CN102302538B - Humifuse euphorbia herb extract, preparation process and application thereof - Google Patents
Humifuse euphorbia herb extract, preparation process and application thereof Download PDFInfo
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- CN102302538B CN102302538B CN2011102556013A CN201110255601A CN102302538B CN 102302538 B CN102302538 B CN 102302538B CN 2011102556013 A CN2011102556013 A CN 2011102556013A CN 201110255601 A CN201110255601 A CN 201110255601A CN 102302538 B CN102302538 B CN 102302538B
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- euphorbiae humifusae
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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Abstract
The invention discloses a humifuse euphorbia herb extract, a preparation process and an application thereof, and belongs to the field of natural pharmaceutical chemistry. According to the present invention, the humifuse euphorbia herb is subjected to reflux extraction; then the extracting solution is condensed; the condensed solution is placed on a polyamide column; a gradient elution treatment is adopted respectively through water, 30% ethanol and 50% ethanol; the 50% ethanol eluent is collected; the collected eluent is subjected to condensing and drying to prepare the humifuse euphorbia herb extract. The main ingredient of the humifuse euphorbia herb extract comprise: 24-27 wt% of total flavonoid, wherein quercetin is the main ingredient in the total flavonoid, and has the content of 12-14 wt%. With the present invention, the product is eluted through the polyamide column, and the degradable tannin component is removed, such that the final extract is purified so as to establish a solid foundation for further development and application of the product. The experiment results show that: the humifuse euphorbia herb extract prepared through the process has a good effect of inhibition of drug resistance avian Escherichia coli.
Description
Technical field
The present invention relates to a kind of Herba Euphorbiae Humifusae extract, preparation technology and application thereof, belong to the Natural Medicine Chemistry field.
Background technology
Herba Euphorbiae Humifusae is the herb of euphorbia plant Herba Euphorbiae Humifusae or Herba Euphorbiae supinae drying, is herbaceos perennial, has removing summer-heat poison, dampness removing jaundice eliminating, promoting blood circulation and hemostasis, the disease-resistant function such as former.Modern study shows that Herba Euphorbiae Humifusae mainly contains hydrolyzable tannin class and the flavone compounds such as Quercetin, kaempferol; Pharmacological research proves that it has the biological activitys such as antibiotic, antiviral, antioxidation, hepatoprotective, hemostasis.
Common water extract-alcohol precipitation or simple alcohol extraction are all adopted in the at present extraction of Herba Euphorbiae Humifusae, and its tannin, oil-soluble impurities is more, purity is low, dry after extract draw moist excessive.
Summary of the invention
The object of the present invention is to provide a kind of new Herba Euphorbiae Humifusae extract preparation technology, the extract for preparing through this technique has the good colibacillary effect in inhibition drug resistance fowl source.
The technical solution used in the present invention is: the preparation technology of Herba Euphorbiae Humifusae extract, it is characterized in that, and may further comprise the steps successively:
(1) get Herba Euphorbiae Humifusae, the alcohol reflux of adding 70% 2 times, each 3 hours, 70% amount of alcohol added was 8 times of Herba Euphorbiae Humifusae quality at every turn;
(2) merge extracted twice liquid, then extracting solution is joined in the concentration tank, temperature is 90 ± 1 ℃ and concentrates in the control concentration tank, to the concentrated solution relative density be 1.025;
(3) concentrated solution is put on the polyamide column, the difference water, 30% ethanol, 50% ethanol gradient elution, each gradient elution is to colourless; Collect 50% ethanol elution and put in the concentration tank, temperature is 90 ± 1 ℃ in the control concentration tank, and being concentrated into relative density is 1.025;
(4) 50% ethanol elution after will concentrating is sent into spray dryer, and intake air temperature is 180 ± 5 ℃ in the control container, and the air outlet temperature is 60～70 ℃, carries out spray drying and obtains the Herba Euphorbiae Humifusae extract being convenient to deposit.
The percent of above-mentioned ethanol is percetage by weight.
The main component of the Herba Euphorbiae Humifusae extract that above-mentioned technique makes and content are: total flavones (Quercetin, kaempferol, isoflavone, bisflavone, chalcone etc.) content is 24～27wt%, wherein take Quercetin as main, quercetin content is 12～14wt% in the Herba Euphorbiae Humifusae extract.
This extract has the good colibacillary effect in inhibition drug resistance fowl source.
The invention has the beneficial effects as follows: the product that behind the polyamide column eluting, obtains, removed the property cleared up tannin composition, make final extract obtain purification, carry out next step Application and Development for product and established solid foundation.The Herba Euphorbiae Humifusae extract that the experiment proved that the preparation of this technique has the good colibacillary effect in inhibition drug resistance fowl source.
The specific embodiment
Embodiment 1
1, instrument and material
Herba Euphorbiae Humifusae is built connection Chinese medicine company limited prepared slices of Chinese crude drugs factory available from the Jinan City, and the place of production is Shandong.
Polyamide column 40cm * 200cm manufacturing firm Tianjin atropic is Fine Chemical Co., Ltd hereby
Experimental strain: have chemical sproof fowl source escherichia coli through evaluation from clinical
2, Herba Euphorbiae Humifusae extract preparation
Get Herba Euphorbiae Humifusae medical material 50kg, put in the extraction pot, add 70% ethanol 400Kg, reflux 3 hours, filter, filtering residue adds 70% ethanol 400Kg, reflux 3 hours, filter, filtrate merges, and puts in the concentration tank, and temperature is 90 ± 1 ℃ in the control concentration tank, being concentrated into relative density is 1.025, lets cool.
Concentrated solution is put in 40cm * 200cm polyamide column, the adjusting eluent flow rate is 5L/min, wash with water to colourless (5 hours), use again 30% ethanol elution to colourless (4 hours), then use 50% ethanol elution to colourless (5 hours), collect 50% ethanol elution and put in the concentration tank, temperature is 90 ± 1 ℃ in the control concentration tank, being concentrated into relative density is 1.025, lets cool.
50% ethanol elution after concentrated is sent in the spray dryer, and intake air temperature is 180 ± 5 ℃ in the control container, and the air outlet temperature is 60～70 ℃, carries out spray drying, gets spray powder 2kg.
The percent of above-mentioned ethanol is percetage by weight.
3, Herba Euphorbiae Humifusae extract bacteriostatic experiment
3.1 medicinal liquid preparation: use the 10g extract, add the 100ml sterile distilled water, stir, 3000 turn/min is centrifugal, the removal insoluble matter, and autoclaving, and get final product.
3.2 the preparation of bacterial suspension: the drug resistance escherichia coli are inoculated in nutrient agar slant medium with inoculating loop, cultivated 24 hours for 37 ℃, propagate in aseptic broth bouillon, cultivated through 18 hours, propagate again and in aseptic broth bouillon, cultivated 6 hours, bacterial concentration is done dilution in 1: 100
3.3 bacteriostatic experiment: get aseptic small test tube, every pipe adds broth bouillon 1ml.Taking liquid 1ml adds the 1st pipe, get 1ml behind the mixing and add the 2nd pipe, the 1st pipe is added broth bouillon 1ml, get 1ml behind the 2nd pipe mixing and add the 3rd pipe, the 2nd pipe is added broth bouillon 1ml, so serial dilution to the 10 pipes, taking out 1ml from the 10th pipe discards, the 11st effective 2ml broth bouillon is done contrast, and such 1～10 pipe (was pressed the extract conversion namely 1: 40,1: 80......1: 20480) for the medicinal liquid of doubling dilution.The every pipe of the 1st～9 and the 11st pipe adds bacterium liquid 0.05ml, and the 10th pipe does not add bacterium liquid.With the abundant mixing of all test tubes, put 37 ℃ and cultivated observed result 24 hours.
3.4 the result judges: namely the 10th pipe is without Escherichia coli Growth to require the medicinal liquid control tube, and bacterium liquid control tube i.e. the 11st pipe has Escherichia coli Growth normal, tests valid.Take the high dilution of the medicinal liquid that suppresses Escherichia coli Growth as antibacterial potency.Take the high dilution that can suppress Escherichia coli Growth as minimum inhibitory concentration MIC.Experiment repeats 3 times.
The result shows: the Herba Euphorbiae Humifusae extract of this technique preparation is 5120 to the colibacillary minimum inhibitory concentration MIC in chemical sproof fowl source.
4, quercetin content is measured
4.1 chromatographic condition and system suitability are take octadecylsilane chemically bonded silica as filler; Take methanol-0.4% phosphoric acid solution (50: 50) as mobile phase; Detect wavelength 360nm.
4.2 the accurately weighed Quercetin reference substance of the preparation of reference substance solution is an amount of, adds 80% methanol and makes the solution that every 1mL contains 20 μ g, and get final product.
4.3 the about 0.03g of this product powder is got in the preparation of need testing solution, and is accurately weighed, puts in the tool plug conical flask, the accurate 80% methanol 50mL that adds, sealing, weighed weight, supersound extraction 5 minutes is taken out, more weighed weight, supply the weight that subtracts mistake with 80% methanol, shake up, filter, precision is measured subsequent filtrate 20mL, the accurate 25% hydrochloric acid 7mL that adds, put in 85 ℃ of water-baths and be hydrolyzed 30min, take out, let cool rapidly, go in the 50mL volumetric flask, and add methanol and be diluted to scale, shake up, filter, get subsequent filtrate, and get final product.
4.4 algoscopy is accurate reference substance solution and each 10 μ L of need testing solution of drawing respectively, the injection liquid chromatography is measured, and be get final product.
4.5 computing formula:
R
S: the peak area of need testing solution; C
r: the concentration of reference substance solution;
C
S: the concentration of need testing solution; R
r: the peak of reference substance solution
Content by calculating this product Quercetin is 13.3%.
Claims (2)
1. the preparation technology of a Herba Euphorbiae Humifusae extract is characterized in that, may further comprise the steps successively:
(1) get Herba Euphorbiae Humifusae, the alcohol reflux of adding 70% 2 times, each 3 hours, 70% amount of alcohol added was 8 times of Herba Euphorbiae Humifusae quality at every turn;
(2) merge extracted twice liquid, then extracting solution is joined in the concentration tank, temperature is 90 ± 1 ℃ and concentrates in the control concentration tank, to the concentrated solution relative density be 1.025;
(3) concentrated solution is put on the polyamide column, the difference water, 30% ethanol, 50% ethanol gradient elution, each gradient elution is to colourless; Collect 50% ethanol elution and put in the concentration tank, temperature is 90 ± 1 ℃ in the control concentration tank, and being concentrated into relative density is 1.025;
(4) 50% ethanol elution after will concentrating is sent into spray dryer, and intake air temperature is 180 ± 5 ℃ in the control container, and the air outlet temperature is 60～70 ℃, carries out spray drying and makes product.
2. the prepared Herba Euphorbiae Humifusae extract of claim 1 suppresses the application of the medicine aspect the escherichia coli of drug resistance fowl source in preparation.
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| CN111643573A (en) * | 2020-07-09 | 2020-09-11 | 江苏农牧科技职业学院 | Traditional Chinese medicine composition for preventing and treating duck colibacillosis and preparation method and application thereof |
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