterized in that: select AB-8 for use, middle polarity such as HPD400 or low pole macroporous adsorbent resin are as the purification resin, Radix Aucklandiae ethanol extraction is in the sample solution concentration 0.1～0.4g/mL of Radix Aucklandiae crude drug amount, absorption flow velocity 3～9BV/h, resin column blade diameter length ratio 1: 5～1: 10, applied sample amount with total lactone is 5～10mg/mL, 1～4 times of resin volume of 0～20% ethanol elution carries out remove impurity, the remove impurity flow velocity is 3～8BV/h, with 3～6 times of resin volumes of 40～90% ethanol elutions, elution flow rate is 5～9BV/h.
9, as the application of claim 1,3,4 described extracts, it is characterized in that, this extract can be pressed the arbitrary proportion compatibility separately or with other any Chinese and western drugs or food, be used to prepare medicine or functional food, prepared medicine or functional food can be capsule, tablet, pill, granule, oral liquid, syrup, electuary, medicated wine, injection, unguentum, powder, beverage etc.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102133247A (en) * | 2011-01-28 | 2011-07-27 | 西南大学 | Costustoot extractive with blood sugar reduction activity and application thereof |
| CN103108620A (en) * | 2010-09-17 | 2013-05-15 | 株式会社芳珂 | Collagen production promoter, hyaluronic acid production promoter, and wrinkle diminishing agent |
| CN103159820A (en) * | 2012-12-13 | 2013-06-19 | 大兴安岭林格贝有机食品有限责任公司 | Method using microwave reverse flow technique to extract marsh marigold lactone in marsh marigold |
| CN104125835A (en) * | 2012-02-16 | 2014-10-29 | 草堂药品工业株式会社 | Method for extracting treatment ingredients for gastrointestinal disease from bark of liriodendron tulipifera |
| CN110038007A (en) * | 2018-12-29 | 2019-07-23 | 成都中医药大学 | A kind of composition with improvement acute gastric mucosal injury effect |
| CN117045563A (en) * | 2023-09-28 | 2023-11-14 | 云南英格生物技术有限公司 | Radix aucklandiae root extract and its preparation method and application |
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2007
- 2007-06-18 CN CN2007101112288A patent/CN101073590B/en active Active
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103108620A (en) * | 2010-09-17 | 2013-05-15 | 株式会社芳珂 | Collagen production promoter, hyaluronic acid production promoter, and wrinkle diminishing agent |
| CN103108620B (en) * | 2010-09-17 | 2014-09-03 | 株式会社芳珂 | Collagen production promoter, hyaluronic acid production promoter, and wrinkle diminishing agent |
| CN102133247A (en) * | 2011-01-28 | 2011-07-27 | 西南大学 | Costustoot extractive with blood sugar reduction activity and application thereof |
| CN102133247B (en) * | 2011-01-28 | 2013-03-13 | 西南大学 | Costustoot extractive with blood sugar reduction activity and application thereof |
| CN104125835A (en) * | 2012-02-16 | 2014-10-29 | 草堂药品工业株式会社 | Method for extracting treatment ingredients for gastrointestinal disease from bark of liriodendron tulipifera |
| CN103159820A (en) * | 2012-12-13 | 2013-06-19 | 大兴安岭林格贝有机食品有限责任公司 | Method using microwave reverse flow technique to extract marsh marigold lactone in marsh marigold |
| CN103159820B (en) * | 2012-12-13 | 2015-08-26 | 大兴安岭林格贝寒带生物科技股份有限公司 | A kind of method utilizing microwave counter current technology to extract kincup lactone in kincup |
| CN110038007A (en) * | 2018-12-29 | 2019-07-23 | 成都中医药大学 | A kind of composition with improvement acute gastric mucosal injury effect |
| CN117045563A (en) * | 2023-09-28 | 2023-11-14 | 云南英格生物技术有限公司 | Radix aucklandiae root extract and its preparation method and application |
| CN117045563B (en) * | 2023-09-28 | 2023-12-29 | 云南英格生物技术有限公司 | Radix aucklandiae root extract and its preparation method and application |
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