CN102961427A - Wild chrysanthemum extraction process and measuring method for total flavonoids in wild chrysanthemums - Google Patents
Wild chrysanthemum extraction process and measuring method for total flavonoids in wild chrysanthemums Download PDFInfo
- Publication number
- CN102961427A CN102961427A CN2012105489566A CN201210548956A CN102961427A CN 102961427 A CN102961427 A CN 102961427A CN 2012105489566 A CN2012105489566 A CN 2012105489566A CN 201210548956 A CN201210548956 A CN 201210548956A CN 102961427 A CN102961427 A CN 102961427A
- Authority
- CN
- China
- Prior art keywords
- ethanol
- solution
- wild
- extraction
- shake
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Saccharide Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to the technical field of extraction of Chinese traditional medicines and particularly relates to a wild chrysanthemum extraction process and a measuring method for total flavonoids in wild chrysanthemums. The wild chrysanthemum extraction process sequentially comprises the following steps of: ethanol extraction, first concentration and filtration, resin adsorption, second concentration, spray drying and the like to obtain a wild chrysanthemum extract. The wild chrysanthemum extraction process and the measuring method for the total flavonoids in the wild chrysanthemums, provided by the invention, have the advantages that the ethanol heating reflux extraction is carried out on the wild chrysanthemums by using an orthogonal experiment method, the wild chrysanthemum extract is not reacted with chrysanthemum components, the total flavonoid component of the wild chrysanthemums can be dissolved to the maximum extent, and therefore, the optimal extraction process is obtained. The extraction ratio of the total flavonoids in the wild chrysanthemums is up to 6.23%, and the content of the total flavonoids is up to 9.5%. The wild chrysanthemums are low in raw material cost and suitable for large-scale industrial production, and therefore, the extraction development for the flavonoids in the chrysanthemums has higher practical significance. Macroporous resin has the characteristics of high adsorbing capacity and high desorption ratio is adopted.
Description
Technical field
The present invention relates to the Chinese medicine extraction technical field, be specifically related to a kind of Flos Chrysanthemi Indici extraction process, mother chrysanthemum total flavone assay method.
Background technology
Flos Chrysanthemi Indici is the dry capitulum of feverfew Flos Chrysanthemi (Chrysanthemum indicum L), is China's conventional Chinese medicine, the effect of have dispelling wind, heat clearing away, make eye bright, detoxifying.The diseases such as primary treatment headache, dizzy, conjunctival congestion, irritable feverish sensation of chest and heart, furuncle, toxic swelling.Modern pharmacological research shows, Flos Chrysanthemi has treatment coronary heart disease, reduces blood pressure, prevents hyperlipidemia, antibiotic, antiviral, antiinflammatory, the anti-ageing multiple pharmacologically active of waiting for a long time.The chemical constituent more complicated of Flos Chrysanthemi, wherein flavone compound is its main effective ingredient.Studies show that at present flavone compound can be prevented and treated cardio-cerebrovascular and respiratory system disease, have that antiinflammatory is antibacterial, a blood sugar lowering and strengthen the pharmacological action such as immunologic function.
1, Flos Chrysanthemi Indici chemical constitution study, the chemical constituent of Flos Chrysanthemi Indici has:
Flavonoid comprises luteolin-7-O-BETA-glucopyranoside, acacetin-7-rhamnosidgluoside, luteolin, apiolin, gold and joyous plain class etc.
Volatile oil is divided into terpenoid and non-terpenoid.Terpenoid comprises monoterpene, sesquiterpene, triterpene and containing oxygen derivative thereof etc.; Non-terpenoid comprises Camphora, vinyl compound, ketone compounds, Borneolum Syntheticum, yejuhua lactone, Flos Chrysanthemi Indici alcohols etc.
Other compositions: such as chlorogenic acid, Flos Chrysanthemi Indici polysaccharide, aminoacid and various trace element etc.
2, the main pharmacological of mother chrysanthemum total flavone
Mother chrysanthemum total flavone has antiinflammatory and protect the liver pharmacological action, there are some researches show 250, the continuous 3d gavage of 500mg/kg mother chrysanthemum total flavone, can obviously suppress the mice ear that dimethylbenzene is induced; 168, the continuous 3d gavage of the mother chrysanthemum total flavone of 336mg/kg can alleviate the rat paw edema that carrageenin is induced, and continuously 7d administration can also suppress the granuloma that cotton balls brings out; The external level that can also obviously suppress secretion by peritoneal macrophages PGE2 and leukotriene B4.84,168, the mother chrysanthemum total flavone gastric infusion of 336mg/kg is in arthritis model rat 28d, can significantly alleviate the inflammatory toes swelling in joint; Can obviously suppress the breeder reaction of lymphocyte of adjurant arthritis rat cell, induce its apoptosis; Research find its performance antiinflammatory action may with induce its apoptosis relevant by the expression of downward modulation arthritis synovial cell TRA IL; Mother chrysanthemum total flavone can also partly recover the form of arthritis model lymphocyte of adjurant arthritis rat secretory organelle, suppresses the secretion of inflammatory mediator interleukin 1 B, TNF A and brings into play antiinflammatory action.Mother chrysanthemum total flavone can also be by activating caspase-3, and the apoptosis of synoviocytes of the rat arthritis model due to the inducing adjuvant suppresses its increment and brings into play antiinflammatory action.In addition, can also protect Acute Liver Injury Induced by carbon tetrachloride, this may express relevant with removing oxygen-derived free radicals, inhibition lipid peroxidation, inhibition TNF A.
3, the mensuration of mother chrysanthemum total flavone and Study on extraction
At present, few to extraction and the separation purifying technique research report of mother chrysanthemum total flavone, comprehensively research is not yet arranged deeply.
Jia Lingyun etc. carry out systematic study with ultraviolet spectrophotometry to the total flavones extracting mode as index take this rhinoceros grass element-7-O-glucose former times.Found that: ethanol refluxing process is best, and the total flavones that extracts in the Flos Chrysanthemi with the method for 14 times of amount 95% alcohol reflux 80min (2 times) can obtain higher extracted efficient.
Wang Jiawen etc. investigate extraction process and solvent take the Flos Chrysanthemi general flavone content as investigating index, adopt orthogonal experiment, and its major influence factors is studied.The result shows that the alcohol reflux rate is the highest, extracts the Flos Chrysanthemi total flavones with 20 times of amount 50% ethanol in 85 ℃ of lower reflux, extract, 0.5h (twice) method and can obtain the higher extracted rate.
Wu Xiaochun extracts flavone in the Flos Chrysanthemi with ultrasonic wave extraction, extracts on the basis in single factor, takes Orthogonal Optimization Test, inquires into concentration of alcohol, solid-liquid ratio, extraction temperature and extraction time to the impact of chrysanthemum total flavone extraction process.The result shows that the principal element that affects Flos Chrysanthemi flavone supersound extraction is the liquor-saturated concentration of second, secondly is extraction time, extraction temperature and solid-liquid ratio.Optimal extract process is concentration of alcohol 60%, and solid-liquid ratio 1: 40 extracts 40 ℃ of temperature, extraction time 50min, and recording chrysanthemum total flavone is 3.97%.
Luo Xianhua etc. produce Flos Chrysanthemi Indici as raw material take Guizhou, take boiling water extraction and alcohol steep L9 (3
4) orthogonal experiment, determine that each method is to the optimal extract process of mother chrysanthemum total flavone.Found that: the mother chrysanthemum total flavone extracted amount of ethanol extraction method is higher, and its extraction ratio is 1.9 times of boil water extraction method.
Summary of the invention
The present invention is intended to overcome the technical problem that exists in the above-mentioned prior art, proposes a kind of extraction ratio height, the reliable Flos Chrysanthemi Indici extraction process of assay method, mother chrysanthemum total flavone assay method.
The technical solution used in the present invention is as follows:
The Flos Chrysanthemi Indici extraction process is characterized in that, comprises the steps:
1., ethanol extraction
Add 60% ethanol in Flos Chrysanthemi Indici dry product coarse powder, reflux is extracted 3 times under 70 ℃ of conditions, extracts 3h at every turn, and the weight ratio of Flos Chrysanthemi Indici dry product coarse powder and 60% ethanol is 10: 1 when extracting at every turn, gets ethanol extract;
2., for the first time concentrated and filtration
With the ethanol extract concentrating under reduced pressure, decompression recycling ethanol is extremely most, filtered while hot;
3., resin absorption
The ethanol concentrated solution is adsorbed in AB-8 type macroporous adsorbent resin, the weight ratio of AB-8 type macroporous adsorbent resin and ethanol concentrated solution is 7: 1, use 70% ethanol elution after absorption is finished, the weight ratio of 70% ethanol and ethanol concentrated solution liquid is 12: 1, again the Recycled ethanol eluent;
4., concentrated for the second time
With ethanol elution concentrating under reduced pressure again, get extractum, the proportion of extractum is 1.1～1.2;
5., spray drying
Extractum is carried out spray drying, get Flos Chrysanthemi Indici extract.
The invention also discloses the mother chrysanthemum total flavone assay method, comprise the steps:
1., instrument and reagent
Instrument: UV-2450 spectrophotometry instrument;
Reagent: control substance of Rutin, 60% ethanol, 5% sodium nitrite solution, 10% aluminum nitrate solution, 1mol/L sodium hydroxide test solution;
2., solution preparation
The standard solution preparation
Precision takes by weighing control substance of Rutin 10mg, puts in the 50mL measuring bottle, adds ethanol and makes dissolving, and be diluted to scale, shakes up, and get final product;
Working curve is drawn
The accurate reference substance solution 1,2,3,4,5 and 6mL of drawing is put respectively in the 25mL measuring bottle, respectively adds ethanol to 6mL, add 5% sodium nitrite solution 1mL, shake up, placed 6 minutes, add 10% aluminum nitrate solution 1mL, shake up, placed 6 minutes, add 1mol/L sodium hydroxide test solution 10mL, shake up, add water to scale, shake up, placed 15 minutes, and measured absorbance at the wavelength place of 500nm, calculate regression equation with the concentration that absorbance is corresponding with it;
The need testing solution preparation
Precision takes by weighing sample 30mg, puts in the 25mL measuring bottle, adds appropriate amount of ethanol, and supersonic oscillations 30min is cooled to room temperature, adds ethanol dilution to scale, shakes up, and filters and get final product;
The blank solution preparation
With corresponding solution as blank;
3., sample determination
The accurate need testing solution 2mL that draws puts in the 25mL measuring bottle method under the sighting target directrix curve preparation, add ethanol to 6mL, add 5% sodium nitrite solution 1mL, shake up, placed 6 minutes, and added 10% aluminum nitrate solution 1mL, shake up, placed 6 minutes, and added 1mol/L sodium hydroxide test solution 10mL, shake up, add water to scale, shake up, placed 15 minutes, measure absorbance at the wavelength place of 500nm;
4., the result calculates
The content of total flavones from the regression equation calculation need testing solution.
The advantage of Flos Chrysanthemi Indici extraction process of the present invention, mother chrysanthemum total flavone assay method is:
1., take orthogonal test method, Flos Chrysanthemi Indici is carried out the alcohol heating reflux lixiviate, do not react with the Flos Chrysanthemi composition, and can dissolve to greatest extent the mother chrysanthemum total flavone composition, obtained best extraction process.
2., mother chrysanthemum total flavone extraction rate reached to 6.23%, general flavone content 9.5mg/mL.The cost of raw material of Flos Chrysanthemi Indici is low, is fit to large commercial production, and the extraction of exploitation Flos Chrysanthemi flavone has more practical significance.
3., to adopt macroporous resin to have adsorbance large, the characteristics that desorption efficiency is large.
The specific embodiment
One, extracts embodiment
1., ethanol extraction
Add 60% ethanol (percent by volume, lower same) in Flos Chrysanthemi Indici dry product coarse powder, reflux is extracted 3 times under 70 ℃ of conditions, extracts 3h at every turn, and the weight ratio of Flos Chrysanthemi Indici dry product coarse powder and 60% ethanol is 10: 1 when extracting at every turn, gets ethanol extract;
2., for the first time concentrated and filtration
With the ethanol extract concentrating under reduced pressure, decompression recycling ethanol is extremely most, filtered while hot;
3., resin absorption
The ethanol concentrated solution is adsorbed in AB-8 type macroporous adsorbent resin, the weight ratio of AB-8 type macroporous adsorbent resin and ethanol concentrated solution is 7: 1, usefulness 70% ethanol (percent by volume after absorption is finished, together lower) eluting, the weight ratio of 70% ethanol and ethanol concentrated solution liquid is 12: 1, again the Recycled ethanol eluent;
4., concentrated for the second time
With ethanol elution concentrating under reduced pressure again, get extractum, the proportion of extractum is 1.1～1.2;
5., spray drying
Extractum is carried out spray drying, get Flos Chrysanthemi Indici extract.
Two, mother chrysanthemum total flavone assay method embodiment
1., instrument and reagent
Instrument: UV-2450 spectrophotometry instrument;
Reagent: control substance of Rutin, 60% ethanol, 5% sodium nitrite solution, 10% aluminum nitrate solution, 1mol/L sodium hydroxide test solution;
2., solution preparation
The standard solution preparation
Precision takes by weighing control substance of Rutin 10mg, puts in the 50mL measuring bottle, adds ethanol and makes dissolving, and be diluted to scale, shakes up, and get final product;
Working curve is drawn
The accurate reference substance solution 1,2,3,4,5 and 6mL of drawing is put respectively in the 25mL measuring bottle, respectively adds ethanol to 6mL, add 5% sodium nitrite solution 1mL, shake up, placed 6 minutes, add 10% aluminum nitrate solution 1mL, shake up, placed 6 minutes, add 1mol/L sodium hydroxide test solution 10mL, shake up, add water to scale, shake up, placed 15 minutes, and measured absorbance at the wavelength place of 500nm, calculate regression equation with the concentration that absorbance is corresponding with it;
The need testing solution preparation
Precision takes by weighing sample 30mg, puts in the 25mL measuring bottle, adds appropriate amount of ethanol, and supersonic oscillations 30min is cooled to room temperature, adds ethanol dilution to scale, shakes up, and filters and get final product;
The blank solution preparation
With corresponding solution as blank;
3., sample determination
The accurate need testing solution 2mL that draws puts in the 25mL measuring bottle method under the sighting target directrix curve preparation, add ethanol to 6mL, add 5% sodium nitrite solution 1mL, shake up, placed 6 minutes, and added 10% aluminum nitrate solution 1mL, shake up, placed 6 minutes, and added 1mol/L sodium hydroxide test solution 10mL, shake up, add water to scale, shake up, placed 15 minutes, measure absorbance at the wavelength place of 500nm;
4., the result calculates
The content of total flavones from the regression equation calculation need testing solution.
Three, the selection of extraction process condition
1., the selection of ethanol extraction process conditions
Get Flos Chrysanthemi Indici dry product coarse powder 50g, get the ethanol of 10 times of amounts according to the single factor experiment result by table 1 condition at every turn, get L9 (3
4) orthogonal array arrangement test extraction, merging alcohol extract after extracting filters, decompression recycling ethanol is to most, filtered while hot, the water gaging such as add and with 4% sodium hydroxide solution accent pH to 6～7, leave standstill 12h in 3～5 ℃ of cold preservations and filter, be settled to 250mL with distilled water after 60 ℃ of heating, get the total flavones extracting solution.
After the ultrafiltration, measure by above-mentioned Determination Method of Flavone Content.
Extraction ratio is calculated as follows: (sample total flavones amount/sample size) * 100, concrete outcome see Table 1, table 2 and table 3.
Table 1 factor and level
Table 2 mother chrysanthemum total flavone extracts orthogonal experiments
Positive quadraturing design test shows that ethanol extraction mother chrysanthemum total flavone optimal level is combined as A1B3D3C3.Namely adopt 60% ethanol, 70 ℃ of temperature, each 3h, extract 3 times.
Concentration of alcohol (A), extraction temperature (B) affect large on the total flavones extracted amount, extraction time, (D) took second place, and extraction time (C) impact is minimum.
The variance analysis of table 3 orthogonal experiments
Annotate: F0.05 (2,2)=19.00, F0.01 (2,2)=99.00, * are that significantly * * is for extremely remarkable.
Variance analysis shows, is not considering in the interactive situation, concentration of alcohol, extract temperature the total flavones extracted amount is had appreciable impact, and extraction time, extraction time does not make significant difference.
2., the mother chrysanthemum total flavone purification preparation (demonstration test) of sample liquid
Get Flos Chrysanthemi Indici dry product coarse powder 5kg, according to above-mentioned 1. middle orthogonal design L9 (3
4) the mother chrysanthemum total flavone ethanol extraction optimal level group technology A1B3D3C3 that filters out verifies extraction, extraction ratio 6.23%, identical with optimal case in the orthogonal test scheme, illustrate that optimizing is successfully, is suitable for production application.And produce cold preservation (general flavone content 9.5mg/mL) for subsequent use after the sample liquid by above-mentioned 1. method.
3., the selection of resin absorption technique condition
DM301 type, AB-8 type, S-8 type, D4020 type, ADS-17 type, NKA-9 type, D3520 type resin embathed with 4 times of volume 95% ethanol or acetone first all can, end when embathing liquid and add suitable quantity of water without the white opacity phenomenon, water cleans up repeatedly to distinguishing the flavor of without the alcohol flavor or without ketone, the sodium hydroxide solution that adds 4 times of volume 2mol/L, soak 12h, to be washed to neutrality.The hydrochloric acid that adds again 4 times of volume 4mol/L soaks 12h, washes with water to the rear 60 ℃ of dry for standby of neutrality.
Accurately take by weighing through totally 3 parts of above-mentioned pretreated dried resin 1g, put in the 100mL triangular flask, concussion is adsorbed after accurately adding the above-mentioned sample liquid 20mL that 2. produces, 120 times/min of frequency, interval 1min, then vibration 2h leaves standstill 20h, make its absorption that reaches capacity, draw upper strata liquid and measure total flavones concentration, be calculated as follows the resin saturated extent of adsorption: saturated extent of adsorption=[(concentration after initial concentration-absorption) * adsorption liquid volume]/amount of resin (mg/g dried resin), get meansigma methods 3 times.To behind the static saturated adsorption total flavones, leach by resin, blot surface moisture, leach behind the same method concussion 2h behind the ethanol 20mL of accurate adding 60% concentration, measure the concentration of eluent total flavones, calculate eluting rate: eluting rate=[eluent concentration * effluent volume]/saturated extent of adsorption * 100%, get meansigma methods 3 times, the results are shown in Table 4.
7 kinds of resins of table 4 are to the static saturated adsorption eluting result of mother chrysanthemum total flavone:
Table 4 is the result show, 7 kinds of macroporous adsorbent resins to the static saturated adsorption capacity of mother chrysanthemum total flavone all more than 90mg, maximum with AB-8 type resin static adsorbance, be 113.15mg/g, be higher than other 6 kinds of macroporous resins.
In static eluting, AB-8 type macroporous resin eluting rate is 93.8%, is higher than other 6 kinds, and AB-8 type macroporous resin shows best combination property.
4., AB-8 type resin is measured the dynamic adsorption of mother chrysanthemum total flavone-elution amount
Take by weighing the AB-8 type adsorbent resin 100g and the 20g that have handled well, wet method is packed in the chromatographic column of 3cm * 500cm respectively, with the flow velocity upper prop of the above-mentioned Flos Chrysanthemi Indici extracting solution 330mL (9.5mg/mL) that 2. produces with 2～3mL/min, cross 3 times of resinite accumulated amounts of the complete rear usefulness of post (3BV, it is colourless to eluent that distilled water down together) is washed post with the speed of 3～4mL/min, be eluted to water white transparency with the ethanol of 4 BV 70% with the elution speed of 2～3mL/min again, collect 70% ethanol elution, concentrating under reduced pressure, dry, claim quality, carry out determination of total flavonoids by the mother chrysanthemum total flavone assay method, calculate the dynamic adsorption elution amount, the total flavones response rate etc. (the front total flavones quality of total flavones quality/mistake post * 100 behind the response rate=mistake post) the results are shown in Table 5 (n=3).
Table 5AB-8 type macroporous adsorbent resin is to the dynamic adsorption of mother chrysanthemum total flavone-eluting result
| Amount of resin/g | 100 | 20 |
| Loading total flavones amount/g | 3.1 | 3.1 |
| Receive to get purified amount/g | 3.15 | 2.06 |
| Receive to get total flavones amount/g | 2.87 | 1.89 |
| Total flavones purity/% | 91.1 | 91.8 |
| Adsorbance (dried resin)/(mg/g) | 30.8 | 94.5 |
| The total flavones response rate/% | 92.58 | 60.97 |
Table 5 shows that dress post amount is that the chromatographic column total flavones response rate of 100g is 92.58%, show and adsorb fully, and every gram resin absorption amount is 30.8mg, does not reach saturated.
Dress post amount is that the chromatographic column total flavones response rate of 20g is 60.97%, show not absorption fully, and every gram resin absorption amount is 94.5mg, and adsorbance has reached saturated.
Its adsorbance 94.5mg/g (dried resin) is AB-8 type macroporous adsorbent resin to the saturated dynamic adsorption-elution amount of mother chrysanthemum total flavone.
The present invention is take mother chrysanthemum total flavone content and the response rate etc. as investigating index, research Extraction Techniques of Total Flavonoids in Chrysanthemum Indicun and macroporous adsorbent resin separation and purification mother chrysanthemum total flavone technique.The result shows: take alcohol steep (extraction) L9 (3
4) orthogonal test method, the mother chrysanthemum total flavone optimal extract process is concentration of alcohol 60%, extract temperature 70 C, extraction time 3h, extraction time 3 times.
AB-8 type macroporous adsorbent resin is 113.15mg/g to the mother chrysanthemum total flavone static saturated adsorption capacity, eluting rate is 93.8%, dynamically saturated extent of adsorption is 94.5mg/g (dried resin), the total flavones response rate 92.6%, purity is more than 90%, is the best macroporous adsorbent resin of separation and purification mother chrysanthemum total flavone.
Above content only is that the present invention is conceived example and explanation; under those skilled in the art described specific embodiment is made various modifications or replenish or adopt similar mode to substitute; only otherwise depart from the design of invention or surmount this scope as defined in the claims, all should belong to protection scope of the present invention.
Claims (2)
1. the Flos Chrysanthemi Indici extraction process is characterized in that, comprises the steps:
1., ethanol extraction
Add 60% ethanol in Flos Chrysanthemi Indici dry product coarse powder, reflux is extracted 3 times under 70 ℃ of conditions, extracts 3h at every turn, and the weight ratio of Flos Chrysanthemi Indici dry product coarse powder and 60% ethanol is 10: 1 when extracting at every turn, gets ethanol extract;
2., for the first time concentrated and filtration
With the ethanol extract concentrating under reduced pressure, decompression recycling ethanol is extremely most, filtered while hot;
3., resin absorption
The ethanol concentrated solution is adsorbed in AB-8 type macroporous adsorbent resin, the weight ratio of AB-8 type macroporous adsorbent resin and ethanol concentrated solution is 7: 1, use 70% ethanol elution after absorption is finished, the weight ratio of 70% ethanol and ethanol concentrated solution liquid is 12: 1, again the Recycled ethanol eluent;
4., concentrated for the second time
With ethanol elution concentrating under reduced pressure again, get extractum, the proportion of extractum is 1.1～1.2;
5., spray drying
Extractum is carried out spray drying, get Flos Chrysanthemi Indici extract.
2. the mother chrysanthemum total flavone assay method is characterized in that, comprises the steps:
1., instrument and reagent
Instrument: UV-2450 spectrophotometry instrument;
Reagent: control substance of Rutin, 60% ethanol, 5% sodium nitrite solution, 10% aluminum nitrate solution, 1mol/L sodium hydroxide test solution;
2., solution preparation
The standard solution preparation
Precision takes by weighing control substance of Rutin 10mg, puts in the 50mL measuring bottle, adds ethanol and makes dissolving, and be diluted to scale, shakes up, and get final product;
Working curve is drawn
The accurate reference substance solution 1,2,3,4,5 and 6mL of drawing is put respectively in the 25mL measuring bottle, respectively adds ethanol to 6mL, add 5% sodium nitrite solution 1mL, shake up, placed 6 minutes, add 10% aluminum nitrate solution 1mL, shake up, placed 6 minutes, add 1mol/L sodium hydroxide test solution 10mL, shake up, add water to scale, shake up, placed 15 minutes, and measured absorbance at the wavelength place of 500nm, calculate regression equation with the concentration that absorbance is corresponding with it;
The need testing solution preparation
Precision takes by weighing sample 30mg, puts in the 25mL measuring bottle, adds appropriate amount of ethanol, and supersonic oscillations 30min is cooled to room temperature, adds ethanol dilution to scale, shakes up, and filters and get final product;
The blank solution preparation
With corresponding solution as blank;
3., sample determination
The accurate need testing solution 2mL that draws puts in the 25mL measuring bottle method under the sighting target directrix curve preparation, add ethanol to 6mL, add 5% sodium nitrite solution 1mL, shake up, placed 6 minutes, and added 10% aluminum nitrate solution 1mL, shake up, placed 6 minutes, and added 1mol/L sodium hydroxide test solution 10mL, shake up, add water to scale, shake up, placed 15 minutes, measure absorbance at the wavelength place of 500nm;
4., the result calculates
The content of total flavones from the regression equation calculation need testing solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105489566A CN102961427A (en) | 2012-12-14 | 2012-12-14 | Wild chrysanthemum extraction process and measuring method for total flavonoids in wild chrysanthemums |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105489566A CN102961427A (en) | 2012-12-14 | 2012-12-14 | Wild chrysanthemum extraction process and measuring method for total flavonoids in wild chrysanthemums |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102961427A true CN102961427A (en) | 2013-03-13 |
Family
ID=47792046
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012105489566A Pending CN102961427A (en) | 2012-12-14 | 2012-12-14 | Wild chrysanthemum extraction process and measuring method for total flavonoids in wild chrysanthemums |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102961427A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103267738A (en) * | 2013-05-15 | 2013-08-28 | 浙江大学 | Method for measuring content of flavonoid of silkworm larva body |
| CN105030869A (en) * | 2015-06-29 | 2015-11-11 | 安徽瑞思威尔科技有限公司 | Bo-chrysanthemum total flavone extract preparation method based on response surface optimization |
| CN105062130A (en) * | 2015-08-11 | 2015-11-18 | 浙江理工大学 | Preparation method of wild chrysanthemum natural dye and preparation of anti-bacterial textiles adopting wild chrysanthemum natural dye |
| CN106038652A (en) * | 2016-06-30 | 2016-10-26 | 卢月莲 | Method for extracting and purifying total flavonoids of chrysanthemum |
| CN107917886A (en) * | 2016-10-10 | 2018-04-17 | 武汉光谷人福生物医药有限公司 | The method for measuring total sugar content in Desmodium styracifolium general flavone |
| CN109323998A (en) * | 2018-09-30 | 2019-02-12 | 东阳市杰迩威生物科技有限公司 | The detection method of general flavone in Chinese yew extract |
| WO2022134245A1 (en) * | 2020-12-21 | 2022-06-30 | 海南葫芦娃药业集团股份有限公司 | Heat-clearing and exterior syndrome-relieving traditional chinese medicine composition and preparation method therefor |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857621A (en) * | 2009-04-13 | 2010-10-13 | 上海特善食品科技有限公司 | Preparation method of linarin extracts in wild chrysanthemum flowers |
| CN102552363A (en) * | 2010-12-15 | 2012-07-11 | 中国医药研究开发中心有限公司 | Preparation method for mother chrysanthemum extract |
| CN102743424A (en) * | 2012-07-10 | 2012-10-24 | 郑州大学 | Flos chrysanthemi indici effective ingredient and application thereof |
-
2012
- 2012-12-14 CN CN2012105489566A patent/CN102961427A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857621A (en) * | 2009-04-13 | 2010-10-13 | 上海特善食品科技有限公司 | Preparation method of linarin extracts in wild chrysanthemum flowers |
| CN102552363A (en) * | 2010-12-15 | 2012-07-11 | 中国医药研究开发中心有限公司 | Preparation method for mother chrysanthemum extract |
| CN102743424A (en) * | 2012-07-10 | 2012-10-24 | 郑州大学 | Flos chrysanthemi indici effective ingredient and application thereof |
Non-Patent Citations (3)
| Title |
|---|
| 《大孔吸附树脂分离纯化野菊花总黄酮》 20091231 郁建生 574-579 2 , * |
| 郁建生: "《大孔吸附树脂分离纯化野菊花总黄酮》", 31 December 2009 * |
| 郁建生: "分光光度法测定复方草珊瑚注射液中总黄酮含量方法探讨", 《中兽医医药杂志》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103267738A (en) * | 2013-05-15 | 2013-08-28 | 浙江大学 | Method for measuring content of flavonoid of silkworm larva body |
| CN105030869A (en) * | 2015-06-29 | 2015-11-11 | 安徽瑞思威尔科技有限公司 | Bo-chrysanthemum total flavone extract preparation method based on response surface optimization |
| CN105062130A (en) * | 2015-08-11 | 2015-11-18 | 浙江理工大学 | Preparation method of wild chrysanthemum natural dye and preparation of anti-bacterial textiles adopting wild chrysanthemum natural dye |
| CN105062130B (en) * | 2015-08-11 | 2018-05-22 | 浙江理工大学 | A kind of preparation method of wild chrysanthemum natural dye and its preparation of antimicrobial form textile |
| CN106038652A (en) * | 2016-06-30 | 2016-10-26 | 卢月莲 | Method for extracting and purifying total flavonoids of chrysanthemum |
| CN107917886A (en) * | 2016-10-10 | 2018-04-17 | 武汉光谷人福生物医药有限公司 | The method for measuring total sugar content in Desmodium styracifolium general flavone |
| CN109323998A (en) * | 2018-09-30 | 2019-02-12 | 东阳市杰迩威生物科技有限公司 | The detection method of general flavone in Chinese yew extract |
| WO2022134245A1 (en) * | 2020-12-21 | 2022-06-30 | 海南葫芦娃药业集团股份有限公司 | Heat-clearing and exterior syndrome-relieving traditional chinese medicine composition and preparation method therefor |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102961427A (en) | Wild chrysanthemum extraction process and measuring method for total flavonoids in wild chrysanthemums | |
| CN102302592B (en) | Preparation technology and purpose of citrus grandis peel flavones | |
| CN103961381B (en) | Method for negative-pressure boiling extraction and preparation of low-acid ginkgo extract | |
| CN101392000B (en) | High efficiency separation purification method of ginkgolide A, B, C, J and bilobalide monomer | |
| CN101139320A (en) | Method for separating nuciferine and lotus leaf flavone from lotus leaf | |
| CN102101876A (en) | Preparation method of arctiin | |
| CN102382151A (en) | Separation and purification method for safflower yellow | |
| CN1269831C (en) | Method for preparing polygonin and resveratrol | |
| CN104693034B (en) | The purification process of Cichoric acid in a kind of Echinacea | |
| CN102093328B (en) | Method for enriching and purifying procyanidin in pine bark | |
| CN109096351A (en) | A kind of buckeye saponin extraction technique | |
| CN103073561B (en) | Process of extracting artemisinin by biological enzyme-percolation method | |
| CN111595972A (en) | Preparation method and quality detection method of lithocarpus polystachyus rehd total flavone extract | |
| CN107412431A (en) | Ultrasonic assistant extracts Physalis pubescens L general flavone and purifying process | |
| CN103232515A (en) | Cyclocarya paliurus glucoside I preparation method | |
| CN103242422A (en) | Method for extracting cyclocaric acid A from cyclocarya paliurus leaves | |
| CN110386861A (en) | The novel technological method of cannabidiol is extracted in industrial hemp | |
| CN109010409B (en) | Extraction and purification process and content detection method of total flavonoids in herminium leaves | |
| CN106336440A (en) | Method for extracting and separating out oleanolic acid from olive leaves | |
| CN101612237B (en) | Method for extracting purified cortex phellodendri total alkaloid by utilizing ion-exchange fiber | |
| CN103193750B (en) | Method for preparing shikimic acid and anise flavonoid by joint separation of macroporous resin XAD7HP | |
| CN103232470A (en) | Method for preparing high-purity ailanthone | |
| CN103214544A (en) | Method for extracting ursolic acid from paulownia leaves | |
| CN102010449A (en) | Method for preparing geraniin | |
| CN101879241A (en) | Method for extracting alkaloid from radix zanthoxyli |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20130313 |