CN101104010A - Extracting and purifying technology for haw flavonoids substances - Google Patents
Extracting and purifying technology for haw flavonoids substances Download PDFInfo
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- CN101104010A CN101104010A CNA2007100526498A CN200710052649A CN101104010A CN 101104010 A CN101104010 A CN 101104010A CN A2007100526498 A CNA2007100526498 A CN A2007100526498A CN 200710052649 A CN200710052649 A CN 200710052649A CN 101104010 A CN101104010 A CN 101104010A
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Abstract
Disclosed is an extraction and purification process of hawthorn flavonoid ingredients. The process is practiced in steps that firstly, hawthorn decoction pieces are dried and processed into particles with 3-8 mm diameter; the particles with ethanol with 70 percent of concentration are refluxed and extracted for three times; for the first time the particles and the ethanol with eight times of weight of the particles are extracted for two hours, and for the second and the third times, the particles and the ethanol with 6 times of weight of the particles are extracted for one hour; the liquid extractive is combined and decompressed for ethanol recovering, and then are condensed to extractive concentrated solution; secondly, water is added into the extractive concentrated solution until every milliliter of the extractive concentrated solution contains 0.1g of crude drug, the pH is regulated between 3 and 4, and then filtrate is produced after the solution is filtered; thirdly, the filtrate is made to pass through a D-101 macroporous resin column for adsorption, water washing and ethanol elution; lastly, the ethanol eluant is collected and condensed to the eluant with 1.1g per milliliter in consistency, and then the hawthorn extractive is produced after the condensed eluant is dried by spray. With the hawthorn extraction method, the total flavone transfer rate of hawthorn can be achieved to 79.5 per cent, and the total flavone content in the hawthorn extractive is calculated by rutin to be 24.6 per cent.
Description
Technical field
The present invention relates to a kind of extracting method of Chinese medicine, be specifically related to extracting method and the extract thereof of Fructus Crataegi.
Background technology
Fructus Crataegi is the dry mature fruit of may Fructus Pyri Pashiae Crataegus pinnatifida Bge.var major.N.E.Br. of the little section of rose or Fructus Crataegi C.pinnatifida Bge., records in version " Chinese pharmacopoeia in 2005.Effect with promoting digestion and removing stagnation, blood circulation promoting and blood stasis dispelling.Now find and separate the composition that obtains to have kind more than 150 from Fructus Crataegi (sarcocarp, nuclear and leaf), main component is flavonoid, organic acid etc.Flavone is the main active of Fructus Crataegi, has now separated to obtain hyperin, rutin, Quercetin, vitexin etc.In recent years, Fructus Crataegi is used for diseases such as clinical treatment hypertension, coronary heart disease and hyperlipemia.Modern pharmacological research shows that the main effective ingredient of Fructus Crataegi is a flavone compound, has blood pressure lowering, increases effects such as coronary flow, cardiotonic, blood fat reducing.Therefore, the research and development of Fructus Crataegi total flavones have important economic benefit and social benefit.
More to Folium Crataegi total flavones extraction and purification process document, and do not see and adopt the positive quadraturing design test method Fructus Crataegi total flavones extraction, purifying process to be carried out the report of comprehensive systematic study.This research contents has stronger practical value.
Current, the single medicinal material extract just day by day comes into one's own as a kind of emerging product, and it is a support with modern extraction and separation technology, uses the quality controllable and stable extract and the preparation thereof of preparation technology's production of standard; Adopt by " Chinese crude drug quality of production management regulation " (GAP) requirement standardized planting and gather and the quality controllable Chinese crude drug processed is a raw material, with modern extractive technique, again press " Good Manufacturing Practice and Quality Control of Drug " (GMP) management mode improving the extract product of producing under the Quality Monitoring Control System with controlled quality standard.The technological progress of Chinese medicine industry and the requirement of the modernization of Chinese medicine have been embodied.
Summary of the invention
The object of the present invention is to provide the drying means of extraction, purification and the extract of the effective site of a kind of Fructus Crataegi.
Another purpose of the present invention has been to provide the Fructus Crataegi total flavones extract that adopts said method to obtain.
The extracting method of a kind of Fructus Crataegi of the present invention comprises: the Fructus Crataegi ethanol extract concentrates the back aqueous precipitation, crosses macroporous resin column, and ethanol elution is used in washing, concentrates ethanol elution, spray drying.
Concrete extraction step is as follows:
1). get the Fructus Crataegi decoction pieces, dry, be processed into the particle of 3-8 millimeter, add the alcohol reflux three times of concentration 60-80%, add the ethanol extraction 2 hours of 8 times of amounts of Fructus Crataegi weight for the first time, the ethanol extraction 1 hour that adds for the second time 6 times of amounts, add the ethanol extraction 1 hour of 6 times of amounts for the third time, merge 3 times extracting solution, decompression recycling ethanol, be concentrated to no ethanol flavor, must extract concentrated solution;
2), extraction concentrated solution that step 1) is obtained adds water to every milliliter and contains crude drug 0.1 gram, adjust pH is 3～4, filter, filtrate;
3), with step 2) filtrate that obtains crosses the D-101 macroporous resin column and adsorbs, washes with water and ethanol elution, absorption, washing and ethanol elution process conditions are: the adsorption liquid flow velocity be 2-6 times of column volume/hour, the absorption liquid measure is 4 times of column volumes; The washing speed be 2 times of column volumes/hour, the washing volume be 6 times of column volumes; The eluting concentration of ethanol is 60-90%, flow velocity be 2 times of column volumes/hour, consumption is 4.5 times of column volumes;
4), collect ethanol elution, being concentrated into density is 1.1 grams per milliliters, spray drying obtains the Fructus Crataegi extract product, general flavone content counts 24.6% with rutin in the extract.Collect exsiccant Fructus Crataegi extract product, seal, put coldly, weigh, put dry place and preserve.
The said extracted optimum condition:
The alcohol reflux three times that adds concentration 70% in the described step 1).
In the described step 3) absorption flow velocity be 2 times of column volumes/hour, adsorbance is 4 times of column volumes; The washing speed be 2 times of column volumes/hour, the washing volume be 6 times of column volumes; The eluting concentration of ethanol is 80%, flow velocity be 2 times of column volumes/hour, consumption is 4.5 times of column volumes.
The spray drying condition is in the described step 4): the spray dryer intake air temperature is 170 ℃, and the air outlet temperature is 90 ℃, and the atomizing disk rotating speed is 20000 rev/mins.
Adopt Fructus Crataegi extracting method of the present invention, its Fructus Crataegi total flavones rate of transform reaches 79.5%, and general flavone content counts 24.6% with rutin in the extract.
The % of concentration of alcohol described in the present invention is meant in the 100 volume ethanol aqueous solutions and contains the ethanol volume fraction.
The present invention compared with prior art has following advantage:
1, work simplification.The present invention adopts the alcohol reflux of suitable concn, flavone component rate of transform height; Simultaneously, after in this method ethanol extract concentrate not had the alcohol flavor, the adding distil water dissolving, filter, filtrate is crossed post, and processing had both guaranteed whole transfers of effective ingredient like this, and filtrate also helps the absorption of effective ingredient, and can prevent the obstruction of resin column effectively, guarantee the smoothness of big production technology.
2, adopt spray drying can obviously shorten the heated time of active component, reduce the composition loss.
3, this process using D-101 macroporous resin carries out separation and purification.This resin price is lower, and safety is higher, is that present domestic medicine trade uses maximum a kind of macroporous resins.
Description of drawings
Fig. 1 technical process flow process figure
The leakage plot of D101 macroporous resin column absorption total flavones on Fig. 2 Fructus Crataegi sample solution
Figure 38 0% ethanol is the elution curve of total flavones in the eluant eluting resin column
Technological process shown in Figure 1 is: 15 kilograms of hawthorn medicinal materials (medicine materical crude slice), extract 3 times with 70% alcohol reflux, for the first time with 120 liters of ethanol, refluxing extraction 2 hours, second and third time is respectively 90 liters with ethanol, and respectively refluxing extraction is 1 hour, and the hawthorn extract that obtains for 3 times merges, Recycled ethanol, be concentrated to without the ethanol flavor, placement is spent the night, and filters, filtrate is diluted to 150 liters, and is for subsequent use; The filtrate of dilution is passed through macroreticular resin with 2 times of column volumes/hour speed, use first 6 times of column volume distilled water flushings after the absorption fully, use again 80% ethanol of 4.5 times of column volumes with identical flow velocity wash-out, collect eluent, eluent is concentrated into an amount of volume, spray-drying gets the haw thorn extract sealing and preserves.
The specific embodiment
Below in conjunction with embodiment the inventive method is further described.
The extraction process experiment of embodiment 1 Fructus Crataegi total flavones
(1) uses ethanol reflux extraction to experimentize, adopt L
9(3
4) orthogonal experiment method investigates the technological parameter of factors such as concentration of alcohol, ethanol consumption (multiple of Fructus Crataegi weight), extraction time and decoction pieces granularity in the alcohol reflux Fructus Crataegi total flavones, and adopt ultraviolet one visible spectrophotometry that content of total flavone in the extract is measured, and compare analysis as index.The results are shown in Table 1, table 2, table 3.
Table 1 experimental factor water-glass
| Level | Factor | |||
| A concentration of alcohol (%) | B ethanol consumption (multiple) | The C time (hour) | D |
|
| 1 2 3 | 60 70 80 | 6 8 10 | 2 2-1 2-1-1 | The coarse powder of decoction pieces particle (3 millimeters-8 millimeters) |
Table 2 L
9(3
4) orthogonal design table
| Sequence number | A | B | C | D | General flavone content (milligram/gram) |
| 1 2 3 4 5 6 7 8 9 | 1 1 1 2 2 2 3 3 3 | 1 2 3 1 2 3 1 2 3 | 1 2 3 2 3 1 3 1 2 | 1 2 3 3 2 1 2 3 1 | 10.6177 13.9070 14.3542 15.1080 15.3369 15.7158 11.5840 13.4341 11.8438 |
Table 3 result of the test analysis of variance table
| A | B | C | D | |
| K 1 K 2 K 3 R S S K MAX K MIN ∑ Yi F S | 38.8789 46.1607 36.8619 9.2988 15.9512 46.1607 36.8619 121.9015 2 7.9756 | 37.3097 42.6780 41.9138 5.3683 5.6223 42.6780 37.3097 121.9015 2 2.8111 | 39.7676 40.8588 41.2751 1.5075 0.4041 41.2751 39.7676 121.9015 2 0.2020 | 37.7984 41.2068 42.8963 5.0979 4.4956 42.8963 37.7984 121.9015 2 1.2478 |
| F P | 39.4768 ＜0.05 | 13.9143 ＞0.05 | 0.0000 ＞0.05 | 11.1259 ＞0.05 |
Orthogonal experiments shows (seeing Table 1, table 2, table 3), influence factor's maximum be concentration of alcohol, secondly be ethanol consumption and decoction pieces granularity, extraction time does not have obvious influence, it is A that intuitive analysis goes out optimum extraction process
2B
2C
3D
3Investigating in the decoction pieces granularity factor particle does not have evident difference with coarse powder to the Fructus Crataegi total flavones yield, and be processed into coarse powder increases difficulty and production cost on the explained hereafter in addition, so the selection decoction pieces is processed into 3 millimeters-8 millimeters particle.In sum, selected only process conditions are A
2B
2C
3D
2, be about to Fructus Crataegi and be processed into 3 millimeters-8 millimeters particles, add 70% ethanol of 8 times of amounts, to extract 3 times, extraction time was respectively 2 hours, and 1 hour, 1 hour.
(2) demonstration test: get the Fructus Crataegi particle, totally 3 parts, carry out demonstration test according to preferred extraction process, record general flavone content and be respectively 15.23 milligrams/gram, 15.17 milligrams/gram, 15.32 milligrams/gram, demonstration test result shows that preferred extraction process stablizes feasible.
The purification by macroporous resin technological experiment of embodiment 2 Fructus Crataegi total flavones
Extract the hawthorn extract that obtains with aforementioned preferred extraction conditions and carry out following experiment:
(1) screening experiment of macroporous resin
Resin source: D101 resin (Tianjin sea light chemical industry company limited), AB-8, D4020 resin (Chemical Plant of Nankai Univ.), SP825, HP20, SP70 (MIT).
The The selection result of resin sees Table 4, table 5, table 6.
The static saturated extent of adsorption measurement result of five kinds of resins of table 4
| The resin kind | Polarity | Fructus Crataegi total flavones adsorbance (milligram) |
| D-101 AB-8 SP825 HP20 D4020 | Nonpolar low pole is nonpolar nonpolar | 11.37 11.09 11.42 7.48 5.87 |
Five kinds of resin desorption of table 5 measurement result
| The resin kind | Fructus Crataegi total flavones elution amount (milligram) | Eluting rate (%) |
| D101 AB-8 SP825 HP20 D4020 | 8.88 8.37 9.03 5.20 3.45 | 78.1 75.5 79.1 69.5 58.8 |
Five kinds of dynamic The selection result of macroporous resin of table 6
| The resin kind | Upper column quantity (milligram) | Than adsorbance (milligram/gram) | Than elution amount (milligram/gram) |
| D-101 AB-8 SP825 HP20 D4020 | 141.28 144.49 142.97 140.53 142.38 | 15.57 15.02 16.24 10.26 9.35 | 12.77 11.71 13.13 7.24 5.61 |
Result of the test shows: D-101, AB-8 and SP825 type macroporous resin are to the ratio adsorbance of Fructus Crataegi total flavones and all be better than the macroporous resin of HP20 and D4020 model than elution amount.Wherein the resin effect of SP825 model is best, is the D-101 type secondly.But both difference on effect are not clearly, it is lower to investigate D-101 type macroporous resin price, and safety is higher, is that present domestic medicine trade uses maximum a kind of macroporous resins, so this research selects for use D-101 type macroporous resin that Fructus Crataegi total flavones is carried out purification research.
(2) D-101 resin purification technological experiment
1. adsorption conditions optimization experiment
The pH value that adopts the concentration (in the crude drug amount that is contained in the sample) of the above sample flow velocity of orthogonal test method, medicinal liquid and go up the sample medicinal liquid is used L as investigating factor
9(3
4) hand over table to arrange test down, factor and level arrangement see Table 7.General flavone content is measured in above 9 groups of tests respectively, and estimated.Analysis result sees Table 8, table 9.
Table 7 factor level table
| Level | Factor | |||
| The last sample flow velocity of A (times column volume/hour) | The last sample concentration of B (grams per milliliter) | The C blank | The last sample medicinal liquid of |
|
| 1 2 3 | 2 4 6 | 0.05 0.1 0.2 | 3～4 5～6 7～8 | |
Table 8 orthogonal experiments
| The experiment number | Factor | The result | |
| A | B | C | D |
| 1 2 3 4 5 6 7 8 9 K1 K2 |
1 1 1 2 2 2 3 3 3 173.9500 154.3600 156.7400 19.5900 76.1796 | 1 2 3 1 2 3 1 2 3 130.1400 178.7600 176.1500 48.6200 498.6263 | 1 2 3 2 3 1 3 2 161.6400 164.1600 159.2500 4.9100 4.0190 | 1 2 3 3 1 2 2 3 1 180.4200 153.4300 151.2000 29.2200 176.3602 | 53.70 61.75 58.50 38.27 62.58 53.51 38.17 54.43 64.14 |
Table 9 variance analysis
| Soruces of variation | SS | f | S | F | P |
| A B C D | 76.2126 498.5299 4.0025 175.2353 | 2 2 2 2 | 38.1063 249.2649 2.0012 88.1176 | 19.0414 124.5557 1 44.0317 | P＜0.05 P＜0.01 P＞0.05 P＜0.05 |
Annotate: F
0.05(2,2)=19.00, F
0.01(2,2)=99.0
Intuitive analysis shows, 3 factors are followed successively by the influence degree of the adsorption efficiency of Fructus Crataegi total flavones on macroporous adsorbent resin: go up sample concentration (B)＞medicinal liquid pH (D)＞go up sample flow velocity (A), preferred compositions is A
1B
2D
1, see Table 3-9.ANOVA showed significant, in the adsorption process of Fructus Crataegi total flavones, A, D two factors have appreciable impact, and the B factor affecting is very remarkable.
2. applied sample amount is investigated
Get 0.1 grams per milliliter sample solution, transfer pH3～4, be added on the 20 gram D101 resin columns (20 millimeters * 400 millimeters), with 2 times of column volumes/hour flow velocity pass through.Each flow point is collected 10 milliliters, measures and calculate the concentration of total flavones in the flow point.Measurement result is seen Fig. 1.When applied sample amount is 80 milliliters, (be about 4 times of column volumes) as can be seen among the figure and begin to leak, (be about 13 times of column volumes) when applied sample amount is 260 milliliters and reach the absorption saturation.
3. ethanol elution concentration is investigated
Other gets four parts of upper props of 20g resin, adsorb by above condition, after the suitable quantity of water flushing, respectively with an amount of 60%, 70%, 80%, 90% ethanol with 2 times of column volumes/hour the flow velocity eluting, measure general flavone content in the eluent, calculate eluting rate; Volatilize solvent, with the extractum weight, the accurate title, decide and calculate content of total flavone, the results are shown in Table 10.
The amount of total flavones in the table 10 variable concentrations eluent
| Concentration of alcohol | 60％ | 70％ | 80％ | 90％ |
| Elution amount (mg) eluting rate (%) general flavone content (%) | 169.8 86.57 25.4 | 180.1 91.83 26.7 | 183.6 93.61 28.1 | 184.2 93.91 19.7 |
The result shows: 80% and 90% elute effect differs not obvious, and safety factors and cost etc. are taken all factors into consideration and selected 80% ethanol elution for use from production process.
4. elution rate is investigated
Carrying out dynamic adsorption by above-mentioned condition, is eluant with 80% ethanol, respectively with 2,4,6 times of column volumes/hour the speed eluting, measure in the ethanol elution thing total flavones amount and calculate eluting rate, the result show elution rate be 2 times of column volumes/hour the time eluting rate the highest.
5. the ethanol elution amount is investigated
Carrying out dynamic adsorption by above-mentioned condition, is that eluant carries out eluting with 80% ethanol, and the quantitative collection effluent is also measured wherein total flavones concentration.The results are shown in Figure 2.
The result shows: with 90 milliliters of (about 4.5 times of column volumes) 80% ethanol with 2 times of column volumes/hour flow velocity adsorbed flavones ingredient of eluting 20g resin fully.
6. washing condition is investigated
Get by above-mentioned condition and adsorb good macroporous resin column, use distilled water flushing, flow velocity be 2 times of column volumes/hour, each flow point is collected 10 milliliters, is concentrated into 1 milliliter, with alphanaphthol reaction (Molish reaction) inspection knowledge, when reaction is negative, stops to wash.Experimental result shows, can remove substantially with the sugar on the resin column of 120 milliliters of washings (about 6 times of column volumes) back.
Embodiment 3 pilot scale amplification tests
Take by weighing 15 kilograms of Fructus Crataegi decoction pieces, 70% alcohol reflux 3 times is for the first time with 120 liters of ethanol, reflux, extract, 2 hours, second and third time is respectively 90 liters with ethanol, reflux, extract, is 1 hour respectively, merges 3 times extracting solution, reclaims ethanol to there not being the alcohol flavor, placement is spent the night, inferior daily filter cloth filtering precipitation is diluted to every milliliter of solution that contains crude drug 0.1 gram, and is standby.
With 20 kilograms of an amount of soak with ethanol of pharmaceutical grade D101 type macroporous resin, the wet method upper prop, standby after handling.
Extract medicinal liquid and go up sample adding resin column at twice, each 75 liters, last sample flow velocity be 2 times of column volumes/hour, pH value is original liquid pH value (being about pH 3～4), behind the last sample earlier with the distilled water flushing of 6 times of column volumes, 4.5 times of column volume 80% ethanol of reuse are with identical flow velocity eluting, collect ethanol elution, be concentrated into small size (density is about 1.1 grams per milliliters), (the spray dryer intake air temperature is 170 ℃ to spray drying, the air outlet temperature is 90 ℃, and the atomizing disk rotating speed is 20000 rev/mins).Collect dry extract, seal, put coldly, weigh, put dry place and preserve.Adopt ultraviolet visible spectrophotometry to measure content of total flavone (in rutin) in the extract, calculate the rate of transform (in the rate of transform=extract in content of total flavone/crude drug content of total flavone * 100%) and receive cream rate (receipts cream rate=extract gross weight/crude drug gross weight * 100%).Result of the test sees Table 11.
Table 11 pilot experiment result
| The test batch | Dosage (kilogram) | Receive cream rate (%) | The rate of transform (%) | Extractive total flavone content (%) |
| 123 meansigma methodss | 15.0 15.0 15.0 15.0 | 3.1 3.1 3.0 3.1 | 79.3 80.1 79.2 79.5 | 24.5 24.7 24.6 24.6 |
Three batches of pilot scales are amplified result of study and shown: its Fructus Crataegi total flavones rate of transform reaches 79.5%, and general flavone content counts 24.6% with rutin in the extract.The technological parameter that shows this research is feasible, and stable process conditions is expected to carry out the transition to industrialization production.
Claims (5)
1. a Fructus Crataegi extract is characterized in that general flavone content counts 24.6% with rutin in the extract.
2. the extracting method of the described Fructus Crataegi extract of claim 1 is characterized in that extraction step is:
1), gets the Fructus Crataegi decoction pieces, dry, be processed into the particle of 3-8 millimeter, add the alcohol reflux three times of concentration 60-80%, add the ethanol extraction 2 hours of 8 times of amounts of Fructus Crataegi weight for the first time, the ethanol extraction 1 hour that adds for the second time 6 times of amounts, add the ethanol extraction 1 hour of 6 times of amounts for the third time, merge 3 times extracting solution, decompression recycling ethanol, being concentrated to does not have the alcohol flavor, must extract concentrated solution;
2), extraction concentrated solution that step 1) is obtained adds water to every milliliter and contains crude drug 0.1 gram, adjust pH is 3～4, filter, filtrate;
3), with step 2) filtrate that obtains crosses the D-101 macroporous resin column and adsorbs, washes with water and ethanol elution, absorption, washing and ethanol elution process conditions are: the adsorption liquid flow velocity be 2-6 times of column volume/hour, the absorption liquid measure is 4 times of column volumes; The washing speed be 2 times of column volumes/hour, the washing volume be 6 times of column volumes; The eluting concentration of ethanol is 60-90%, flow velocity be 2 times of column volumes/hour, consumption is 4.5 times of column volumes;
4), collect ethanol elution, being concentrated into density is 1.1 grams per milliliters, spray drying obtains the Fructus Crataegi extract product, general flavone content counts 24.6% with rutin in the extract.
3. the extracting method of Fructus Crataegi extract as claimed in claim 2 is characterized in that adding in the described step 1) alcohol reflux three times of concentration 70%.
4. the extracting method of Fructus Crataegi extract as claimed in claim 2, it is characterized in that in the described step 3) adsorption liquid flow velocity be 2 times of column volumes/hour, the absorption liquid measure is 4 times of column volumes; The washing speed be 2 times of column volumes/hour, the washing volume be 6 times of column volumes; The eluting concentration of ethanol is 80%, flow velocity be 2 times of column volumes/hour, consumption is 4.5 times of column volumes.
5. the extracting method of Fructus Crataegi extract as claimed in claim 2, it is characterized in that the spray drying condition is in the described step 4): the spray dryer intake air temperature is 170 ℃, and the air outlet temperature is 90 ℃, and the atomizing disk rotating speed is 20000 rev/mins.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101269135B (en) * | 2008-04-02 | 2011-09-21 | 湖北中医学院 | Technique for extracting and purifying kudzu root, whitethorn, safflower yellow ketones component |
| CN102836188A (en) * | 2012-09-25 | 2012-12-26 | 孙冬梅 | Folium microcotis total flavone extract and preparation method and application thereof |
| CN103223030A (en) * | 2013-04-08 | 2013-07-31 | 张宗升 | Chinese medicinal composition |
| CN103230467A (en) * | 2013-04-08 | 2013-08-07 | 张宗升 | Traditional Chinese medicine extract and preparation method thereof |
| CN104173402A (en) * | 2014-08-14 | 2014-12-03 | 辽宁中医药大学 | Method for preparing general flavone in inula flower medicinal materials and anticancer application of general flavone |
| CN114081918A (en) * | 2021-11-18 | 2022-02-25 | 南京市中医院 | Preparation method of cayratia japonica total flavonoids |
| CN115300552A (en) * | 2022-02-11 | 2022-11-08 | 浙江中医药大学 | Application of hawthorn total flavonoids in preparation of medicine for preventing or treating metabolic syndrome |
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2007
- 2007-07-05 CN CNA2007100526498A patent/CN101104010A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101269135B (en) * | 2008-04-02 | 2011-09-21 | 湖北中医学院 | Technique for extracting and purifying kudzu root, whitethorn, safflower yellow ketones component |
| CN102836188A (en) * | 2012-09-25 | 2012-12-26 | 孙冬梅 | Folium microcotis total flavone extract and preparation method and application thereof |
| CN102836188B (en) * | 2012-09-25 | 2014-04-23 | 孙冬梅 | Folium microcotis total flavone extract and preparation method and application thereof |
| CN103223030A (en) * | 2013-04-08 | 2013-07-31 | 张宗升 | Chinese medicinal composition |
| CN103230467A (en) * | 2013-04-08 | 2013-08-07 | 张宗升 | Traditional Chinese medicine extract and preparation method thereof |
| CN104173402A (en) * | 2014-08-14 | 2014-12-03 | 辽宁中医药大学 | Method for preparing general flavone in inula flower medicinal materials and anticancer application of general flavone |
| CN104173402B (en) * | 2014-08-14 | 2018-01-02 | 辽宁中医药大学 | The preparation method and its anticancer purpose of general flavone in a kind of Inula britannica chinensis medicinal material |
| CN114081918A (en) * | 2021-11-18 | 2022-02-25 | 南京市中医院 | Preparation method of cayratia japonica total flavonoids |
| CN115300552A (en) * | 2022-02-11 | 2022-11-08 | 浙江中医药大学 | Application of hawthorn total flavonoids in preparation of medicine for preventing or treating metabolic syndrome |
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