CN104116963A - Radix fici simplicissimae compound preparation for resisting oxidation and delaying senescence and preparation method of radix fici simplicissimae compound preparation - Google Patents
Radix fici simplicissimae compound preparation for resisting oxidation and delaying senescence and preparation method of radix fici simplicissimae compound preparation Download PDFInfo
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Abstract
The invention discloses a composition of compound radix fici simplicissimae. The composition is characterized by comprising the following substances in parts by weight: 15-50 parts of radix fici simplicissimae, 5-30 parts of Chinese-date, 5-30 parts of poria cocos, 0-20 parts of angelica sinensis and 5-30 parts of semen coicis, wherein the five traditional Chinese medicines can be medicinal materials, medicinal material powder, medicinal slices or extract combination. The invention also provides a preparation method and quality standard of extract thick paste of the compound radix fici simplicissimae. The preparation method comprises the following steps: extracting psoralen components of radix fici simplicissimae by using 95 percent of ethanol, adding the poria cocos, angelica sinensis, semen coicis and Chinese-date into the drug residues, adding water and extracting polysaccharide components. The compound extract is thick paste or powder, and the radix fici simplicissimae, poria cocos and Chinese-date are respectively and qualitatively identified by adopting thin-layer chromatography; and the psoralen in the radix fici simplicissimae is quantitatively analyzed by adopting high performance liquid chromatography. The thick paste can also be used for preparing common oral dosage forms, and the quality standard is applicable to quality control of multiple dosage forms. The composition provided by the invention has the effects of resisting oxidation and delaying senescence.
Description
Technical field
The present invention relates to take Herba Fici Simplicissimae as monarch drug, the compound vitex Radix Fici Hirtae prescription that Fructus Jujubae, Radix Angelicae Sinensis, Poria, Semen Coicis Chinese medicine of the five flavours form, and the preparation technology of compound recipe thick paste, quality standard and application thereof.
Background technology
Herba Fici Simplicissimae (Radix FiciHirtae) is the dry root of moraceae plants ficus simplicissima (Ficus hirta Vahl.), acrid in the mouth, sweet, and property is flat, has the effect of replenishing QI to invigorate the spleen tonifying the lung, dampness removing relaxing muscles and tendons, belongs to tonification class Chinese medicine.For south of the Five Ridges conventional Chinese medicine, have another name called milk wood, Herba Fici Simplicissimae, southern stilbene, Herba Ipomoeae Cairicae, five pawl Radix Fici Hirtaes etc.Its medicinal beginning is loaded in what standby > > that wants of the < < SHENGCAO property of medicine that gram remonstrates with of the Qing Dynasty, and gather medicinal herbs in the < < south of the Five Ridges of its < < Zhiwu Mingshi Tukao > >, Xiao Budan dredging of Wu thereafter, and to record > > etc. all on the books.Herba Fici Simplicissimae is again a kind of by the plant of the integration of edible and medicinal herbs of multi-national use, and among the people being called as " panacis quinquefolii radix " in Guangdong is also folklore very wide " Baoshang material ", and its applicating history is long, and health-care effect is widely approved.
Herba Fici Simplicissimae water extract has the effect that regulates immunologic function, anti-stress and enrich blood, and water extraction liquid contains polysaccharide composition.There is one of main active that bibliographical information proof psoralen is Herba Fici Simplicissimae, the psoralen that isolation identification goes out is furocoumarin compound, there is the effects such as antibacterial, antiviral, anticoagulation, inhibition tumor, immunomodulating, and erythroid hemopoietic is had to certain facilitation, and ethanol extraction method can effectively extract the compositions such as psoralen and bergapten.
Fructus Jujubae, has another name called Fructus Jujubae, dry Fructus Jujubae, Chinese date, originates from China, in the China's plantation of existing more than 8,000 year history, is just listed in since ancient times one of " five fruits " (chestnut, Fructus Persicae, Lee, Fructus Pruni, Fructus Jujubae).The nutritional labelings such as Fructus Jujubae rich in proteins, fat, saccharide, carotene, vitamin B group, vitamin C, Citrin and calcium, phosphorus, ferrum and cyclic adenosine monophosphate.Wherein ascorbic content comes out at the top in fruit, the laudatory title that has vitamin king, wherein, cyclic adenosine monophosphate, the essential composition of human body cell energy metabolism especially, can muscle strength reinforcing, allaying tiredness, blood vessel dilating, increase myocardial contraction, improve myocardial nutrition, control cardiovascular system diseases is had to good effect; Chinese medicine theory thinks, Fructus Jujubae has the effects such as tonify deficiency QI invigorating, nourishing blood to tranquillize the mind, invigorating the spleen and regulating the stomach, and Fructus Jujubae has good therapeutic effect to diseases such as chronic hepatitis, liver cirrhosis, anemia, anaphylactoid purpura; Fructus Jujubae contains triterpenoid compound and cyclic adenosine monophosphate, has stronger anticancer, anti-allergic effects.Fructus Jujubae can moisten cardiopulmonary, cough-relieving, tonifying five ZANG-organs, it is deficient to control, except the intestines and stomach addiction gas, can also regulating the spleen and stomach support spleen, flat gastric qi, logical nine orifices, help 12 through etc.In Fructus Jujubae, contain 50 number of chemical materials, contain polysaccharide, protein, fat, carbohydrate, vitamin A, B, B2, C, E, P, organic acid and comprise 36 kinds of trace element of selenium.Adopt extraction process by water, can effectively extract the compositions such as polysaccharide, water soluble vitamins.
Radix Angelicae Sinensis sweet in the mouth and weighing, therefore specially can enrich blood, its gas is light and pungent, thus again can promoting the circulation of blood, invigorating middle warmer has, in row, has benefit, is the key medicine in blood.Thereby it can be enriched blood, can invigorate blood circulation again, both can stimulate the menstrual flow, again can be active.Modern study shows: Radix Angelicae Sinensis has the effect of removing free radical; ferulic acid from Chinese angelica has lipoid peroxidization resistant, can directly eliminate free radical, inhibited oxidation reaction and radical reaction; and can be combined with biological film phospholipid, the infringement of protecting film lipid antagonism radical pair tissue.The effect of Radix Angelicae Sinensis aging resistance, Radix Angelicae Sinensis decoct has obvious impact to learning and memory of little mouse, by maze method, measures, Radix Angelicae Sinensis can improve the dementia due to aluminum chloride, reduce the Metabolism of Lipoprotein-cholesterol level of dementia mice brain, and the activity of Type B monoamine oxidation, senile dementia can be treated.
Poria, is the sclerotium of On Polyporaceae Poria, comes from < < Sheng Nong's herbal classic > >, is commonly called as Poria, Song Ling, Poria.Originate in the ground such as Yunnan, Anhui, Hubei, Henan, Sichuan.Ancients claim that Poria is " god medicine " at 4 o'clock, because its effect is very extensive, regardless of the four seasons, by it and various compatibility of drugs, no matter cold, temperature, wind, all diseases that wets can be brought into play its unique effects.Poria sweet in the mouth, light, property are flat, be used as medicine there is promoting diuresis to eliminate damp pathogen, the function of strengthening the spleen stomach function regulating, mind tranquilizing and the heart calming.
Poria energy enhancing human body immunity function, pachyman has obvious antitumor and protects the liver dirty effect.Also can be used as food materials use, have cake, Poria cocos congee, very nutritious, taste is gentle.Coordinate to boil waterly with the precious Ganoderma of fine jade, contribute to treat diabetes, tumor chronic diseases.
Semen Coicis is the grass Semen Coicis (dry mature kernal of Coix lacryma-jobi L.var.mayuen. (Roman.) Stapf.The provinces such as main product Hunan, Hebei, Jiangsu, Fujian.Sweet in the mouth, light, cold nature.There are invigorating spleen to remove dampness, clearing away heat and discharging pus function.For diseases such as diarrhea due to hypofunction of the spleen edema beriberi, leucorrhea, wet, arthralgia, acute appendicitis, consumptive lung diseases.Semen Coicis is one of traditional food resource of China, can make medicated porridge, meal, various wheaten food edible for people.Especially more suitable to the old and the weak patient.Its main component comprises the compositions such as lipid, unsaturated fatty acid, saccharide, and Semen Coicis saccharide contains rhamnose, arabinose, mannose, galactose and glucose.Its water extract has hypoglycemic activity to mice, and its active component is three kinds of polysaccharide.
Therefore, in this prescription, with the Chinese medicine of the five flavours of integration of edible and medicinal herbs, form, Herba Fici Simplicissimae is monarch drug, replenishing QI to invigorate the spleen tonifying the lung, and qi invigorating functions is obvious, and Fructus Jujubae, when being classified as ministerial drug has the effect of tonify deficiency QI invigorating, nourishing blood to tranquillize the mind, invigorating the spleen and regulating the stomach, and nourishing blood function is remarkable; Poria, Semen Coicis, be adjuvant drug, amounts to the drying damp and strengthening spleen effect of QI invigorating, is applicable to insufficiency of vital energy and blood, spleen and loses the disease due to operation, dampness retardance.
The present invention has compared single Herba Fici Simplicissimae and the effect of compound recipe aspect antioxidation, slow down aging, and result shows that compound recipe effect is better than single medical material, the synergism of prompting compound Chinese medicinal preparation.
The present invention adopts alcohol extracting method to extract the psoralen constituents in Herba Fici Simplicissimae, and medicinal residues adopt extraction process by water to extract polysaccharide composition with other a few taste medical materials again, better bring into play the benefiting action of polysaccharide composition.The present invention adopts thin layer chromatography to carry out qualitative identification to three taste medical materials in compound recipe, adopts high performance liquid chromatography to carry out assay to the Coumarins composition of monarch drug Herba Fici Simplicissimae, thereby has guaranteed the controllability of large production technology, the stability of end product quality.
Summary of the invention
Primary and foremost purpose of the present invention is to provide a kind of Chinese medicine composition being comprised of Chinese medicine of the five flavours, and it has the effect of resisting oxidation and delaying senility.
Another object of the present invention is to provide a kind of preparation method and quality standard of compound vitex Radix Fici Hirtae compositions thick paste, and the application in oral formulations.
Object of the present invention realizes in the following manner:
1, compound vitex Radix Fici Hirtae prescription
Herba Fici Simplicissimae: 15-50; Fructus Jujubae: 5-30; Poria: 5-30; Radix Angelicae Sinensis: 0-20; Semen Coicis: 5-30.
2, the preparation method of compound vitex Radix Fici Hirtae thick paste
Gomi herbs in step 1, prescription cleans or concocts by pertinent regulations under each medicine item of < < Chinese Pharmacopoeia > > version in 2010, standby.Herba Fici Simplicissimae cleans.
Step 2, get the dry medical material of Herba Fici Simplicissimae and be ground into coarse powder, measure after 95% soak with ethanol 1h condensing reflux 2h, while hot leaching medicinal liquid with 10 times; Add again 8 times of amount 95% alcohol reflux 1h, merge twice filtrate, be evaporated to thick paste standby.Retain medicinal residues, for decocting together with other four Chinese medicine material.
Step 3, three taste pulverizing medicinal materials except Fructus Jujubae are become to coarse powder, Fructus Jujubae directly adds, and the medicinal residues that retain with previous step merge, and decoct with water secondary, and 3 hours for the first time, 12 times of water gagings; 2 hours for the second time, 10 times of water gagings.
Step 4, collecting decoction, filter, and filtrate decompression is concentrated into the thick paste that relative density is 1.30～1.35 (80 ℃).
3, the quality standard of compound vitex Radix Fici Hirtae thick paste
(1) thin layer chromatography is differentiated the contained psoralen of Herba Fici Simplicissimae in Chinese medicine composition:
Precision takes thick paste 3g, adds ethyl acetate 50mL, and ultrasonic 25min filters, and filtrate is concentrated into dry, adds ethyl acetate 2mL in 2mL measuring bottle, as need testing solution.Separately get Herba Fici Simplicissimae control medicinal material 5g, be made in the same way of control medicinal material solution.Separately get psoralen reference substance, add ethyl acetate and dissolve, make every 1mL containing the solution of 2mg, in contrast product solution.According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2010), test, draw each 3 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, normal hexane-chloroform-acetic acid second is cruel-formic acid (20: 4: 5: 0.7) launch after saturated 10 minutes, while launching forward position to 1cm left and right, lamellae edge, take out, dry, put under ultra-violet lamp (365nm) and inspect.In test sample chromatograph, with the corresponding position of reference substance chromatograph on, the fluorescence speckle of aobvious same color.Spray again with 10% ethanol solution of sulfuric acid, be placed in the colour developing of 105 ℃ of baking ovens be heated to clear spot with the corresponding position of control medicinal material chromatograph on, (see Figure of description 1 and accompanying drawing 2, number in the figure 1 is psoralen standard substance to the principal spot of aobvious same color; 2 is that medical material reference substance, 3 is thick paste sample a; 4 is thick paste sample b; 5 is thick paste sample c; 6 negative reference substances).
(2) thin layer chromatography is differentiated the Poria in Chinese medicine composition:
Precision takes thick paste 1g, adds acetone 100mL reflux, extract, 1 hour, filters, and gets filtrate water-bath and is concentrated into about 0.5mL, as need testing solution.Separately get Poria control medicinal material 1g, add acetone 20mL reflux, extract, 1 hour, filter, filtrate is concentrated into about 0.5mL, in contrast medical material solution.According to thin layer chromatography (appendix VI B of Chinese Pharmacopoeia version in 2010), test, draw each 15-20 μ L of above-mentioned two kinds of solution, put respectively in same and take on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is adhesive, petroleum ether (60-90 ℃)-ether (1: 1) of take is developing solvent, launch, take out, dry, spray, with 10% phosphomolybdic acid ethanol solution, is heated to speckle colour developing at 100 ℃ clear.In test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, (see Figure of description 3, number in the figure 1 is medical material reference substance to the speckle of aobvious same color; 2 is that thick paste sample a, 3 is thick paste sample b; 4 is thick paste sample c; 6 negative reference substances).
(3) thin layer chromatography is differentiated the Fructus Jujubae in Chinese medicine composition:
Precision takes thick paste 1g, adds water 40mL and makes to dissolve, and filters, and gets the n-butanol extraction 2 times that filtrate water is saturated, each 20mL, merges n-butyl alcohol liquid, with n-butyl alcohol saturation water washing 2 times, and each 20mL, divide and get n-butyl alcohol liquid evaporate to dryness, residue adds 1mL methanol to be made to dissolve, as need testing solution.Separately get Fructus Jujubae control medicinal material 2g, decoct with water 1 hour, filter, filtrate is concentrated into 20mL, is made in the same way of control medicinal material solution.According to thin layer chromatography (appendix VI B of Chinese Pharmacopoeia version in 2010), test, draw each 5 μ L of above-mentioned two kinds of solution, put respectively in same and take on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is adhesive, n-butyl alcohol-glacial acetic acid-the water (3: 1: 0.5) of take is developing solvent, launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to speckle colour developing at 100 ℃ clear.In test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, (see Figure of description 4, number in the figure 1 is medical material reference substance to an aobvious identical brown speckle; 2 is that thick paste sample a, 3 is thick paste sample b; 4 is thick paste sample c; 6 negative reference substances).
(4) content of the contained psoralen of Herba Fici Simplicissimae in high effective liquid chromatography for measuring Chinese medicine composition:
Liquid phase chromatogram condition: adopt the chromatographic column that octadecylsilane chemically bonded silica is filler, mobile phase is methanol and water (60: 40), and detection wavelength is 254nm, and flow velocity is 1mL/min, and temperature is 30 ℃, and sample size is 10 μ L.
The preparation of reference substance solution: precision takes in psoralen reference substance 2.0mg to 10mL volumetric flask, adds the about 5mL of methanol, slight fever is dissolved, and cooling room temperature adds methanol dilution scale, shakes up.Accurate absorption in dense storing solution 2mL to 10mL volumetric flask, adds methanol dilution scale, shakes up and adds methanol dilution scale, shakes up, and with 0.25 μ m filtering with microporous membrane, obtains reference substance solution (concentration: 0.04mg/mL).
The preparation of sample solution: precision takes thick paste 0.5g, accurately weighed, puts in tool plug conical flask, precision adds methanol 100mL, accurately weighed weight, supersound extraction 40min, let cool, more weighed weight, with methanol, supply the weight of less loss, shake up, filter, discard just filtrate, get subsequent filtrate, with 0.25 μ m filtering with microporous membrane, standby as sample solution.
Accompanying drawing explanation
Fig. 1 is the thin-layer chromatogram of Herba Fici Simplicissimae under 365nm ultraviolet light
Fig. 2 is that Herba Fici Simplicissimae adopts the thin-layer chromatogram after 10% sulphuric acid ethanol colour developing
Fig. 3 is the thin-layer chromatogram of Poria
Fig. 4 is the thin-layer chromatogram of Fructus Jujubae
Fig. 5 is the chromatogram of reference substance psoralen under 254nm wavelength
Fig. 6 is the Herba Fici Simplicissimae medical material thick paste sample chromatogram figure of water extraction under 254nm wavelength
Fig. 7 is the Herba Fici Simplicissimae medical material thick paste sample chromatogram figure of alcohol extraction under 254nm wavelength
Fig. 8 is the thick paste sample chromatogram figure of compound vitex Radix Fici Hirtae under 254nm wavelength
The specific embodiment
Embodiment 1: Herba Fici Simplicissimae medicinal material extract technical study
The preparation of 1.1 Herba Fici Simplicissimae medical material water extraction thick pastes and alcohol extraction thick paste
The preparation method of Herba Fici Simplicissimae water thick paste: take Herba Fici Simplicissimae medical material 200g, with after 10 times of amounts (M/V) distilled water immersion 1h, heated and boiled 1h, while hot leaching medicinal liquid; Add again 8 times of water gagings, boil 30min, merge twice filtrate, be concentrated into thick paste standby (relative density is 1.30～1.35 (80 ℃)).
The preparation method of Herba Fici Simplicissimae alcohol thick paste: take the dry medical material 200g of Herba Fici Simplicissimae, with after 10 times of amount 95% soak with ethanol 1h, heating and refluxing extraction 2h, while hot leaching medicinal liquid; Medicinal residues add 8 times of amount 95% alcohol reflux 1h again, merge twice filtrate, with Rotary Evaporators, are evaporated to thick paste standby (relative density is 1.30～1.35 (80 ℃)).
The assay of psoralen in 1.2 two kinds of thick pastes
Adopt high effective liquid chromatography for measuring, chromatographic condition: adopt the chromatographic column that octadecylsilane chemically bonded silica is filler, mobile phase is methanol and water (60: 40), detection wavelength is 254nm, flow velocity is 1mL/min, and temperature is 30 ℃, and sample size is 10 μ L.
The preparation of reference substance solution: precision takes in psoralen reference substance 2.0mg to 10mL volumetric flask, adds the about 5mL of methanol, slight fever is dissolved, and cooling room temperature adds methanol dilution scale, shakes up.Accurate absorption in dense storing solution 2mL to 10mL volumetric flask, adds methanol dilution scale, shakes up and adds methanol dilution scale, shakes up, and with 0.22 μ m filtering with microporous membrane, obtains reference substance solution (concentration: 0.04mg/mL).
The preparation of sample solution: precision takes water extraction thick paste, each 0.5g of alcohol extraction thick paste respectively, accurately weighed, puts respectively in tool plug conical flask, precision adds methanol 100mL, accurately weighed weight, supersound extraction 40min, let cool, more weighed weight, with methanol, supply the weight of less loss, shake up, filter, discard just filtrate, get subsequent filtrate, with 0.22 μ m filtering with microporous membrane, standby as sample solution.
In two kinds of thick pastes, the assay of psoralen the results are shown in Table the extraction ratio that 1. employing one point external standard methods calculate psoralen in medical material, and result shows with a collection of medical material, adopts 95% alcohol reflux, and the extraction ratio of effective ingredient psoralen is higher than the thick paste of water extraction.
The different extraction process psoralen of table 1 Herba Fici Simplicissimae content results
The assay of polysaccharide composition in 1.3 two kinds of thick pastes
In thick paste prepared by employing ultraviolet spectrophotometry detection Different Extraction Method, the content of polysaccharide composition.
Standard curve test: precision takes glucose (105 ℃ of dry 3h) 15mg and puts in 25mL volumetric flask, and adding distil water is to scale, and being made into concentration is the dextrose standard sample solution of 0.6mg/mL.The above-mentioned solution 0.5,1.2,1.9,2.6 of accurate absorption, 3.3mL put respectively in 25mL volumetric flask, add water to respectively scale, pipette respectively again 2mL and put in 10mL volumetric flask, then add 4% phenol solution 1mL, shake up the rear 7mL concentrated sulphuric acid that adds rapidly, after shaking up, in 40 ℃ of water-baths, be incubated 30min, take out, put 5min in ice-water bath, take out, shake up rear standing 10min, at 490nm, survey trap.The results are shown in Table 2, take absorbance as vertical coordinate, the concentration (μ g/mL) of take is abscissa, carries out linear regression, obtains regression equation and is: y=0.0383x+0.1096 (R
2=0.9995), show that concentration is between 2.40-15.84 μ g/mL, good with trap dependency.
Table 2 standard curve result
The preparation of sample: precision takes water extraction thick paste 2g, adds respectively 80% ethanol 50mL, and ultrasonic 5-10min makes the complete suspendible of thick paste, and lucifuge standing over night is filtered, and it is dry that filtering residue is put infrared drying oven, after being dried, weighs weight.Add again suitable quantity of water heating for dissolving, standardize solution is put in 50mL volumetric flask, then draws 0.5mL standardize solution and put in 25mL volumetric flask, draws 2mL and puts in 10mL volumetric flask, then add people 4% phenol solution 1mL, shake up the rear people 7mL concentrated sulphuric acid that adds rapidly, after shaking up, in 40 ℃ of water-baths, be incubated 30min, take out, put 5min in ice-water bath, take out, shake up rear standing 10min, at 490nm, survey trap.
The measurement result of water extraction thick paste is in Table 4.Alcohol extraction thick paste is because what adopt is 95% alcohol reflux, and polysaccharide composition Precipitation in 80% ethanol, therefore do not contain polysaccharide composition in the thick paste of ethanol extraction.
Polysaccharide component content in table 4 water extraction thick paste
Known from above-mentioned result of the test: adopt the Herba Fici Simplicissimae thick paste of 95% alcohol reflux, the content of psoralen is higher than water extraction thick paste, but in the thick paste of water extraction, contains a large amount of polysaccharide compositions, and polysaccharide composition has good benefiting action.Therefore, in order effectively to extract psoralen in radix fid simplids simae and polysaccharide composition, should adopt different solvents according to two kinds of opposed polarity constituents, substep extracts, first use the Coumarins compositions such as psoralen that ethanol extraction polarity is less, adopt again the polysaccharide composition that water extraction polarity is larger, utilize better the effective ingredient of medical material, bring into play its curative effect.
Embodiment 2: the preparation of compound vitex Radix Fici Hirtae thick paste and the wherein assay of psoralen, polysaccharide
The preparation of 2.1 compound vitex Radix Fici Hirtae thick pastes
According to the result of Herba Fici Simplicissimae medicinal material extract research in embodiment 1, the thick paste preparation technology of compound vitex Radix Fici Hirtae is as follows:
Gomi herbs in step 1, prescription cleans or concocts by pertinent regulations under each medicine item of < < Chinese Pharmacopoeia > > version in 2010, standby.Herba Fici Simplicissimae cleans.
Step 2, get the dry medical material of Herba Fici Simplicissimae and be ground into coarse powder, measure after 95% soak with ethanol 1h condensing reflux 2h, while hot leaching medicinal liquid with 10 times; Add again 8 times of amount 95% alcohol reflux 1h, merge twice filtrate, be evaporated to thick paste standby.Retain medicinal residues, for decocting together with other four Chinese medicine material.
Step 3, three taste pulverizing medicinal materials except Fructus Jujubae are become to coarse powder, Fructus Jujubae directly adds, and the medicinal residues that retain with previous step merge, and decoct with water secondary, and 3 hours for the first time, 12 times of water gagings; 2 hours for the second time, 10 times of water gagings.
Step 4, collecting decoction, filter, and filtrate decompression is concentrated into the thick paste that relative density is 1.30～1.35 (80 ℃).
The assay of psoralen in 2.2 compound vitex Radix Fici Hirtae thick pastes
The preparation of chromatographic condition, sample solution is according in embodiment 1 1.2, and three batch sample measurement results are 0.3526,0.4123,0.3827mg/g.
The assay of polysaccharide in 2.3 compound vitex Radix Fici Hirtae thick pastes
The preparation method of sample according in embodiment 1 1.3 carry out, and adopt standard curve under 1.3 to calculate (if absorbance surpasses the range of linearity, can suitably dilute).The results are shown in Table 5.
The content results of polysaccharide composition in table 5 compound recipe thick paste
Embodiment 3: adopt oxidization time method to measure oxidation resistance
The antioxidation, the anti-aging effects that compare Herba Fici Simplicissimae water extract, ethanol extract and compound preparation.
3.1 reference substance preparations: precision takes vitamin C powder 0.05g, puts in 50mL conical flask, adds water 10mL, is stirred to dissolving, shifts and puts in 50mL volumetric flask, is diluted with water to scale, shakes up, standby.
3.2 sample preparations: respectively water intaking carry, alcohol extraction, the about 0.5g of compound recipe thick paste, accurately weighed, totally 3 parts, put 50mL conical flask.Add respectively 50% ethanol 10mL, 50 ℃ of supersound extraction 30min, take out, cooling, filter, and filtrate is put in 50mL measuring bottle, adds water to scale, shakes up.Standby after diluting 2 times.
3.3 assay methods: accurate reference substance solution, each 10mL of sample solution of drawing, put in 50mL tool plug conical flask, add immediately 20% sulfuric acid solution 2mL, jolting 1min, adds 0.02 molL immediately
-1potassium permanganate solution 0.05mL, timing, when the aubergine of solution disappears completely, writing time.
3.4 result of the tests and data
Oxidization time measurement result is in Table 6, oxidization time is the thick paste of compound recipe thick paste sample > water extraction thick paste > vitamin C > ethanol extraction successively, Herba Fici Simplicissimae recomposition compound recipe is described after oxidation resistance than single medical material, increase.
Table 6 oxidization time method measurement result
Embodiment 4: adopt Prussia's blue laws to measure oxidation resistance
By the mensuration to reducing power, compare antioxidation, the anti-aging effects of Herba Fici Simplicissimae water extract, ethanol extract and compound preparation.
Reference substance solution, sample solution 0.1mL in accurate absorption embodiment 3, add 2.5mL phosphate buffer (0.2M, PH=6.6,0.2M Na respectively
2hPO
4: 0.2M NaH
2pO
462.5) and 5.0mL1% (w/v) potassium ferricyanide K=37.5:
3[Fe (CN)
6] solution, cooling rapidly after 50 ℃ of water-bath 20min, add trichloroacetic acid (TCA) solution of 2.5mL10% (w/v), mix, the centrifugal 10min of 3000rmp, get supernatant 2.5mL, add the ferric chloride solution of 2.5mL distilled water and 0.5mL0.1% (w/v), mix homogeneously, after 10min, in 700nm place, measure its light absorption value, take distilled water as blank, and the larger expression reducing power of light absorption value is stronger, and result contrasts (result of the test is in Table 7) with ascorbic reducing power.Result shows: reducing power is followed successively by vitamin C > compound recipe thick paste > water extraction thick paste > alcohol extraction thick paste.
Table 7 reduction force method measurement result
Embodiment 5: the preparation of compound vitex Radix Fici Hirtae granule
[prescription]
[technique]
The dry medical material of Herba Fici Simplicissimae that takes recipe quantity is ground into coarse powder, with after 10 times of amount 95% soak with ethanol 1h, and condensing reflux 2h, while hot leaching medicinal liquid; Medicinal residues add 8 times of amount 95% alcohol reflux 1h again, merge twice filtrate, are evaporated to thick paste 1.30～1.35 (80 ℃) standby.
In Herba Fici Simplicissimae medicinal residues, then add Poria, Radix Angelicae Sinensis, the Semen Coicis of recipe quantity, three taste medical materials (coarse powder), then the Fructus Jujubae that takes recipe quantity is in three taste medicinal material coarse powder, adds 12 times of water gagings (weight and volume ratio), decocts 3 hours, filters; Filtering residue adds 10 times of water gagings (weight and volume ratio) again, decocts 2 hours, filters, and merges twice filtrate, and being evaporated to relative density is the thick paste of 1.30～1.35 (80 ℃).
Above-mentioned two kinds of thick pastes are mixed, add starch, Icing Sugar, mix, prepare soft material, cross 14 mesh sieves and granulate, 60 ℃ dry, and 14 order granulate, pack aluminium plastic bag into, obtain, and every packed amount is 25g.
Embodiment 6: the preparation technology of compound vitex Radix Fici Hirtae granule investigates
6.1 disintegrating process are investigated
Take flour extraction as investigating index, and the four Chinese medicine material that need are pulverized, in prescription ratio, is investigated, and the results are shown in Table 8 as follows:
Table 8, disintegrating process are investigated
6.2 water extraction process are investigated
The moisture content test: in prescription ratio (50g), take the gomi herbs that need decoct with water, add 12 times of amounts of water, soaked overnight, taking medicinal residues weight in wet base is 197g.Water absorption rate (%)=(197-65)/65 * 100%=226%
Extraction process test: take the gomi herbs that need decoct with water in prescription ratio (500g), add respectively not commensurability decocting to boil, collecting decoction, is condensed into thick paste, is dried to dry cream, paste-forming rate is investigated, to determine its optimum extraction process.Result of the test is in Table 9.From result of the test, test No. 1 suitable with the test paste-forming rate of No. 2, but it is less to test No. 2 total amount of water, is easy to concentrate, and is suitable for large production.Therefore selecting amount of water is 12 times, 10 times.
Table 9, Study on extraction result
Process certification experiment: extraction process is carried out respectively to three batches of checkings (5kg medical material expands 10 times of recipe quantities), result table 10.Result shows, by recipe quantity, amplifies 10 times, and demonstration test result shows, consistent with lab scale result of the test, and three batches of test repeatabilities are good, stable yield.Determine that thus water extraction optimum process condition is: the medical material of recipe quantity decocts with water secondary, and amount of water is respectively 12 times, 10 times, and decocting time is respectively 3 hours, 2 hours.
Table 10, water extraction process demonstration test result table
6.3 concentrated and drying processes
Carry out respectively normal pressure and concentrate and concentrating under reduced pressure, normal pressure is concentrated time-consuming, labor efficiency is low, and concentration time length is easily destroyed effective ingredient, therefore adopt concentrating under reduced pressure.After concentrating under reduced pressure (0.08Mpa, 65 ℃) is the thick paste of 1.30-1.35 (80 ℃) to relative density, standby.
6.4 Study on Forming
The selection of wetting agent: thick paste adds starch, Icing Sugar mix homogeneously, because extractum amount is larger in this product, if take water as wetting agent, easily glue sieve, so the ethanol of variable concentrations of take respectively screens (50% ethanol, 75% ethanol, water are a small amount of) as wetting agent, cross 14 mesh sieves and granulate, 60 ℃ of wet granulars are dry.Cross 14 mesh sieve granulate.Take granule integrity, whether by screen cloth, be easily evaluation index, compare, the results are shown in Table 11.By comparing, having selected 75% ethanol is that wetting agent is for granulating.
Table 11, wetting agent are selected result of the test
Mobility of particle is investigated: by fixed funnel method, measure angle of repose, to determine the mobility of this product.Through the mensuration of 10 times, the meansigma methods of its angle of repose is 35.8 °, shows that mobility is better.
Granule factors influencing: in this product granule, the proportion of extractum is larger, therefore humidity is larger on the impact of granule, carry out the moisture absorption weightening finish experiment under different humidity condition, experimental result is in Table 12: experimental result shows, humidity is larger on granule impact, fill in time after granulation; During production, should note regulating indoor humidity, be controlled at below 60%.
Table 12 granule moisture absorption weightening finish experimental result
6.5 pilot scale scale-ups
By drafting manufacturing condition, carry out three batches of magnify 20 amounts productions, investigate the reasonability of this product production technology, the results are shown in Table 7.Result shows, this technique is suitable for large production, and technique is reasonable, and repeatability is good.
Table 13, pilot scale processing parameter
The quality standard of embodiment 7 compound vitex Radix Fici Hirtae granules
Compound vitex Radix Fici Hirtae granule
Fufang?Wuzhi?Maotao?Keli
[prescription]
[method for making]
The dry medical material of Herba Fici Simplicissimae that takes recipe quantity is ground into coarse powder, with after 10 times of amount 95% soak with ethanol 1h, and condensing reflux 2h, while hot leaching medicinal liquid; Medicinal residues add 8 times of amount 95% alcohol reflux 1h again, merge twice filtrate, are evaporated to thick paste 1.30～1.35 (80 ℃) standby.In Herba Fici Simplicissimae medicinal residues, then add Poria, Radix Angelicae Sinensis, the Semen Coicis of recipe quantity, three taste medical materials (coarse powder), then the Fructus Jujubae that takes recipe quantity is in three taste medicinal material coarse powder, adds 12 times of water gagings (weight and volume ratio), decocts 3 hours, filters; Filtering residue adds 10 times of water gagings (weight and volume ratio) again, decocts 2 hours, filters, and merges twice filtrate, and being evaporated to relative density is the thick paste of 1.30～1.35 (80 ℃).Above-mentioned two kinds of thick pastes are mixed, add starch, Icing Sugar, mix, prepare soft material, cross 14 mesh sieves and granulate, 60 ℃ dry, and 14 order granulate, pack aluminium plastic bag into, obtain, and every packed amount is 25g.
[character] this product is granule, and content is tan granule and powder; Lightly seasoned, micro-sweet.
[discriminating]
1, precision takes granular contents 3g, adds ethyl acetate 50mL, and ultrasonic 25min filters, and filtrate is concentrated into dry, adds ethyl acetate 2mL in 2mL measuring bottle, as need testing solution.Separately get Herba Fici Simplicissimae control medicinal material 5g, be made in the same way of control medicinal material solution.Separately get psoralen reference substance, add ethyl acetate and dissolve, make every 1mL containing the solution of 2mg, in contrast product solution.According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2010), test, draw each 3 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, normal hexane-chloroform-acetic acid second is cruel-formic acid (20: 4: 5: 0.7) launch after saturated 10 minutes, while launching forward position to 1cm left and right, lamellae edge, take out, dry, put under ultra-violet lamp (365nm) and inspect.In test sample chromatograph, with the corresponding position of reference substance chromatograph on, the fluorescence speckle of aobvious same color.Spray again with 10% ethanol solution of sulfuric acid, be placed in the colour developing of 105 ℃ of baking ovens be heated to clear spot with the corresponding position of control medicinal material chromatograph on, the principal spot of aobvious same color.
2, precision takes granular contents 1g, adds acetone 100mL reflux, extract, 1 hour, filters, and gets filtrate water-bath and is concentrated into about 0.5mL, as need testing solution.Separately get Poria control medicinal material 1g, add acetone 20mL reflux, extract, 1 hour, filter, filtrate is concentrated into about 0.5mL, in contrast medical material solution.According to thin layer chromatography (appendix VI B of Chinese Pharmacopoeia version in 2010), test, draw each 15-20 μ L of above-mentioned two kinds of solution, put respectively in same and take on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is adhesive, petroleum ether (60-90 ℃)-ether (1: 1) of take is developing solvent, launch, take out, dry, spray, with 10% phosphomolybdic acid ethanol solution, is heated to speckle colour developing at 100 ℃ clear.In test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, the speckle of aobvious same color.
3, precision takes granular contents 1g, adding water 40mL makes to dissolve, filter, get the n-butanol extraction 2 times that filtrate water is saturated, each 20mL, merge n-butyl alcohol liquid, with n-butyl alcohol saturation water washing 2 times, each 20mL, divides and gets n-butyl alcohol liquid evaporate to dryness, residue adds 1mL methanol to be made to dissolve, as need testing solution.Separately get Fructus Jujubae control medicinal material 2g, decoct with water 1 hour, filter, filtrate is concentrated into 20mL, is made in the same way of control medicinal material solution.According to thin layer chromatography (appendix VI B of Chinese Pharmacopoeia version in 2010), test, draw each 5 μ L of above-mentioned two kinds of solution, put respectively in same and take on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is adhesive, n-butyl alcohol-glacial acetic acid-the water (3: 1: 0.5) of take is developing solvent, launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to speckle colour developing at 100 ℃ clear.In test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, an aobvious identical brown speckle.
[inspection] should meet every regulation relevant under granule item (appendix of Chinese Pharmacopoeia version in 2010).
[assay] measured according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2010).
Chromatographic condition and system suitability adopt the chromatographic column that octadecylsilane chemically bonded silica is filler, and mobile phase is methanol and water (60: 40), and detection wavelength is 254nm, and flow velocity is 1mL/min, and column temperature is 30 ℃.Theoretical cam curve is calculated and is not less than 3000 by psoralen.
It is appropriate that the preparation precision of reference substance solution takes psoralen reference substance, adds methanol and make every 1ml containing the solution of 40 μ g, obtains.
The preparation precision of need testing solution takes granular contents 1g, accurately weighed, puts in tool plug conical flask, precision adds methanol 100mL, accurately weighed weight, supersound extraction 40min, let cool, weighed weight again, supplies the weight of less loss with methanol, shake up, filter, get subsequent filtrate, with 0.22 μ m filtering with microporous membrane, obtain.
Algoscopy is accurate reference substance solution and each 10 μ L of need testing solution of drawing respectively, and injection liquid chromatography, measures, and obtains.
Every bag of this product in psoralen, must not be less than 0.30mg containing Herba Fici Simplicissimae.
[usage and consumption] one time 1 bag, puts into warm water or meat soup.
[specification] aluminium plastic bag packing, every packed 25g
[storage] sealing.
[effect duration] 2 years.
Embodiment 8: the preparation of compound vitex Radix Fici Hirtae drop pill
8.1 according to the compound extract thick paste of power 1-4, as drug extract.
8.2. substrate: Polyethylene Glycol (1500,2000,4000,6000,8000,10000,20000), pharmaceutically suitable carrier such as s6, betacyclodextrin, poloxamer, methyl starch sodium, sodium lauryl sulphate, stearic acid, sodium stearate, glycerin gelatine, polyvinylpyrrolidone, Lac, substrate with arbitrarily two or more, by 1: 1～1: 10 proportioning, be made into mixed-matrix, the hardness of adjustment pill, stripping time limit, outward appearance etc. are investigated index, to be defined as best proportioning.
8.3 proportionings: with g HuokgWei unit, by weight, drug extract: substrate=1: 1～1: 9.
8.4 preparation process comprise: according to the given ratio of formula, accurately take drug extract and substrate, be placed on heating while stirring in heating container, until the fused solution that obtains containing drug extract and substrate and/or emulsion and/or suspension are standby.
Adopt homemade or general pill dripping machine, and adjust the temperature control system of pill dripping machine, make the water dropper temperature of pill dripping machine heat and remain on 50 ℃-90 ℃, the temperature of condensing agent is cooling and remain on-5 ℃-10 ℃ (condensing agents are methyl-silicone oils or/and liquid paraffin or/and vegetable oil); By the fused solution that contains drug extract and substrate and/or emulsion and/or suspension, pour in the water dropper tank of pill dripping machine, by certain speed dripping, guarantee that ball type is complete and get final product.
The best proportioning of 8.5 substrate is: polyethylene glycol 6000 mixes according to 6: 4 with PEG20000; The best proportioning of medicine and substrate is 1: 2.The drop pill that production obtains, roundness, formability, hardness are all good, and average ball is heavily 0.03834g, and be 3min disintegration, and the ball method of double differences is different and meet 2010 editions regulations of Chinese Pharmacopoeia disintegration.
Claims (11)
1. the Chinese medicine composition being comprised of Chinese medicine of the five flavours, is characterized in that in weight portion, comprises the material of following umber: Herba Fici Simplicissimae: 15-50; Fructus Jujubae: 5-30; Poria: 5-30; Radix Angelicae Sinensis: 0-20; Semen Coicis: 5-30.
2. Chinese medicine composition as claimed in claim 1, it is characterized in that being that single medical material combines in proportion, single medical material is pulverized respectively rear combination, single medical material is ground into powder after combining in proportion, single medical material extracts respectively rear combination, certain simply or after a few taste medicinal material extract with other medical materials combinations.
3. Chinese medicine composition as claimed in claim 1, Chinese medicine of the five flavours can be medical material, medicinal powder, decoction pieces or extract.
4. Chinese medicine composition as claimed in claim 1, is characterized in that the preparation of extract comprises the steps:
The dry medical material of Herba Fici Simplicissimae that takes recipe quantity is ground into coarse powder, with after 10 times of amount 95% soak with ethanol 1h, and condensing reflux 2h, while hot leaching medicinal liquid; Medicinal residues add 8 times of amount 95% alcohol reflux 1h again, merge twice filtrate, are evaporated to thick paste 1.30～1.35 (80 ℃) standby.
In Herba Fici Simplicissimae medicinal residues, then add Poria, Radix Angelicae Sinensis, the Semen Coicis of recipe quantity, three taste medical materials (coarse powder), then the Fructus Jujubae that takes recipe quantity is in three taste medicinal material coarse powder, adds 12 times of water gagings (weight and volume ratio), decocts 3 hours, filters; Filtering residue adds 10 times of water gagings (weight and volume ratio) again, decocts 2 hours, filters, and merges twice filtrate, and being evaporated to relative density is the thick paste of 1.30～1.35 (80 ℃).
Above-mentioned two kinds of thick pastes are mixed, obtain; Or two kinds of thick pastes are mixed to rear dried dry powder and get final product; Or mix and get final product after two kinds of thick pastes are dried to respectively to dry powder.
5. extract as claimed in claim 4, for the preparation of conventional peroral dosage forms such as granule, capsule, tablet, powder, drop pill, decoctions.
6. Chinese medicine composition as claimed in claim 1, is characterized in that adopting thin layer chromatography to carry out qualitative identification to Herba Fici Simplicissimae, Poria and Fructus Jujubae.Adopt high performance liquid chromatography to carry out assay to psoralen contained in Herba Fici Simplicissimae.
7. the extract as described in claim 1-4, wherein the qualitative identification method of Herba Fici Simplicissimae is carried out as follows:
Extract thick paste as prepared in claim 4, precision takes thick paste 3g, adds ethyl acetate 50mL, and ultrasonic 25min filters, and filtrate is concentrated into dry, adds ethyl acetate 2mL in 2mL measuring bottle, as need testing solution.Separately get Herba Fici Simplicissimae control medicinal material 5g, be made in the same way of control medicinal material solution.Separately get psoralen reference substance, add ethyl acetate and dissolve, make every 1mL containing the solution of 2mg, in contrast product solution.According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2010), test, draw each 3 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, normal hexane-chloroform-acetic acid second is cruel-formic acid (20: 4: 5: 0.7) launch after saturated 10 minutes, while launching forward position to 1cm left and right, lamellae edge, take out, dry, put under ultra-violet lamp (365nm) and inspect.In test sample chromatograph, with the corresponding position of reference substance chromatograph on, the fluorescence speckle of aobvious same color.Spray again with 10% ethanol solution of sulfuric acid, be placed in the colour developing of 105 ℃ of baking ovens be heated to clear spot with the corresponding position of control medicinal material chromatograph on, the principal spot of aobvious same color.
8. the extract as described in claim 1-4, wherein the qualitative identification method of Poria is carried out as follows:
Extract thick paste as prepared in claim 4, precision takes thick paste 1g, adds acetone 100mL reflux, extract, 1 hour, filters, and gets filtrate water-bath and is concentrated into about 0.5mL, as need testing solution.Separately get Poria control medicinal material 1g, add acetone 20mL reflux, extract, 1 hour, filter, filtrate is concentrated into about 0.5mL, in contrast medical material solution.According to thin layer chromatography (appendix VI B of Chinese Pharmacopoeia version in 2010), test, draw each 15-20 μ L of above-mentioned two kinds of solution, put respectively in same and take on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is adhesive, petroleum ether (60-90 ℃)-ether (1: 1) of take is developing solvent, launch, take out, dry, spray, with 10% phosphomolybdic acid ethanol solution, is heated to speckle colour developing at 100 ℃ clear.In test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, the speckle of aobvious same color.
9. the extract as described in claim 1-4, wherein the qualitative identification method of Fructus Jujubae is carried out as follows:
Extract thick paste as prepared in claim 4, precision takes thick paste 1g, adds water 40mL and makes to dissolve, and filters, get the n-butanol extraction 2 times that filtrate water is saturated, each 20mL, merges n-butyl alcohol liquid, with n-butyl alcohol saturation water washing 2 times, each 20mL, divide and get n-butyl alcohol liquid evaporate to dryness, residue adds 1mL methanol to be made to dissolve, as need testing solution.Separately get Fructus Jujubae control medicinal material 2g, decoct with water 1 hour, filter, filtrate is concentrated into 20mL, is made in the same way of control medicinal material solution.According to thin layer chromatography (appendix VI B of Chinese Pharmacopoeia version in 2010), test, draw each 5 μ L of above-mentioned two kinds of solution, put respectively in same and take on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is adhesive, n-butyl alcohol-glacial acetic acid-the water (3: 1: 0.5) of take is developing solvent, launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to speckle colour developing at 100 ℃ clear.In test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, an aobvious identical brown speckle.
10. the extract as described in claim 1-4, in thick paste, the assay of psoralen in radix fid simplids simae carries out as follows:
Liquid phase chromatogram condition: adopt the chromatographic column that octadecylsilane chemically bonded silica is filler, mobile phase is methanol and water (60: 40), and detection wavelength is 254nm, and flow velocity is 1mL/min, and temperature is 30 ℃, and sample size is 10 μ L.
The preparation of reference substance solution: precision takes in psoralen reference substance 2.0mg to 10mL volumetric flask, adds the about 5mL of methanol, slight fever is dissolved, and cooling room temperature adds methanol dilution scale, shakes up.Accurate absorption in dense storing solution 2mL to 10mL volumetric flask, adds methanol dilution scale, shakes up and adds methanol dilution scale, shakes up, and with 0.22 μ m filtering with microporous membrane, obtains reference substance solution (concentration: 40 μ g/mL).
The preparation of sample solution: extract thick paste as prepared in claim 4, precision takes thick paste 0.5g, accurately weighed, put in tool plug conical flask, precision adds methanol 100mL, accurately weighed weight, supersound extraction 40min, lets cool, more weighed weight, the weight of supplying less loss with methanol, shakes up, and filters, discard just filtrate, get subsequent filtrate, with 0.22 μ m filtering with microporous membrane, standby as sample solution.
11. Chinese medicine compositions as claimed in claim 1 have QI invigorating, enrich blood, the effect of dampness removing, and the disease for due to insufficiency of vital energy and blood, dysfunction of the spleen in transportation, has the effect of antioxidation, slow down aging.
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| CN111413254A (en) * | 2020-04-21 | 2020-07-14 | 回音必集团安徽制药有限公司 | Method for testing thick paste viscosity |
| CN113754677A (en) * | 2021-08-18 | 2021-12-07 | 厦门大学 | Novel coumarin dimer and preparation method and application thereof |
| CN115327001A (en) * | 2022-09-27 | 2022-11-11 | 广州科曼生物科技有限公司 | Ficus simplicissima lour formula particle contrast extract and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105558649A (en) * | 2014-10-14 | 2016-05-11 | 黄名玉 | Radix Fici Simplicissimae health beverage |
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| CN111413254A (en) * | 2020-04-21 | 2020-07-14 | 回音必集团安徽制药有限公司 | Method for testing thick paste viscosity |
| CN111413254B (en) * | 2020-04-21 | 2023-03-21 | 回音必集团安徽制药有限公司 | Method for testing thick paste viscosity |
| CN113754677A (en) * | 2021-08-18 | 2021-12-07 | 厦门大学 | Novel coumarin dimer and preparation method and application thereof |
| CN113754677B (en) * | 2021-08-18 | 2022-09-20 | 厦门大学 | Novel coumarin dimer and preparation method and application thereof |
| CN115327001A (en) * | 2022-09-27 | 2022-11-11 | 广州科曼生物科技有限公司 | Ficus simplicissima lour formula particle contrast extract and preparation method thereof |
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