CN1931258B - Preparation process and use of loquat seed extract - Google Patents
Preparation process and use of loquat seed extract Download PDFInfo
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Abstract
The present invention is preparation process and use of loquat seed extract. The loquat seed extract with amygdalin, saponin and water soluble polysaccharide as main medicinal components is prepared with loquat seed as material and through extracting with organic solvent, filtering the extracted liquid, decompress concentrating the filtrate while recovering solvent and vacuum concentrating. The loquat seed extract has the functions of relieving cough, eliminating phlegm, diminishing inflammation, relieving asthma, lowering blood sugar and antagonizing virus and is prepared into orally taken preparation. The present invention has novel design, simple technological process, high extracting efficiency and low production cost.
Description
Technical field
The present invention relates to a kind of green chemical industry preparation method of from plant, extracting medicinal active ingredient, more specifically relate to a kind of preparation method and purposes of loquat seed extract.
Background technology
Folium Eriobotryae is the rare special product fruit of China subtropical zone for the Rosaceae Folium Eriobotryae belongs to [Eriobotrya japonica (Thunb.) Lindl.] plant.China is topmost in the world Folium Eriobotryae manufacturing country, cultivated area and output account for the whole world 2/3, its main producing region is the Putian, Fujian, Zhe Jiangtang is dwelt and mountain, Dongting Lake, Jiangsu, 354 of existing Folium Eriobotryae cultivars, and main high-yield variety be red No. 3 and No. 4, city etc. too of No. 6, clock, liberation clock, length early.
The Folium Eriobotryae of Putian, Fujian is " three Daxing assumed name fruits ", is important " name, excellent, the spy " fruit in Fujian Province.160,000 mu of the existing planting loquat areas in the whole city, account for global planting loquat area 1/6,1/4 and the Fujian Province in the whole nation 1/2.The planting loquat area of Putian, Fujian Chang Taizhen reaches 70,000 mu, be chosen as " the famous-brand and high-quality base of subtropical crop " by the Ministry of Agriculture, and being awarded the title in " Chinese Folium Eriobotryae first township ", the Folium Eriobotryae of production is awarded " pollution-free food ", " Fujian Province's famous brand agricultural product " and titles such as " original producton location marked products ".
As the seeds that " mountain area forestry comprehensive exploitation " project is given priority to, Folium Eriobotryae is one of the fastest economic tree of development in recent years, and national Fractus Eriobotryae gross annual output amount has reached 16～200,000 tons.The Folium Eriobotryae whole body is all precious, Radix Eriobotryae, flower, really, position such as nuclear contains compositions such as abundant volatile oil, amygdaloside, saponin, water soluble polysaccharide, triterpenic acid, water soluble polysaccharide and organic acid, mainly be to eat raw at present, except that eating raw, also part is processed into sweet can, preserved fruit, fruit jam etc., but do not carry out Radix Eriobotryae as yet, flower, really, the deep development and the comprehensive utilization at position such as nuclear.Loquat is nutritious, wet one's whistle, cough-relieving, be good for the stomach, effect such as heat clearing away, be described as health fruit, be subjected to the welcome of domestic and international consumer deeply.
The kernel part of Folium Eriobotryae karyonide rosaceous plant Folium Eriobotryae, has very high medical value, be rich in amygdaloside, free hydrogen cyanic acid, saponin, chlorogenic acid, polysaccharide, caffeic acid, little catechuic acid, little Fructus Citri tangerinae catechuic acid, ceryl alcohol, 4-methylene-DL-proline, anti--4-methylol proline, suitable-medicinal active ingredients such as 4-methylol proline, amygdaloside content is 1.64%, be about 39% of Semen Armeniacae Amarum, have effects such as tangible anti-cancer, analgesia, function [Chai Zhenlin etc. such as hydrocyanic acid has cough-relieving, relieving asthma, the Zhejiang forestry science and technology, 2003,23 (3): 30-32].
Japan once reported in 1996, and the amygdaloside composition that Radix Eriobotryae contains has antiinflammatory, antitumor and immunity effect effect [respecting one under gloomy, Japanese natural medical science, 1996,6:76-77].
Chinese medicine thinks that Radix Eriobotryae is as strengthening the body resistance Chinese medicine, and the antiinflammatory that it had, antitumor, immunity effect effect are regulated the antibody mediated immunity function based on forward.The modern pharmacology pharmacodynamic study shows that loquat seed extract has the non-specific phagocytic function that strengthens antibody, ability, T lymhocyte transformation rate and the NK cell killing activity [Li Ying etc., Chinese medicine information, 1999, (1): 51-52] that the B cell produces antibody.
The marrow of Chinese medicine " in healthy energy deposits; heresy can not be done "; promptly comprised normal flora (bacillus bifidus, lactobacillus, enterococcus, enterobacteria and bacteroid) and immunologic function to the protective effect of body, also comprised the facilitation of normal flora body's immunity.Loquat seed extract has dual regulation effect [Li Ying etc., Chinese microecology magazine, 2005,17 (4): 247-248] to immune function of mice and normal intestinal flora.
The nutritive value of Radix Eriobotryae is also higher, compositions such as rich in proteins, fat, vitamin, dietary fiber, carbohydrate and trace element, and Radix Eriobotryae carbohydrate total amount is 1.91 times of Semen Armeniacae Amarum, vitamin content and Semen Armeniacae Amarum are approaching.But because the Radix Eriobotryae amylose content is very high, the food mouthfeel of processing is poor, easy easily abdominal distention, indigestibility of " returning life ", food back, should not stir-fry and eat usefulness; Content of reducing sugar is also higher in the Radix Eriobotryae, easily produces brown stain in the course of processing, is not suitable for the processing beverage product.
Need it should be noted that the extremely toxic substance hydrocyanic acid that contains in the Radix Eriobotryae up to 0.04% especially, toxicity is bigger than Semen Armeniacae Amarum, and hydrocyanic acid is about 0.05g to people's lethal dose.Calculate that according to the total amount of amygdalin in eriobotrya japonia nut and free hydrogen cyanic acid the adult takes 10～15 of Radix Eriobotryaes, 5～7 of children's can cause death, reach 55, children's and reach 12～15 and just can cause death but the adult takes Semen Armeniacae Amarum.Therefore, Radix Eriobotryae being developed and utilized as direct raw-food material must be very prudent.
In China, the Folium Eriobotryae aboundresources, cheap and easy to get, drug effect is clear and definite, and among the people being widely used in food and the medicine is rare large natural medicinal plant resource.Usually, to account for fruit heavy by 10% for peaberry.But the annual whole nation has number all to give up with ten thousand tons Radix Eriobotryae and does not add utilization, has not only polluted environment, has also wasted valuable resource.Along with the Folium Eriobotryae industrialization constantly advances to the depth level, more and more seem important as the comprehensive development and utilization of the Radix Eriobotryae of industrialization important component part.For realizing the efficient utilization of resource and the sustainable development of production conscientiously, research is the preparation method of extract and the purposes of main medicinal ingredient with Radix Eriobotryae amygdaloside, saponin and water soluble polysaccharide, has certain directive significance for the comprehensive utilization and the series product development of Radix Eriobotryae.
The Radix Eriobotryae saponin is soluble in hot water, ethanol isopolarity solvent mainly based on oleanane type and ursane type pentacyclic triterpene.But Radix Eriobotryae saponin aglycon is then water insoluble, can only be dissolved in ethanol, methanol, acetone isopolarity aqueous solutions of organic solvent, therefore, adopts water extraction method the saponins compound in the Radix Eriobotryae can not to be extracted fully.
Radix Eriobotryae amygdaloside (Amygdalin, C
20H
27O
11) the cyanogen glycosides then formed by benzaldehyde, hydrocyanic acid and glucose, dissolve in ethanol, methanol, acetone and the water isopolarity solvent, be dissolved in fat-soluble organic solvents such as ether, normal hexane hardly.The dissolubility of amygdaloside in cold ethanol is very little, and dissolubility is very big in hot ethanol and boiling water.When adopting water extraction, easily by acid and enzyme institute catalyzing hydrolysis, the Alpha-hydroxy benzene acetonitrile aglycon that obtains is very unstable for amygdaloside, easily decomposes to generate benzaldehyde and hydrocyanic acid, thereby has reduced the yield of amygdaloside.
Because Radix Eriobotryae complex chemical composition, pure dissolubility medicinal active ingredients such as the saponin that is soluble in ethanol isopolarity organic solvent and amygdaloside had both been contained, also contain the impurity component such as protein, enzyme, polysaccharide, inorganic salt, organic acid, aminoacid, oligosaccharide of soluble in water or buffer, 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, though loquat-shell aqueous extract can tentatively satisfy tcm clinical practice medication demand, obtained clinical efficacy preferably, but owing to both contained main medicinal active ingredient such as Radix Eriobotryae saponin and amygdaloside in the loquat-shell aqueous extract, also contain impurity components such as amounts of protein, polysaccharide, quintessence oil, tannin, chlorophyll, inorganic salt and organic acid, the quality of product, content of drug effect components and clinical efficacy all have the space of further raising, and adopting the polar organic solvent aqueous solution to extract is a selection preferably.
Summary of the invention
One of purpose of the present invention is to provide a kind of preparation method of loquat seed extract, not only technology is simple, extraction efficiency is high for this preparation method, production cost is low, and the yield height of the Radix Eriobotryae amygdaloside, saponin and the water soluble polysaccharide that extract, can adapt to and satisfy modern Chinese medicine clinical application demand.
Two of purpose of the present invention is to provide a kind of loquat seed extract with preparation to be used to prepare to have cough-relieving clinically, reduces phlegm, relievings asthma, the purposes of the medicinal preparation for oral administration of antiinflammatory, antiviral or hypoglycemic activity, and described medicinal preparation for oral administration can be capsule, granule, tablet, oral liquid, syrup, microcapsule, powder, drop pill or pill etc.
The preparation method characteristic of loquat seed extract of the present invention is: be raw material with the Radix Eriobotryae, extracting with Radix Eriobotryae amygdaloside, saponin and water soluble polysaccharide with polar organic solvent is the extract of main medicinal ingredient, merge extractive liquid,, filter, filtrate decompression reclaims solvent, vacuum concentration becomes loquat seed extract.
Above-mentioned polar organic solvent can be one or more mixed solvents in methanol, ethanol, propanol, isopropyl alcohol, n-butyl alcohol or the acetone, preferentially selects methanol or acetone for use.Mainly the extraction effect based on methanol, ethanol, propanol, isopropyl alcohol, n-butyl alcohol or acetone isopolarity organic solvent is suitable for this, but for other polar organic solvent, the boiling point of methanol or acetone is lower, energy consumption is littler, can significantly reduce the preparation cost of product.
The major advantage of preparation method of the present invention is: made full use of the notable difference of impurity component dissolubility in the polar organic solvent aqueous solution such as Radix Eriobotryae amygdaloside, saponin and water soluble polysaccharide isoreactivity composition and protein, quintessence oil, inorganic salt, really reached the high efficiency separation of medicinal active ingredient such as Radix Eriobotryae amygdaloside, saponin and water soluble polysaccharide and impurity component.
The purposes that the present invention utilizes loquat seed extract to make medicinal preparation for oral administration has the following advantages: adopt modernization of Chinese medicine production technology to extract the Chinese medicine extract that the main medicinal active ingredient of Radix Eriobotryae is made the current international practice, " 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
The preparation method of the embodiment of the invention is: with bright Radix Eriobotryae or Radix Eriobotryae powder is raw material, adopt 30～65% polar organic solvent aqueous solution of 10～20 times of Radix Eriobotryae dry weights (W/W), under 50～80 ℃ of conditions, extract 1～3 time, each 1～3 hour, merge extractive liquid,, filter, filtrate-0.06～-0.09MPa, 50～65 ℃ of conditions under, become loquat seed extract through decompression and solvent recovery, vacuum concentration.
Above-mentioned polar organic solvent can be one or more mixed solvents in methanol, ethanol, propanol, isopropyl alcohol, n-butyl alcohol or the acetone, preferentially selects methanol or acetone for use.Mainly the extraction effect based on methanol, ethanol, propanol, isopropyl alcohol, n-butyl alcohol or acetone isopolarity organic solvent is suitable for this, but for other polar organic solvent, the boiling point of methanol or acetone is lower, energy consumption is littler, can significantly reduce the preparation cost of product.
Loquat seed extract of the present invention have be used to prepare cough-relieving, reduce phlegm, antiinflammatory, relieving asthma, the purposes of the medicinal preparation for oral administration of blood sugar lowering or antivirus action, described medicinal preparation for oral administration can be: capsule, granule, tablet, oral liquid, syrup, microcapsule, powder, drop pill or pill etc.
Foregoing invention adopts one of major advantage of one or more mixed solvents in methanol, ethanol, propanol, isopropyl alcohol, n-butyl alcohol or the acetone to be: the solubility property of methanol isopolarity organic solvent is good, penetration capacity to the Radix Eriobotryae plant cell is strong, easier being penetrated in the Radix Eriobotryae internal organizational structure improved the dissolution rate and the extraction efficiency of medicinal active ingredients such as Radix Eriobotryae amygdaloside, saponin and water soluble polysaccharide greatly.
Two of the major advantage of one or more mixed solvents in foregoing invention employing methanol, ethanol, propanol, isopropyl alcohol, n-butyl alcohol or the acetone is: the methanol isopolarity organic solvent extraction that adopts heat, can avoid in the leaching process amygdaloside to be become benzaldehyde and hydrocyanic acid with enzymatic hydrolysis, thereby improve the extraction efficiency and the yield of medicinal ingredient amygdaloside greatly by acid.
Foregoing invention adopts methanol, ethanol, propanol, isopropyl alcohol, three of the major advantage of one or more mixed solvents in n-butyl alcohol or the acetone is: methanol isopolarity organic solvent is to the Radix Eriobotryae amygdaloside, targeted activity such as saponin and water soluble polysaccharide solubility of substances is very big, and to protein, the dissolubility of impurity such as inorganic salt is less, can make amygdaloside, when saponin and water soluble polysaccharide isoreactivity composition are separated by selectivity from Radix Eriobotryae efficiently, greatly reduce protein in the extracting solution, quintessence oil, the content of impurity such as chlorophyll, be more conducive to follow-up further separation and purification and high-purity Radix Eriobotryae amygdaloside, the preparation of saponin and water soluble polysaccharide, significantly promote the quality and the added value of product, obviously increased the competitiveness of product in market.
The physical and chemical parameter assay method of each prepared product of the present invention is as follows:
(1) Radix Eriobotryae amygdaloside Determination on content: adopting high performance liquid chromatography, is contrast with the amygdaloside.Chromatographic condition: chromatographic column is selected Waters Nova-Pak C for use
18Post (Φ 3.9 * 15mm, 4 μ m), pre-column C
18(3.9mm * 15mm), UV-detector, mobile phase are methanol: 0.01% phosphate aqueous solution (20: 80), and flow velocity 1.0mL/min, 34 ℃ of column temperatures detect wavelength 215nm, sample size 20 μ L.
(2) mensuration of Radix Eriobotryae saponin content: adopting vanillin-concentrated sulphuric acid colorimetry, is contrast with the oleanolic acid.Get the sample liquid 1ml that dilutes suitable multiple, add the 0.5ml vanillin, add the 2.5ml concentrated sulphuric acid again, behind the reaction 10min, measure its absorbance down in the 580nm wavelength, with water as blank.
(3) Radix Eriobotryae water soluble polysaccharide Determination on content: adopting the phenolsulfuric acid method, is contrast with glucose or D-galactose.Sample solution is diluted to certain multiple, gets 1mL in test tube, moisturizing adds 1mL 6% phenol again to 2.0mL, add the 5mL concentrated sulphuric acid immediately, leave standstill 10min, shake up, room temperature is placed 20min, and 721 spectrophotometers are in 490nm place photometry density value, with water as blank.
(4) the Radix Eriobotryae gross protein adopts FoLin-phenol method to measure, and is contrast with the bSA.Water content adopts quick moisture test apparatus to measure.
After measured, the used Putian of the experiment content that produces main medicinal active ingredients such as amygdaloside, saponin and water soluble polysaccharide in the Radix Eriobotryae dry fruit (water content 2.3%) is respectively 16.8～22.3g/kg, 11.2～15.8g/kg and 102.7～176.2g/kg.
Medicinal preparation for oral administration preparation method of the present invention is as follows:
(1) the spray drying condition is: feeding liquid concentration 10～20 Baume degrees (60 ℃), 160～250 ℃ of PG-5 type spray dryer inlet temperatures, 60～110 ℃ of outlet temperatures, centrifugal head operating pressure 1.6～3.0kgf/cm
2
(2) capsule preparation: according to the formulation method of routine, select No. 1 hard capsule, the about 0.30g of the tolerant loadings of every intragranular, on the full-automatic hard capsule filler of NJP-1000B type, carry out the medicated powder filling, on the flat Autoblisterpackagingmachine of JPB-25 IIB type, carry out the aluminium foil blister package, can be made into clinical suitable Folium Eriobotryae fermented product oral capsule.
(3) drop pill preparation: according to the formulation method of routine, adjust the temperature control system of the general drop pill machine of TZDW-1 type, make the water dropper temperature remain on 50～85 ℃, the temperature of coolants such as liquid paraffin remains on-4～40 ℃; Get the glycerin gelatine of Folium Eriobotryae fermented product and 1～9 times of weight thereof, place heater, suspension is made in heating under stirring condition, be placed in the water dropper jar of drop pill machine, splash in the coolant by water dropper, the drop pill that will be shunk molding by the outlet of drop pill machine takes out, and removes the coolant on surface, is dried to the agent of Folium Eriobotryae fermented product oral administration dripping pill.
(4) granule preparation: according to the formulation method of routine, pelletize on SHK-220 type efficient wet mixer-granulator is packed on JXD-30A type granule automatic packaging machine, can be made into clinical suitable Folium Eriobotryae fermented product oral granular formulation.
The embodiment of preparation method of the present invention is presented below:
Embodiment 1
Producing Radix Eriobotryae with the Putian, Fujian Province is raw material, with the washing of bright Radix Eriobotryae, dry (air-dry, all can dry or dry), pulverize, cross 16～24 mesh sieves and get the Radix Eriobotryae powder, 3.0kg Radix Eriobotryae powder is put into extraction pot, 38% methanol aqueous solution with 10 times of weight of Radix Eriobotryae powder (W/W), under 63 ℃ of conditions, extract 3 times, each 2 hours, merge extractive liquid,, filter, filtrate through filtrate-0.06～-0.09MPa, 50～65 ℃ of conditions under, become loquat seed extract through decompression and solvent recovery, vacuum concentration.After measured, in the loquat seed extract of preparation, the extraction ratio of Radix Eriobotryae amygdaloside is 94.9%, and the extraction ratio of Radix Eriobotryae saponin is 82.3%, and the extraction ratio of Radix Eriobotryae water soluble polysaccharide is 76.9%.
Embodiment 2
16～24 order Radix Eriobotryae powder 2.5kg are put into extraction pot, 30% methanol aqueous solution with 20 times of weight of Radix Eriobotryae powder (W/W), under 50 ℃ of conditions, extract 2 times, each 3 hours, merge extractive liquid,, filter, filtrate through filtrate-0.06～-0.09MPa, 50～65 ℃ of conditions under, become loquat seed extract through decompression and solvent recovery, vacuum concentration.After measured, in the loquat seed extract of preparation, the extraction ratio of Radix Eriobotryae amygdaloside is 94.8%, and the extraction ratio of Radix Eriobotryae saponin is 81.9%, and the extraction ratio of Radix Eriobotryae water soluble polysaccharide is 76.1%.
Embodiment 3
16～24 order Radix Eriobotryae powder 2.5kg are put into extraction pot, 65% methanol aqueous solution with 17 times of weight of Radix Eriobotryae powder (W/W), reflux, extract, is 1 hour under 80 ℃ of conditions, filter, filtrate through filtrate-0.06～-0.09MPa, 50～65 ℃ of conditions under, become loquat seed extract through decompression and solvent recovery, vacuum concentration.After measured, in the loquat seed extract of preparation, the extraction ratio of Radix Eriobotryae amygdaloside is 91.6%, and the extraction ratio of Radix Eriobotryae saponin is 84.25%, and the extraction ratio of Radix Eriobotryae water soluble polysaccharide is 75.8%.
Embodiment 4
Producing Radix Eriobotryae with the Putian, Fujian Province is raw material, with the washing of bright Radix Eriobotryae, dry (air-dry, all can dry or dry), pulverize, cross 16～24 mesh sieves and get the Radix Eriobotryae powder, 3.0kg Radix Eriobotryae powder is put into extraction pot, 65% ethanol water with 20 times of weight of Radix Eriobotryae powder (W/W), under 80 ℃ of conditions, extracted 1 hour, filter, filtrate through filtrate-0.06～-0.09MPa, 50～65 ℃ of conditions under, become loquat seed extract through decompression and solvent recovery, vacuum concentration.After measured, in the loquat seed extract of preparation, the extraction ratio of Radix Eriobotryae amygdaloside is 92.8%, and the extraction ratio of Radix Eriobotryae saponin is 83.7%, and the extraction ratio of Radix Eriobotryae water soluble polysaccharide is 74.8%.
Embodiment 5
16～24 order Radix Eriobotryae powder 2.5kg are put into extraction pot, 52% ethanol water with 15 times of weight of Radix Eriobotryae powder (W/W), under 68 ℃ of conditions, extract 2 times, each 2 hours, merge extractive liquid,, filter, filtrate through filtrate-0.06～-0.09MPa, 50～65 ℃ of conditions under, become loquat seed extract through decompression and solvent recovery, vacuum concentration.After measured, in the loquat seed extract of preparation, the extraction ratio of Radix Eriobotryae saponin is 93.4%, and the extraction ratio of Radix Eriobotryae water soluble polysaccharide is 82.3%, and the extraction ratio of Radix Eriobotryae amygdaloside is 77.3%.
Embodiment 6
16～24 order Radix Eriobotryae powder 2.5kg are put into extraction pot, 30% ethanol water with 10 times of weight of Radix Eriobotryae powder (W/W), under 50 ℃ of conditions, extract 3 times, each 3 hours, merge extractive liquid,, filter, filtrate through filtrate-0.06～-0.09MPa, 50～65 ℃ of conditions under, become loquat seed extract through decompression and solvent recovery, vacuum concentration.After measured, in the loquat seed extract of preparation, the extraction ratio of Radix Eriobotryae amygdaloside is 93.9%, and the extraction ratio of Radix Eriobotryae saponin is 81.4%, and the extraction ratio of Radix Eriobotryae water soluble polysaccharide is 78.2%.
Embodiment 7
Producing Radix Eriobotryae with the Putian, Fujian Province is raw material, with the washing of bright Radix Eriobotryae, dry (air-dry, all can dry or dry), pulverize, cross 16～24 mesh sieves and get the Radix Eriobotryae powder, 3.0kg Radix Eriobotryae powder is put into extraction pot, 30% aqueous acetone solution with 14 times of weight of Radix Eriobotryae powder (W/W), under 50 ℃ of conditions, extract 3 times, each 3 hours, merge extractive liquid,, filter, filtrate through filtrate-0.06～-0.09MPa, 50～65 ℃ of conditions under, become loquat seed extract through decompression and solvent recovery, vacuum concentration.After measured, in the loquat seed extract of preparation, the extraction ratio of Radix Eriobotryae amygdaloside is 94.6%, and the extraction ratio of Radix Eriobotryae saponin is 80.1%, and the extraction ratio of Radix Eriobotryae water soluble polysaccharide is 79.3%.
Embodiment 8
16～24 order Radix Eriobotryae powder 2.5kg are put into extraction pot, 65% aqueous acetone solution with 10 times of weight of Radix Eriobotryae powder (W/W), reflux, extract, is 2 times under 80 ℃ of conditions, each 1 hour, merge extractive liquid,, filter, filtrate through filtrate-0.06～-0.09MPa, 50～65 ℃ of conditions under, become loquat seed extract through decompression and solvent recovery, vacuum concentration.After measured, in the loquat seed extract of preparation, the extraction ratio of Radix Eriobotryae amygdaloside is 93.1%, and the extraction ratio of Radix Eriobotryae saponin is 85.6%, and the extraction ratio of Radix Eriobotryae water soluble polysaccharide is 75.8%.
Embodiment 9
16～24 order Radix Eriobotryae powder 2.5kg are put into extraction pot, 47% aqueous acetone solution with 20 times of weight of Radix Eriobotryae powder (W/W), reflux, extract, is 2 hours under 75 ℃ of conditions, filter, filtrate through filtrate-0.06～-0.09MPa, 50～65 ℃ of conditions under, become loquat seed extract through decompression and solvent recovery, vacuum concentration.After measured, in the loquat seed extract of preparation, the extraction ratio of Radix Eriobotryae amygdaloside is 93.7%, and the extraction ratio of Radix Eriobotryae saponin is 82.4%, and the extraction ratio of Radix Eriobotryae water soluble polysaccharide is 75.2%.
Explanation about loquat seed extract purposes of the present invention
The loquat-shell aqueous extract of previous embodiment 1 preparation is carried out spray drying, make then have reduce phlegm, cough-relieving, relieving asthma, the oral granular formulation of inflammation-diminishing function.
Reduce phlegm, cough-relieving, relieving asthma, animal pharmacodynamics evaluation experimental such as antiinflammatory is described as follows.
1 material
(body weight 22 ± 2g) and normal feedstuff are available from Medical University Of Fujian's animal center for cleaning level male mice.Data are carried out with SPSS software, adopt Independent-Sample T Test method that each group data is carried out average, standard error calculating and significance test.
2 methods
(1) cough-relieving experiment
Adopt the strong aqua ammonia spraying to draw the method for coughing, mice is adapted to normal feedstuff raise random packet after 3 days, 10 every group, mice ad lib and drinking-water.Negative control group is given normal saline, positive controls is given codeine solution (0.125g/ml), the administration group gavages medicinal liquid (be equivalent to human dosage 50 times), each is organized dosage and is 0.4ml/ day, behind the gastric infusion 1h, mice is put into experimental provision, spray into the atomization gas of concentrated ammonia solution with the ultrasound medical nebulizer, spraying 40s, cough latent period of every mice and cough number of times in the record 5min, relatively t check between group.
(2) experiment of eliminating the phlegm
Adopt the phenol red expelling phlegm method of lumbar injection, mice is adapted to normal feedstuff raise random packet after 3 days, 10 every group, mice ad lib and drinking-water.Negative control group is given normal saline, and positive controls is given ammonium chloride solution (5.0g/ml), and the administration group gavages medicinal liquid (be equivalent to human dosage 50 times), each is organized dosage and is 0.4ml/ day, behind the gastric infusion 1h, and 0.6ml/ lumbar injection 0.25% phenol red solution, 30min post-tensioning cervical vertebra is put to death mice, separates trachea, inserts No. 7 syringe needle, 5% sodium bicarbonate flushing 3 times, each 0.5mL merges flushing liquor, with phenol red standard pipe colorimetric, increment rate is calculated in relatively t check between group.
(3) experiment of relievining asthma
Adopt the histamine spraying to cause the method for breathing heavily, mice is adapted to normal feedstuff raise random packet after 3 days, 10 every group, mice ad lib and drinking-water.Negative control group is given normal saline, positive controls is given aminophylline solution (0.5g/ml), the administration group gavages medicinal liquid (be equivalent to human dosage 50 times), each is organized dosage and is 0.4ml/ day, behind the gastric infusion 1h, mice is put into experimental provision, spray into the atomization gas of 2% acecoline and 0.1% histamine phosphate mixed in equal amounts solution with the ultrasound medical nebulizer, spraying 15s, the spraying certainly of every mice begins incubation period of twitching, rolling and reacting to animal in the record 6min, rate elongation is calculated in relatively t check between group.
(4) antiinflammatory experiment
Adopt the swollen method of caused by dimethylbenzene xylene, mice is adapted to normal feedstuff raise random packet after 3 days, 10 every group, mice ad lib and drinking-water.Control group administered physiological saline, positive controls is given hydrocortisone solution (0.375g/ml), the administration group gavages medicinal liquid (be equivalent to human dosage 50 times), each is organized dosage and is 0.4ml/ day, each organizes gastric infusion 1 time every day, and continuous 3 times, behind last administration 1h, with dimethylbenzene cotton balls contact mouse right ear 5s, 15min post-tensioning cervical vertebra is put to death mice respectively.With diameter 8mm card punch the mice ears are downcut with the position, measure left and right sides ear weight difference, relatively t check between group is calculated and is pressed down swollen rate.
3 reduce phlegm, cough-relieving, relieving asthma, animal pharmacodynamics experimental result such as antiinflammatory
The reducing phlegm of loquat seed extract, cough-relieving, relieving asthma, animal pharmacodynamics experimental result such as antiinflammatory is shown in table 1～table 4 respectively.From the result as seen, prepared loquat seed extract can prolong mice ammonia cause the cough number of times coughing incubation period and reduce mice, promote phenol red excretion, prolong animal roll reaction incubation period, suppress ear swelling due to the dimethylbenzene.
Result of study shows, the loquat seed extract of the present invention's preparation has certain cough-relieving, reduces phlegm, relievings asthma, inflammation-diminishing function.Can be developed further into the novel Chinese patent medicine or the natural health care of the treatment respiratory inflammation disease of high-efficiency low-toxicity.
(X ± SD) influences n=10 to table 1 loquat seed extract cough-relieving animal pharmacodynamics experimental result
| Group | Incubation period (s) | The cough number of times (inferior/5min) |
| Loquat seed extract codeine positive control normal saline negative control | 117.9±19.7 **138.5±12.3 ***75.3±10.8 | 20.1±5.2 * 13.4±5.6 ** 26.4±7.0 |
Compare with the normal saline negative control group
*: P＜0.05;
*: P＜0.01;
* *: P＜0.001.
Table 2 loquat seed extract reduces phlegm, and (X ± SD) influences n=10 to animal pharmacodynamics experimental result
| Group | Colorimetric | Increment rate (%) |
| Loquat seed extract ammonium chloride positive control normal saline negative control | 2.2±0.4 ***2.4±0.5 ***1.2±0.3 | 83.3 100.0 |
Compare with the normal saline negative control group
*: P＜0.05;
*: P＜0.01;
* *: P＜0.001.
Table 3 loquat seed extract is relievingd asthma, and (X ± SD) influences n=10 to animal pharmacodynamics experimental result
| Group | Incubation period (s) | Rate elongation (%) |
| Loquat seed extract aminophylline positive control normal saline negative control | 168.4±32.6 *202.5±29.5 **127.6±27.5 | 32.0 58.7 |
Compare with the normal saline negative control group
*: P＜0.05;
*: P＜0.01;
* *: P＜0.001.
(X ± SD) influences n=10 to table 4 loquat seed extract antiinflammatory animal pharmacodynamics experimental result
| Group | Swelling degree (%) | Press down swollen rate (%) |
| Loquat seed extract hydrocortisone positive control normal saline negative control | 24.6±8.7 *17.8±9.3 **34.6±9.8 | 28.9 48.9 |
Compare with the normal saline negative control group
*: P＜0.05;
*: P＜0.01;
* *: P＜0.001.
More than the part embodiment of the present invention of Chan Shuing is intended to describe in detail preparation method of the present invention, but is not limited thereto.
The present invention is not only novel, technology is simple, the extraction efficiency height, production cost is low, and utilize the kernel of Chinese large characteristic fruit Folium Eriobotryae, adopt modernization of Chinese medicine production technology to extract the Chinese medicine extract that the main medicinal active ingredient of Radix Eriobotryae is made the current international practice, " three-hypers ", " three is little " and advantages such as " three just " with modern Chinese medicine product, can adapt to and satisfy modern Chinese medicine clinical application demand, meet the modernization of Chinese medicine and international industrial policy that country advocates, have bigger dissemination.
Claims (5)
1. the preparation method of a loquat seed extract, it is characterized in that: be raw material with the Radix Eriobotryae, extracting with Radix Eriobotryae amygdaloside, saponin and water soluble polysaccharide with polar organic solvent is the extract of main medicinal ingredient, merge extractive liquid,, filter, filtrate becomes loquat seed extract through decompression and solvent recovery, vacuum concentration; Preparation process is: be raw material with the Radix Eriobotryae, adopt 30～65% polar organic solvent aqueous solution of the Radix Eriobotryae dry weight of 10～20 times of W/W, under 50～80 ℃ of conditions, extract 1～3 time, each 1～3 hour, merge extractive liquid,, filter, filtrate-0.06～-0.09MPa, 50～65 ℃ of conditions under, become loquat seed extract through decompression and solvent recovery, vacuum concentration; Described polar organic solvent is one or more mixed solvents in methanol, ethanol, propanol, isopropyl alcohol, n-butyl alcohol or the acetone.
2. the preparation method of a kind of loquat seed extract according to claim 1, it is characterized in that: described polar organic solvent is methanol or acetone.
The loquat seed extract that obtains of a loquat seed extract preparation method as claimed in claim 1 or 2 have cough-relieving in preparation, reduce phlegm, the application in antiinflammatory or the antiasthmatic effect medicinal preparation for oral administration.
4. application according to claim 3 is characterized in that: described medicinal preparation for oral administration is: capsule, granule, tablet, oral liquid, syrup, powder or pill.
5. application according to claim 3 is characterized in that: described medicinal preparation for oral administration is microcapsule or drop pill.
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| CN103127266A (en) * | 2011-11-29 | 2013-06-05 | 广西中医学院 | Loquat-shaped cake diuretic and extraction and preparation method thereof |
| CN104448015A (en) * | 2014-11-20 | 2015-03-25 | 四川旭华制药有限公司 | Method for ultrasonically extracting polysaccharide substance from loquat leaf |
| CN104490667B (en) * | 2014-12-04 | 2017-08-08 | 深圳市仙迪化妆品有限公司 | A kind of cosmetics containing the anti-skin ageing of loquat seed extract |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1557832A (en) * | 2004-02-06 | 2004-12-29 | 张绍良 | Peocess for extracting ursolic acid from flower of loquat |
| CN1640885A (en) * | 2004-01-08 | 2005-07-20 | 中国科学院上海药物研究所 | Loguat leaf total dehydrocamphenilic acid and its preparation method and use |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1640885A (en) * | 2004-01-08 | 2005-07-20 | 中国科学院上海药物研究所 | Loguat leaf total dehydrocamphenilic acid and its preparation method and use |
| CN1557832A (en) * | 2004-02-06 | 2004-12-29 | 张绍良 | Peocess for extracting ursolic acid from flower of loquat |
Non-Patent Citations (4)
| Title |
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| 京谷庄二郎.枇杷核提取物改善肝纤维化的作用（1）：引起肝损害的物质对改善肝纤维化作用的影响.国外医学中医中药分册26 2.2004,26(2),124. |
| 京谷庄二郎.枇杷核提取物改善肝纤维化的作用(1):引起肝损害的物质对改善肝纤维化作用的影响.国外医学中医中药分册26 2.2004,26(2),124. * |
| 李鹰等.枇杷核提取物对机体免疫功能影响的探讨.中医药信息 1.1999,(1),51-52. |
| 李鹰等.枇杷核提取物对机体免疫功能影响的探讨.中医药信息 1.1999,(1),51-52. * |
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