CN1943647A - The method for preparing triterpenic acid extract from the loquat leaves - Google Patents
The method for preparing triterpenic acid extract from the loquat leaves Download PDFInfo
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- CN1943647A CN1943647A CN 200610069441 CN200610069441A CN1943647A CN 1943647 A CN1943647 A CN 1943647A CN 200610069441 CN200610069441 CN 200610069441 CN 200610069441 A CN200610069441 A CN 200610069441A CN 1943647 A CN1943647 A CN 1943647A
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- loquat leaf
- triterpene acids
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Abstract
This invention can provide a method for preparing triterpenic acid extract from the loquat leaves. The characters of its preparing method: take loquat leaves. As raw material, distilling the triterpenic acid by using hydrophilic organic solvent, combine the distilled liquid, filter the combined liquid, retrieve the solvent through reducing pressure, then concentrate the solvent through vacuum so that the triterpenic acid extract will be achieved. The conception of this invention is novel, its technology is simple with high rate of distilling but low production costs, and the distilled extract has the strong points of 'three -high', 'three-small', and 'three-convenience', having comparatively large popularization.
Description
Technical field
The present invention relates to a kind of Green Chemistry production method of from plant, extracting medicinal active ingredient, more specifically relate to a kind of triterpene acids loquat leaf preparation method of extract.
Background technology
China is topmost in the world Folium Eriobotryae manufacturing country, and Folium Eriobotryae cultivated area and output account for more than 2/3 of the whole world, and its main producing region is the Putian, Fujian, Zhe Jiangtang is dwelt and mountain, Dongting Lake, Jiangsu.160,000 mu of the existing planting loquat areas in Putian, Fujian, account for the whole world 1/6,1/4 and the Fujian Province in the whole nation 1/2.
The Folium Eriobotryae whole body is all precious, Folium Eriobotryae, flower, really, position such as nuclear is rich in triterpenic acid, volatile oil, amygdaloside, saponin, flavone, water soluble polysaccharide and organic acid isoreactivity composition.At present, Folium Eriobotryae is based on fresh fruit supply, does not carry out the deep development and the comprehensive utilization at other position as yet.
In the Folium Eriobotryae producing region, Folium Eriobotryae, flower, examine these parts that have than high added value and be wasted basically, do not obtain due application.Usually do not influencing under the prerequisite that Fractus Eriobotryae produces can gather in year 50000 tons of Folium Eriobotryae dry products of the whole nation.Therefore, Folium Eriobotryae is carried out the deep development utilization, help promoting the sustainable sound development of Folium Eriobotryae industry,, improve the economic worth of Folium Eriobotryae, develop new product, have crucial social benefit and economic worth comprehensive utilization Folium Eriobotryae resource.
The leaf of Folium Eriobotryae leaf system rosaceous plant Folium Eriobotryae [Eriobotrya japonica (Thunb.) Lindl.], cold nature, the bitter in the mouth suffering, relieving cough and asthma, the lung heat clearing stomach function regulating, lowering the adverse-rising QI to resolve phlegm records in going through an edition Chinese Pharmacopoeia.The tradition tcm clinical practice often becomes compound medicines to be used as medicine with processed with honey Folium Eriobotryae or Folium Eriobotryae with other drug matching, has obtained certain preventing phlegm from forming and stopping coughing, antiinflammatory clinical efficacy such as relieving asthma.
Oleanolic acid extensively is present in about 60 section's 190 kind of plant with free form or glucosides form, in plants such as east area of the Liao River, coextensive with eastern and southern Liaoning Province Hu wood, Herba Swertiae Mileensis, Fructus Ligustri Lucidi, Folium Eriobotryae, Radix Hemsleyae Macrospermae.Ursolic acid then is distributed widely in about 27 section's 62 kind of plant with free form or glucosides form, in plants such as Fructus Crataegi, Folium Vaccinii vitis-idaeae, Fructus Mume, Herba Sambuci Chiensis, Herba Hedyotidis Diffusae, Folium Eriobotryae, Herba Plantaginis, Fructus Ligustri Lucidi.
Ursolic acid and oleanolic acid are two isomerss, and character is very similar, usually coexistence in plant.Because the complex structure of ursolic acid and oleanolic acid, the synthetic difficulty is all extracted in Chinese herbal medicine or plant both at home and abroad.Ursolic acid and oleanolic acid are white crystalline powder, and odorless is tasteless, are soluble in dioxane, pyridine, dissolve in methanol, ethanol, acetone isopolarity organic solvent, are slightly soluble in fat-soluble solvents such as chloroform, ether, and be water insoluble.
The modern pharmacology pharmacodynamic study shows that Folium Eriobotryae contains chemical constituents such as triterpenic acid, saponin, amygdaloside, flavone, tannin, vitamin.Wherein, triterpene acids loquat leaf is the pentacyclic triterpenoid based on ursolic acid and oleanolic acid, have effects such as antitumor, antioxidation, anti-hepatitis, antiinflammatory are antibacterial, blood fat reducing, antiulcer, especially the antitumor of triterpene acids loquat leaf, antioxidation, anti-hepatitis effect are remarkable, and toxicity is low, few side effects, clinical safe in utilization, be expected to develop become efficient, low toxicity have that preventing phlegm from forming and stopping coughing, antiinflammatory are relievingd asthma, the novel therapeutic medicine or the health food of antiviral, antitumor, anti-hepatitis function.
Because Folium Eriobotryae complex chemical composition, pure dissolubility medicinal active ingredients such as the ursolic acid that is soluble in ethanol isopolarity organic solvent and oleanolic acid had both been contained, also contain water-soluble biological small molecular weight impurities such as the water-soluble biological macromole impurity such as protein, enzyme, polysaccharide of soluble in water or buffer and inorganic salt, organic acid, aminoacid, oligosaccharide, even also contain oil-soluble impurities compositions such as the chlorophyll that is soluble in non-polar organic solvents such as petroleum ether, wax, oils and fats, natural gum, quintessence oil.Therefore, adopting hydrophilic organic solvent extraction with aqueous solution triterpene acids loquat leaf to be one selects preferably.
Summary of the invention
The object of the present invention is to provide a kind of triterpene acids loquat leaf preparation method of extract, not only technology is simple for this preparation method, extraction efficiency is high, and the yield height of the triterpene acids loquat leaf extract that extracts.
Triterpene acids loquat leaf preparation method of extract of the present invention is characterized in that: be raw material with the Folium Eriobotryae, adopt hydrophilic organic solvent, extract triterpene acids loquat leaf, merge extractive liquid, filters, and filtrate becomes the triterpene acids loquat leaf extract through decompression and solvent recovery, vacuum concentration.
Than existing extracting method, the present invention adopts hydrophilic organic solvent aqueous solutions such as methanol, ethanol, propanol, isopropyl alcohol or acetone, extracts ursolic acid or oleanolic acid compounds in the Folium Eriobotryae, makes the triterpene acids loquat leaf extract, and its advantage is:
The one, made full use of the difference of impurity component dissolubility in the hydrophilic organic solvent aqueous solution such as triterpene acids loquat leaf and protein, polysaccharide, quintessence oil, inorganic salt, really reached the high efficiency separation of triterpene acids loquat leaf and impurity component.
The 2nd, the solubility property of hydrophilic organic solvents such as methanol, acetone is good, and is strong to the penetration capacity of Folium Eriobotryae plant cell, and easier being penetrated in the Folium Eriobotryae internal organizational structure improved the dissolution rate and the extraction efficiency of triterpene acids loquat leaf greatly.
The 3rd, methanol, hydrophilic organic solvents such as acetone are very big to targeted activity solubility of substances such as triterpene acids loquat leaf, and to protein, polysaccharide, quintessence oil, the dissolubility of impurity such as inorganic salt is less, when triterpene acids loquat leaf isoreactivity composition is separated by selectivity from Folium Eriobotryae efficiently, greatly reduce protein in the extracting solution, polysaccharide, quintessence oil, the content of impurity such as chlorophyll, be more conducive to the preparation of follow-up further separation and purification and high-purity triterpene acids loquat leaf, significantly promote the quality and the added value of product, obviously increased the competitiveness of product in market.
The present invention preferentially selects for use the advantage of methanol or acetone to be: the extraction effect of hydrophilic solvents such as methanol, ethanol, propanol, isopropyl alcohol or acetone is suitable, but for other hydrophilic solvent, the boiling point of methanol or acetone is lower, energy consumption is littler, can significantly reduce the preparation cost of product.
The present invention is the Chinese medicine extract that main medicinal active ingredient such as ursolic acid or oleanolic acid compounds is made the current international practice in the employing modernization of Chinese medicine production technology extraction Folium Eriobotryae, " three-hypers ", " three is little " and advantages such as " three just " with modern Chinese medicine product, energy adapts to and satisfies modern Chinese medicine clinical application demand, meets the modernization of Chinese medicine and international industrial policy that country advocates.
The specific embodiment
Preparation method of the present invention is: be raw material with the Folium Eriobotryae, adopt the water content of 5～10 times of Folium Eriobotryae dry weights (W/W) to be no more than the hydrophilic organic solvent aqueous solution of 35% (W/W), under 50～80 ℃ of conditions, extract 1～3 time, each 1～3 hour, merge extractive liquid,, filter, filtrate-0.05～-0.09MPa, 50～70 ℃ of conditions under, become the triterpene acids loquat leaf extract through decompression and solvent recovery, vacuum concentration.
Above-mentioned hydrophilic organic solvent can be one or more mixed solvents in methanol, ethanol, propanol, isopropyl alcohol or the acetone, preferentially selects methanol or acetone for use.
Above-mentioned triterpene acids loquat leaf is one or more chemical compounds in ursolic acid compounds or the oleanolic acid compounds.
Physical and chemical parameter assay method of the present invention is as follows:
The content of triterpene acids loquat leaf adopts high performance liquid chromatograph to measure.Condition determination: Agilent 1100 type high performance liquid chromatographs (DAD diode array detector), Waters Nova-Pak C
18Chromatographic column (Φ 3.9 * 150mm, 5 μ m), mobile phase be methanol-0.2% phosphate aqueous solution (92: 8) (V/V), flow velocity 1.0mL/min, 34 ℃ of column temperatures, sample size 20 μ L detect wavelength and are respectively 220nm.Ursolic acid and oleanolic acid standard substance are purchased in Nat'l Pharmaceutical ﹠ Biological Products Control Institute.
After measured, testing the middle triterpene acids loquat leaf content of used Putian product Folium Eriobotryae (water content 3.5%) is 9.3～15.6g/kg.
The embodiment of preparation method of the present invention is presented below:
Embodiment 1
Producing Folium Eriobotryae with the Putian, Fujian is raw material, with the washing of bright Folium Eriobotryae, dry (air-dry, all can dry or dry), pulverize, cross 20～30 mesh sieves and get Loquat Leaf, the 2.6kg Loquat Leaf is put into extraction pot, methanol-acetone (1: 1) aqueous solution of 85% with 8 times of Loquat Leaf dry weights (W/W), reflux, extract, is 2 hours under 72 ℃ of conditions, filter, filtrate-0.05～-0.09MPa, 50～70 ℃ of conditions under, become the triterpene acids loquat leaf extract through decompression and solvent recovery, vacuum concentration.After measured, the triterpene acids loquat leaf extraction rate reached 96.3%.
Embodiment 2
20～30 order Loquat Leaf 2.8kg are put into extraction pot, 65% methanol aqueous solution with 10 times of Loquat Leaf dry weights (W/W), under 50 ℃ of conditions, extract 2 times, each 3 hours, merge extractive liquid,, filter, filtrate-0.05～-0.09MPa, 50～70 ℃ of conditions under, become the triterpene acids loquat leaf extract through decompression and solvent recovery, vacuum concentration.After measured, the triterpene acids loquat leaf extraction ratio 94.3%.
Embodiment 3
20～30 order Loquat Leaf 2.9kg are put into extraction pot, 100% methanol with 5 times of Loquat Leaf dry weights (W/W), reflux, extract, is 1 hour under 80 ℃ of conditions, filter, filtrate-0.05～-0.09MPa, 50～70 ℃ of conditions under, become the triterpene acids loquat leaf extract through decompression and solvent recovery, vacuum concentration.After measured, the triterpene acids loquat leaf extraction rate reached 95.8%.
Embodiment 4
Producing Folium Eriobotryae with the Putian, Fujian is raw material, with the washing of bright Folium Eriobotryae, dry (air-dry, all can dry or dry), pulverize, cross 20～30 mesh sieves and get Loquat Leaf, the 2.8kg Loquat Leaf is put into extraction pot, 95% ethanol water with 5 times of Loquat Leaf dry weights (W/W), under 80 ℃ of conditions, extract 2 times, each 1 hour, merge extractive liquid,, filter, filtrate-0.05～-0.09MPa, 50～70 ℃ of conditions under, become the triterpene acids loquat leaf extract through decompression and solvent recovery, vacuum concentration.After measured, the triterpene acids loquat leaf extraction rate reached 94.3%.
Embodiment 5
20～30 order Loquat Leaf 2.7kg are put into extraction pot, 78% methanol-isopropyl alcohol (2: 1) aqueous solution with 8 times of Loquat Leaf dry weights (W/W), under 76 ℃ of conditions, extract 2 times, each 2 hours, merge extractive liquid,, filter, filtrate-0.05～-0.09MPa, 50～70 ℃ of conditions under, become the triterpene acids loquat leaf extract through decompression and solvent recovery, vacuum concentration.After measured, the triterpene acids loquat leaf extraction rate reached 95.4%.
Embodiment 6
20～30 order Loquat Leaf 2.7kg are put into extraction pot, 65% ethanol water with 10 times of Loquat Leaf dry weights (W/W), under 50 ℃ of conditions, extract 3 times, each 3 hours, merge extractive liquid,, filter, filtrate-0.05～-0.09MPa, 50～70 ℃ of conditions under, become the triterpene acids loquat leaf extract through decompression and solvent recovery, vacuum concentration.After measured, the triterpene acids loquat leaf extraction ratio 93.7%%.
Embodiment 7
Producing Folium Eriobotryae with the Putian, Fujian is raw material, with the washing of bright Folium Eriobotryae, dry (air-dry, all can dry or dry), pulverize, cross 20～30 mesh sieves and get Loquat Leaf, the 2.6kg Loquat Leaf is put into extraction pot, 65% aqueous acetone solution with 10 times of Loquat Leaf dry weights (W/W), under 50 ℃ of conditions, extract 3 times, each 3 hours, merge extractive liquid,, filter, filtrate-0.05～-0.09MPa, 50～70 ℃ of conditions under, become the triterpene acids loquat leaf extract through decompression and solvent recovery, vacuum concentration.After measured, the triterpene acids loquat leaf extraction ratio is 94.8%.
Embodiment 8
20～30 order Loquat Leaf 2.8kg are put into extraction pot, 100% acetone with 5 times of Folium Eriobotryae powder dry weights (W/W), reflux, extract, is 1 hour under 80 ℃ of conditions, filter, filtrate-0.05～-0.09MPa, 50～70 ℃ of conditions under, become the triterpene acids loquat leaf extract through decompression and solvent recovery, vacuum concentration.After measured, the triterpene acids loquat leaf extraction rate reached 95.2%.
Embodiment 9
20～30 order Loquat Leaf 2.6kg are put into extraction pot, 84% methanol-ethanol (5: 3) aqueous solution with 9 times of Loquat Leaf dry weights (W/W), reflux, extract, is 2 hours under 80 ℃ of conditions, filter, filtrate-0.05～-0.09MPa, 50～70 ℃ of conditions under, become the triterpene acids loquat leaf extract through decompression and solvent recovery, vacuum concentration.After measured, the triterpene acids loquat leaf extraction ratio 96.6%.
Above embodiment is intended to further describe for example the present invention, rather than limits the present invention by any way.
The present invention is novel, and technology is simple, the extraction efficiency height, and production cost is low, has bigger dissemination.
Claims (7)
1. a triterpene acids loquat leaf preparation method of extract is characterized in that: be raw material with the Folium Eriobotryae, adopt hydrophilic organic solvent, extract triterpene acids loquat leaf, merge extractive liquid, filters, and filtrate becomes the triterpene acids loquat leaf extract through decompression and solvent recovery, vacuum concentration.
2. triterpene acids loquat leaf preparation method of extract according to claim 1, it is characterized in that: be raw material with the Folium Eriobotryae, adopt the water content of 5～10 times of Folium Eriobotryae dry weights (W/W) to be no more than the hydrophilic organic solvent aqueous solution of 35% (W/W), under 50～80 ℃ of conditions, extract 1～3 time, each 1～3 hour, merge extractive liquid, filtered, filtrate-0.05～-0.09MPa, 50～70 ℃ of conditions under, become the triterpene acids loquat leaf extract through decompression and solvent recovery, vacuum concentration.
3. triterpene acids loquat leaf preparation method of extract according to claim 1 and 2 is characterized in that: described hydrophilic organic solvent is one or more mixed solvents in methanol, ethanol, propanol, isopropyl alcohol or the acetone.
4. triterpene acids loquat leaf preparation method of extract according to claim 3 is characterized in that: hydrophilic organic solvent is preferentially selected methanol or acetone for use.
5. triterpene acids loquat leaf preparation method of extract according to claim 1 and 2 is characterized in that: described triterpene acids loquat leaf is one or more chemical compounds in ursolic acid compounds or the oleanolic acid compounds.
6. triterpene acids loquat leaf preparation method of extract according to claim 3 is characterized in that: described triterpene acids loquat leaf is one or more chemical compounds in ursolic acid compounds or the oleanolic acid compounds.
7. triterpene acids loquat leaf preparation method of extract according to claim 4 is characterized in that: described triterpene acids loquat leaf is one or more chemical compounds in ursolic acid compounds or the oleanolic acid compounds.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103705592A (en) * | 2013-01-07 | 2014-04-09 | 中国医学科学院药用植物研究所 | Folium eriobotryae extract extracted by ethanol and preparation and detection methods and application thereof |
| CN104147171A (en) * | 2014-08-28 | 2014-11-19 | 蒋君军 | Extraction method for triterpene acid component from herb residue of loquat leaf |
| CN109700029A (en) * | 2019-03-12 | 2019-05-03 | 苏州丰源宝农业科技有限公司 | A kind of loquat powder production processing and plasma sterilization technique |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100395258C (en) * | 2003-03-28 | 2008-06-18 | 中国医学科学院药用植物研究所 | Loquat leaf triterpene acid composition and its uses in preparation of medicine against inflammation and antitussive |
| CN1237973C (en) * | 2003-11-08 | 2006-01-25 | 余世春 | Chronic bronchitis treating traditional Chinese medicine |
| CN1315865C (en) * | 2004-01-08 | 2007-05-16 | 中国科学院上海药物研究所 | Loguat leaf total dehydrocamphenilic acid and its preparation method and use |
-
2006
- 2006-10-13 CN CN2006100694412A patent/CN1943647B/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103705592A (en) * | 2013-01-07 | 2014-04-09 | 中国医学科学院药用植物研究所 | Folium eriobotryae extract extracted by ethanol and preparation and detection methods and application thereof |
| CN104147171A (en) * | 2014-08-28 | 2014-11-19 | 蒋君军 | Extraction method for triterpene acid component from herb residue of loquat leaf |
| CN109700029A (en) * | 2019-03-12 | 2019-05-03 | 苏州丰源宝农业科技有限公司 | A kind of loquat powder production processing and plasma sterilization technique |
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| CN1943647B (en) | 2011-06-15 |
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