CN102772790B - Compound echinacea purpurea preparation and preparation method and application thereof - Google Patents
Compound echinacea purpurea preparation and preparation method and application thereof Download PDFInfo
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- CN102772790B CN102772790B CN201210217520.9A CN201210217520A CN102772790B CN 102772790 B CN102772790 B CN 102772790B CN 201210217520 A CN201210217520 A CN 201210217520A CN 102772790 B CN102772790 B CN 102772790B
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Abstract
The invention discloses a compound echinacea purpurea preparation. The dose ratio of an echinacea purpurea extract as an effective component to lysozyme is (4-1):1, the dosage of the echinacea purpurea extract and the lysozyme is 20% in total, and the ajudvants contains 64% of saccharose and 16% of dextrin. The echinacea purpurea extract selected by the invention is obtained by extracting echinacea purpurea medicinal material by alkaline ethanol solution and lysozyme for two times, wherein the content of polysaccharide is not less than 21.5%, the content of polyphenol is not less than 8.10% and the content of chicoric acid is not less than 5.00%. The compound preparation provided by the invention has the effects of improving animal immunity, antibiosis and anti-virus, thereby being capable of being taken as the medicine for preventing and treating the animal diseases, in particular to the chicken diseases caused by escherichia coli infections.
Description
Technical field
The invention belongs to plant amedica goods field, relate to a kind of animal immunity potentiator, specifically, relate to a kind of compound recipe Echinacea granule and its preparation method and application.
Background technology
Echinacea is a kind of Echinacea plant that originates in North America and Canada south, and China introduces a fine variety some areas.In Echinacea, contain polysaccharide, polyphenol (comprising chicoric acid, caffeinic derivant), flavonoid, quintessence oil, polyacetylene, alkylamine and alkaloid.There is the immunity of raising and antibacterial and anti-inflammation functions.Polysaccharide can excite the cell of health to go infection; Polyphenols, flavonoid and caffeic acid derivant can improve the immunity of body, and their energy stimulating immune system cellular activities, in the time that these cells have activity, leukocyte surrounds the invader who causes disease more rapidly, make virus or antibacterial death, prevent that them from breeding, or stop their activity.Especially chicoric acid is one of immune active ingredient very important in Echinacea.Pharmacological research in recent years shows, chicoric acid has the immunologic function of enhancing and antiinflammatory action, and can suppress hyaluronidase, and protection collagen protein is avoided the impact of the free radical that can cause degraded.Abroad have Echinacea and preparation thereof for the breeding of pig and the treatment of respiratory syndrome, domestic clinical trial also confirms that the diseases such as the infectious bursal disease, infectious bronchitis, atypical newcastle of circovirus disease, breeding and the respiratory syndrome of Echinacea to pig and chicken have good curative effect.
But, use separately Echinacea in the time for the treatment of severe disease, only depend on the immune system that stimulates body, improve the immunity of body, a little less than its bactericidal antiphlogistic effect.Curative effect is unsatisfactory, and therefore, the medicine of the other types that searching can have complementary functions with Echinacea, builds with it compound formulation, is another outlet of further developing Echinacea purposes.
Molten lysozyme claims again muramidase or N-acetylmuramide lycanohydrlase, is a kind of alkaline enzyme that can be hydrolyzed mucopolysaccharide in pathogenic bacterium, has the natural infection material of bactericidal action.Mainly, by the-acetylmuramic acid in destruction cell wall and the β-Isosorbide-5-Nitrae glycosidic bond between NAG, make the insoluble mucopolysaccharide of cell wall resolve into solubility glycopeptide, cause cell wall rupture content to be overflowed and make bacterolysis.Lysozyme also can the direct combination with electronegative virus protein, forms double salt with DNA, RNA, apoprotein, makes virally inactivated.The effects such as that this enzyme has is antibacterial, antiinflammatory, antiviral.The antimicrobial spectrum of lysozyme is wider, is not only confined to gram positive bacteria, and part gram negative bacteria is also had to inhibition.Lysozyme directly kill pathogenic bacterium function, can make up the deficiency of Echinacea.But lysozyme itself is without the effect of enhancing immunity, alone lysozyme, the body that the function causing for Long-term Infection antibacterial, virus declines, curative effect is not remarkable.And Echinacea raising immunity of organisms function is extremely strong, can excite the cell of health to go infection, just make up the deficiency of lysozyme.
But still less to the compound research of Echinacea and lysozyme both at home and abroad, mostly both are independent use.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, a kind of compound recipe Echinacea preparation is provided, it is taking Echinacea extract and lysozyme as effective ingredient, processes taking sucrose and dextrin as adjuvant.
The inventor is definite through the drug effect contrast screening of bacteriostatic test contrast and practical application, and in the compound preparation of above-mentioned Echinacea extract and lysozyme, the quality usage ratio of effective ingredient Echinacea extract and lysozyme is (4～1): 1.
Wherein, the quality usage ratio of preferred Echinacea extract and lysozyme is 3: 1.
The compound preparation of Echinacea extract of the present invention and lysozyme is a kind of compound granular formulation, and wherein, total consumption of effective ingredient Echinacea extract and lysozyme is 20%, total consumption 80% of adjuvant sucrose and dextrin, wherein, dosage of sucrose is 64%, and dextrin consumption is 16%.
(raw material consumption of the present invention is all in mass, as follows)
The preparation method of the compound granular formulation of Echinacea extract of the present invention and lysozyme is as follows:
Get Echinacea extract and mix with lysozyme, add the purified water of 1.2 times of mixture qualities, stir, obtain Echinacea extract-lysozyme mixed liquor; Get dextrin and sucrose, mix homogeneously, drops into fluid bed, then Echinacea is got to thing-lysozyme mixed liquor under 50 DEG C of conditions and is sprayed onto on the mixture of dextrin and sucrose, obtains effective ingredient and be 20% compound recipe Echinacea granular preparation again.
Also can get Echinacea extract mixes with lysozyme; then add dextrin and sucrose; mix homogeneously; add again 80% alcoholic solution of mixture gross mass 30%; and mix homogeneously, make Echinacea extract-lysozyme soft material, this soft material is made to wet granular by oscillating granulator; again by wet granular 50 DEG C of oven dry, obtain effective ingredient and be Echinacea-lysozyme compound granular formulation of 20%.
The compound preparation of Echinacea extract provided by the present invention and lysozyme, that Echinacea extract and the lysozyme of studying preparation by the inventor is effective ingredient, add that suitable auxiliary element is composite to be processed into, in the Echinacea extract using, polyphenol content >=8.10%, chicoric acid content >=5.00%; Ministry of Public Health ministry standard (first of the biochemical drug) standard that the lysozyme using is carried out, content is 6350 units/mg.
Above-mentioned compound recipe Echinacea preparation has raising animal immunizing power, antibacterial, antiviral functions, can be used as prevention and treatment Animal diseases medicine.
Because the extracting method of Echinacea extract is in the market mainly simple water logging and alcohol extraction, cause extraction efficiency on the low side, exist a certain active constituent content higher, and the lower shortcoming of all the other active constituent contents, thereby affect result of use.For ensureing its curative effect, inventor research provides a kind of extracting method of uniqueness, and the content that makes polysaccharide, polyphenol and chicoric acid in prepared extract is all apparently higher than the prepared Echinacea extract of conventional method in the market.
Echinacea extract provided by the present invention adopts alkaline ethanol solution and lysozyme Echinacea medical material is carried out to extracted twice and obtain, wherein: polyoses content >=21.50%, polyphenol content >=8.70%, chicoric acid content >=5.00%.
The preparation method of Echinacea extract provided by the present invention, is to adopt reflux, extract, in 10～60% alcoholic solution that are first 12 by Echinacea medical material at pH, then, then filtering residue is soaked to the two step extracting method that extract with 1% Lysozyme in Aqueous Solution.
The concrete preparation method of Echinacea extract of the present invention is as follows:
Get 8 parts of concentration and be 10% to 60% alcoholic solution (preferably 30%), with Ca (OH) 2 adjusting pH value to 12, get 1 part of Echinacea medical material, decontamination, pulverizing, be soaked in above-mentioned alkaline ethanol solution 1 hour, and reflux, extract, 3 times, each 2 hours, filter, merging filtrate, obtains filtrate and filtering residue two parts; Filtering residue adds the Lysozyme in Aqueous Solution of 10 times of amounts 1%, and 37 DEG C are soaked 12 hours, filter, and discard precipitation, and filtrate merges with alcohol extract before, obtains Echinacea extracting solution.Filtrate is regulated to pH to 4 ~ 6 with HCl, leave standstill 3 hours, filter, precipitation drying and crushing, obtains Echinacea precipitated powder; Filtrate recycling ethanol is extremely without alcohol taste, and to be concentrated into density be 1.15g/ml, spraying is dry, gained Echinacea powder mixes with Echinacea precipitated powder, Echinacea extract (in the present invention, related consumption umber or percent are except indicating especially, be in mass fraction or quality %, as follows).
In said extracted method, use the alkaline ethanol solution that pH is 12 to carry out reflux, extract, to Echinacea medical material, be conducive to improve the content of polyphenol and chicoric acid in extract, greatly improved extract obtained effectiveness; The main component of plant cell wall is cellulose and pectin, lysozyme can destroy its structure, in filtering residue after ethanol extraction, add appropriate lysozyme, can make the cell wall of Echinacea cell destroy, effective ingredient polysaccharide, polyphenol and chicoric acid wherein are further discharged, improved the extraction ratio of Echinacea.
The present invention also provides a kind of compound recipe Echinacea preparation, using the extract of Echinacea and lysozyme as main effective ingredient, in effective potentiation ratio range, carries out compositely, makes both produce cooperative compensating and potentiation, improves sterilization and disease-resistant function; Add adjuvant and make compound recipe Echinacea granular preparation, both can make convenient drug administration, can improve again the taste of Echinacea, can also be convenient to storage, transport.
Echinacea can improve immunity of organisms, excites the cell of health to go infection, and lysozyme can directly be killed pathogenic bacterium, and both couplings can improve immunity of organisms, can directly kill pathogenic bacterium again, play antiinflammation, treating both the principal and secondary aspects of a disease.Compound formulation of the present invention, has realized the coupling of Echinacea and lysozyme, the better efficacy more any than independent use, and Echinacea, lysozyme are compared with antibiotic, in use all can not produce drug resistance.Lysozyme directly kill pathogenic bacterium function, can make up the deficiency of Echinacea, but without the effect of enhancing immunity; Alone lysozyme, the body that the function causing for Long-term Infection antibacterial, virus declines, curative effect is very micro-, and that Echinacea improves immunity of organisms function is extremely strong, can excite the cell of health to go infection, just makes up the deficiency of lysozyme.Evidence, both couplings, can improve immunity of organisms, can directly kill pathogenic bacterium again, play antiinflammation, and treating both the principal and secondary aspects of a disease, has synergistic function.
Use separately Echinacea in the time for the treatment of severe disease, only depend on the immune system that stimulates body, improve the immunity of body, curative effect is unsatisfactory, uses separately the effect of Echinacea bactericidal antiphlogistic very micro-.And use separately lysozyme, because lysozyme is without the effect of enhancing immunity, the body that the function causing for Long-term Infection antibacterial, virus declines is several without any curative effect.Compound Echinacea preparation provided by the present invention, has realized the coupling of Echinacea and lysozyme, the better efficacy more any than independent use, and Echinacea, lysozyme are compared with antibiotic, in use all can not produce drug resistance, and without recurrence, drug residue free, safety is higher.
Clinical test results demonstration, compound recipe Echinacea granular preparation of the present invention is respond well to treatment chicken colibacillosis.
Detailed directions consumption is as follows:
(1) the mixed drink of prevent disease: in every 1000kg water; Compound recipe Echinacea granular preparation consumption: chicken 100g; Pig 500-1000g, is used in conjunction 10 days.
(2) the mixed drink for the treatment of disease: every 1000kg water, compound recipe Echinacea granular preparation consumption: chicken 200g; Pig 1500-2500g, is used in conjunction 5 days.
Below in conjunction with test method, reasonability of the present invention is described.
Detailed description of the invention
Embodiment mono-. the preparation method of Echinacea extract of the present invention and lysozyme compound preparation.
Embodiment mono-.1. Echinacea extract: lysozyme=4: the preparation of 1 compound granular formulation
Get Echinacea extract 160g, lysozyme 40g, adds purified water 240g, stirs, and obtains Echinacea extract-lysozyme mixed liquor; Get dextrin 160g, sucrose 640g, mix homogeneously, drops into fluid bed again; Then Echinacea is got to thing-lysozyme mixed liquor under 50 DEG C of conditions and be sprayed onto on the mixture of dextrin and sucrose, obtain effective ingredient and be 20% Echinacea lysozyme compound granular formulation; Wherein, Echinacea extract 16%, lysozyme 4%, sucrose 64%, dextrin 16%.
Embodiment mono-.2. Echinacea extract: lysozyme=3: the preparation of 1 compound granular formulation
Get Echinacea extract 150g, lysozyme 50g, adds purified water 240g, stirs, and obtains Echinacea extract-lysozyme mixed liquor; Get dextrin 160g, sucrose 640g, mix homogeneously, drops into fluid bed again; Then Echinacea is got to thing-lysozyme mixed liquor under 50 DEG C of conditions and be sprayed onto on the mixture of dextrin and sucrose, obtain effective ingredient and be Echinacea-lysozyme compound granular formulation of 20%; Wherein, Echinacea extract 15%, lysozyme 5%, sucrose 64%, dextrin 16%.
Embodiment mono-.3. Echinacea extract: lysozyme=1: the preparation of 1 compound granular formulation
Get Echinacea extract 100g, lysozyme 100g, adds purified water 240g, stirs, and obtains Echinacea extract-lysozyme mixed liquor; Get dextrin 160g, sucrose 640g, mix homogeneously, drops into fluid bed again; Then Echinacea is got to thing-lysozyme mixed liquor under 50 DEG C of conditions and be sprayed onto on the mixture of dextrin and sucrose, obtain effective ingredient and be 20% Echinacea lysozyme compound granular formulation; Wherein, Echinacea extract 10%, lysozyme 10%, sucrose 64%, dextrin 16%.
Embodiment bis-. in compound recipe Echinacea preparation of the present invention, the preferred and Piglet s colibacillosis of the usage ratio of effective ingredient Echinacea extract and lysozyme.
Embodiment bis-.1.
The colibacillary effect comparison of vitro inhibition of the Echinacea extract of different proportion and the compound preparation of lysozyme
(1) experiment material
Test strain: broiler source escherichia coli.
Culture medium: III culture medium (pressing 2010 editions preparations of Chinese veterinary pharmacopoeia).
Compound preparation prescription:
Prescription 1: Echinacea extract: lysozyme=5: 1,
Prescription 2: Echinacea extract: lysozyme=4: 1,
Prescription 3: Echinacea extract: lysozyme=3.5: 1,
Prescription 4: Echinacea extract: lysozyme=3: 1,
Prescription 5: Echinacea extract: lysozyme=2.5: 1,
Prescription 6: Echinacea extract: lysozyme=2: 1,
Prescription 7: Echinacea extract: lysozyme=1.5: 1,
Prescription 8: Echinacea extract: lysozyme=1: 1,
Prescription 9: Echinacea extract: lysozyme=1: 2,
Make respectively the composite particles preparation of active constituent content 20%,
Negative control group: normal saline.
Each 100 grams of granule getting above each prescription, is placed in conical flask, adds sterilized water 100ml, stirs moltenly, boils 15 minutes.1000 revs/min centrifugal 10 minutes, get supernatant, 121 DEG C of sterilizings 15 minutes, 4 DEG C of Refrigerator stores are for subsequent use.
(2) experiment content
The preparation of antibacterial flat board: get diameter 90mm, the flat pair of dish of high 16～17mm, injects respectively 60 DEG C of aseptic III culture medium 20ml, makes at the bottom of dish, evenly to spread out cloth, places on level table and makes to solidify, as bottom.Separately get after the appropriate heating of culture medium dissolves, let cool to 48～50 DEG C, add the appropriate 5ml of broiler source escherichia coli suspension, make on bottom evenly stand cloth, as bacterium layer.Be placed on cooling on horizontal stand after, make antibacterial flat board.
The drug sensitive experiment of escherichia coli to difference prescription: the particle solution of above different prescriptions is made drug sensitive test paper by paper disk method, measures the size of inhibition zone.Method: cut-off footpath is that the sterilizing filter paper of 0.6 centimetre soaks 40 minutes in the particle solution of difference prescription, take out for subsequent use, in the antibacterial flat board having prepared, drug sensitive test paper is placed by sterile working, 6 of every kind of medicine pastes, then flat board is put in 37 DEG C of incubators and cultivated the size of measuring inhibition zone after 24 hours, get its meansigma methods.And its meansigma methods and negative control group data are compared, and carry out data analysis with SAS statistical software.
(3) experimental result
| Prescription number | Prescription 1 | Prescription 2 | Prescription 3 | Prescription 4 | Prescription 5 | Prescription 6 | Prescription 7 | Prescription 8 | Prescription 9 | Negative control group |
| Inhibition zone (mm) | 0.81 | 1.64 | 2.77 | 3.03 | 3.10 | 3.12 | 3.11 | 3.13 | 3.12 | 0 |
| Significant difference | P>0.05 | P<0.05 | P<0.05 | P<0.05 | P<0.05 | P<0.05 | P<0.05 | P<0.05 | P<0.05 | - |
Can be found out by above data, when Echinacea extract: when lysozyme is 4: 1, along with the increase of lysozyme proportion, its fungistatic effect obviously strengthens; When Echinacea extract: after lysozyme reaches 3: 1, along with the rising of lysozyme proportion, its fungistatic effect increases not obvious.Therefore single from In Vitro Bacteriostasis effect, Echinacea extract: the usage ratio of lysozyme is that 4: 1 to 1: 1 fungistatic effects are all more satisfactory; Consider, can be by Echinacea extract: the preferable amount ratio of lysozyme is confirmed as 3: 1.
Embodiment bis-.2.
Taking the body weight of broiler as index, the usage ratio of screening Echinacea extract and lysozyme
Test site: Shandong Jia Yi plant
Test chicken situation: healthy broiler, 4 week age.
Test recipe:
Prescription 1: Echinacea extract: lysozyme=5: 1,
Prescription 2: Echinacea extract: lysozyme=4: 1,
Prescription 3: Echinacea extract: lysozyme=3: 1,
Prescription 4: Echinacea extract: lysozyme=2: 1,
Prescription 5: Echinacea extract: lysozyme=1: 1,
Prescription 6: Echinacea extract: lysozyme=1: 2,
Prescription 7: Echinacea extract: lysozyme=1: 3,
Prescription 8: Echinacea extract: lysozyme=1: 4,
Prescription 9: Echinacea extract: lysozyme=1: 5,
Prescription 10: Echinacea extract: lysozyme=1: 0,
Prescription 11: Echinacea extract: lysozyme=0: 1,
The composite particles preparation 100g that makes respectively active constituent content 20%, is watered 500kg, drinks for test broiler, is used in conjunction 5 days;
Negative control group: normal saline is freely drunk.
Experiment grouping and processing:
Test broiler 300 plumages, are divided into 12 groups, every group of 25 plumages at random.Press therapeutic scheme administration.
Contrast on effect:
Second day after last administration, weighs, and carries out significant difference comparison with negative control group.
| prescription | broiler average weight (kg) | significant difference |
| prescription 1 | 1.54 | p>0.05 |
| prescription 2 | 1.66 | p<0.05 |
| prescription 3 | 1.71 | p<0.05 |
| prescription 4 | 1.64 | p<0.05 |
| prescription 5 | 1.58 | p<0.05 |
| prescription 6 | 1.55 | p>0.05 |
| prescription 7 | 1.54 | p>0.05 |
| prescription 8 | 1.50 | p>0.05 |
| prescription 9 | 1.52 | p>0.05 |
| prescription 10 | 1.51 | p>0.05 |
| prescription 11 | 1.46 | p>0.05 |
| negative control group | 1.43 | -. |
Can be found out by above data, when Echinacea extract and lysozyme ratio are between 4: 1～1: 1, broiler weight weightening finish obviously, relatively has significant difference with negative control group; And, when Echinacea extract: lysozyme=3: 1 time, broiler weight weightening finish is the most obvious, illustrates, the optimal proportion of Echinacea extract and lysozyme is 3: 1.
Embodiment bis-.3.
Sick chicken water drinking test and Comparison of therapeutic
Test site: Shandong Jia Yi plant
Chicken house incidence: sick pertussis is coughed and dyspnea, arranges white, yellow green or green loose stool, and around feather is contaminated for anus, and down in spirits, the necking down of eye half are stayed and stood, two wings are sagging.
Test chicken situation: test chicken sum 4000 plumages, 8 week age.
Therapeutic scheme and contrast:
From putting forward Echinacea group: single giving from carrying Echinacea extract 20g+ sucrose 64g+ dextrin 16g, be watered 500kg, be used in conjunction 5 days.
Commercially available Echinacea group: list is given commercially available Echinacea extract 20g+ sucrose 64g+ dextrin 16g, is watered 500kg, is used in conjunction 5 days.
Lysozyme group: single lysozyme 20g+ sucrose 64g+ dextrin 16g that gives, be watered 500kg, be used in conjunction 5 days.
Compound recipe Echinacea groups of grains 1: Echinacea extract: lysozyme=3:1, prepare granule by embodiment 1 method, 100g compound recipe Echinacea granule is watered 500kg, is used in conjunction 5 days.
Compound recipe Echinacea groups of grains 2: Echinacea extract: lysozyme=4:1, prepare granule by embodiment 1 method, 100g compound recipe Echinacea granule is watered 500kg, is used in conjunction 5 days.
Compound recipe Echinacea groups of grains 3: Echinacea extract: lysozyme=1:1, prepare granule by embodiment 1 method, 100g compound recipe Echinacea granule is watered 500kg, is used in conjunction 5 days.
Positive controls: colistine sulfate soluble powder, 100g is watered 400kg, is used in conjunction 5 days.
Experiment grouping and processing:
Test chicken is totally 3000 ptilosis chickens, is divided at random 6 groups, every group of 500 plumages.Press therapeutic scheme administration.
Curative effect determinate standard: cure: through treatment and transference cure, feces, diet want and mental restoration normal; Effective: symptom obviously alleviates, feces, spirit, diet are wanted to take a favorable turn; Invalid or dead: through treating its symptom without taking a turn for the better or death, cuing open inspection has obvious pericarditis, the scorching pathological changes of Glisson's capsule.
Cure rate=(curing the sick chicken number of sick chicken number/group innerlich anwenden in group) × 100%
Effective percentage=(the sick chicken number of effective sick chicken number/group innerlich anwenden in group) × 100%
Mortality rate=(the sick chicken number of dead sick chicken number/group innerlich anwenden in group) × 100%
Comparison of therapeutic:
Second day after last administration, observe the curative effect.
As can be seen from the above results, certainly carry the more commercially available Echinacea group of Echinacea group cure rate high, mortality rate is low, and body weight increase obviously, illustrates from putting forward the more commercially available Echinacea extract curative effect of Echinacea extract curative effect and obviously will get well; Compound recipe Echinacea granule more alone Echinacea, lysozyme and positive controls on to sick chicken cure rate and weight gain effect have significant difference, and cure rate obviously raises, and mortality rate significantly reduces and body weight increases obviously; Especially when Echinacea extract: when lysozyme=3:1, mortality rate obviously declines.
Embodiment tri-. the preparation method of Echinacea extract and Experimental Comparison
Reflux, extract, in 30% alcoholic solution that embodiment tri-.1. are 12 at pH, filtering residue soaks and extracts with 1% Lysozyme in Aqueous Solution again
Get Echinacea medical material 2kg, add 16kg concentration and be 30% alcoholic solution, regulate pH to 12 with Ca (OH) 2, soak 1 hour, and reflux, extract, 3 times, each 2 hours, merge extractive liquid,, double-deck filter paper sucking filtration, merging filtrate, obtains alcohol extract; Filtering residue adds the Lysozyme in Aqueous Solution of 20kg1%, and 37 DEG C are soaked 12 hours, filter, and discard filtering residue, double-deck filter paper sucking filtration for extracting solution, and filtrate merges with alcohol extract before, with hydrochloric acid adjust pH to 4.7, leaves standstill 3 hours; Filter, precipitation crushed after being dried obtains Echinacea precipitated powder 124g, and filtrate decompression is recycled to without alcohol taste and to be concentrated into density be 1.15g/ml, and the dry Echinacea powder 281g that to obtain of spraying, is mixed to get 405g Echinacea extract with Echinacea precipitated powder.
By uv-spectrophotometric instrument, the content of polysaccharide and polyphenol in above-mentioned Echinacea extract is detected, result, for containing polysaccharide 24.71%, contains polyphenol 8.66%; By high performance liquid chromatograph, chicoric acid content in above-mentioned Echinacea extract is detected, result is for containing chicoric acid 5.22%.
Reflux, extract, in 10% alcoholic solution that embodiment tri-.2. are 12 at pH, filtering residue soaks and extracts with 1% Lysozyme in Aqueous Solution again
Get Echinacea medical material 2kg, add 16kg concentration and be 10% alcoholic solution, regulate pH to 12 with Ca (OH) 2, soak 1 hour, and reflux, extract, 3 times, each 2 hours, merge extractive liquid,, double-deck filter paper sucking filtration, merging filtrate, obtains alcohol extract; Filtering residue adds the Lysozyme in Aqueous Solution of 20kg1%, and 37 DEG C are soaked 12 hours, filter, and discard filtering residue, double-deck filter paper sucking filtration for extracting solution, and filtrate merges with alcohol extract before, with hydrochloric acid adjust pH to 4.7, leaves standstill 3 hours; Filter, precipitation crushed after being dried obtains Echinacea precipitated powder 121g, and filtrate decompression is recycled to without alcohol taste and to be concentrated into density be 1.15g/ml, and the dry Echinacea powder 287g that to obtain of spraying, is mixed to get 408g Echinacea extract with Echinacea precipitated powder.
By uv-spectrophotometric instrument, the content of polysaccharide and polyphenol in above-mentioned Echinacea extract is detected, result, for containing polysaccharide 25.23%, contains polyphenol 8.11%; By high performance liquid chromatograph, chicoric acid content in above-mentioned Echinacea extract is detected, result is for containing chicoric acid 5.05%.
Reflux, extract, in 60% alcoholic solution that embodiment tri-.3. are 12 at pH, filtering residue soaks and extracts with 1% Lysozyme in Aqueous Solution again
Get Echinacea medical material 2kg, add 16kg concentration and be 60% alcoholic solution, regulate pH to 12 with Ca (OH) 2, soak 1 hour, and reflux, extract, 3 times, each 2 hours, merge extractive liquid,, double-deck filter paper sucking filtration, merging filtrate, obtains alcohol extract; Filtering residue adds the Lysozyme in Aqueous Solution of 20kg1%, and 37 DEG C are soaked 12 hours, filter, and discard filtering residue, double-deck filter paper sucking filtration for extracting solution, and filtrate merges with alcohol extract before, with hydrochloric acid adjust pH to 4.7, leaves standstill 3 hours; Filter, precipitation crushed after being dried obtains Echinacea precipitated powder 125g, and filtrate decompression is recycled to without alcohol taste and to be concentrated into density be 1.15g/ml, and the dry Echinacea powder 272g that to obtain of spraying, mixes with Echinacea precipitated powder, is total to and obtains 397g Echinacea extract.
By uv-spectrophotometric instrument, the content of polysaccharide and polyphenol in above-mentioned Echinacea extract is detected, result, for containing polysaccharide 21.71%, contains polyphenol 8.71%; By high performance liquid chromatograph, chicoric acid content in above-mentioned Echinacea extract is detected, result is for containing chicoric acid 5.28%.
The conventional water boiling and extraction of embodiment tri-.4.
Get Echinacea medical material 2kg, add 16kg water, soak 1 hour, decoct 3 times, each 2 hours, merge decocting liquid, double-deck filter paper sucking filtration, merging filtrate, it is 1.15g/ml that filtrate is concentrated into density, filters, filtrate spraying is dry, obtains Echinacea powder 364g.
By uv-spectrophotometric instrument, the content of polysaccharide and polyphenol in above-mentioned Echinacea extract is detected, result, for containing polysaccharide 19.46%, contains polyphenol 3.62%; By high performance liquid chromatograph, chicoric acid content in above-mentioned Echinacea extract is detected, result is for containing chicoric acid 0.36%.
The conventional ethanol extraction of embodiment tri-.5.
Get Echinacea medical material 2kg, add 16kg concentration and be 30% alcoholic solution, soak 1 hour, and reflux, extract, 3 times, each 2 hours, merge extractive liquid,, double-deck filter paper sucking filtration, merging filtrate, decompression filtrate recycling ethanol is extremely without alcohol taste, continuing to be concentrated into density is 1.15g/ml, and spraying is dry, obtains Echinacea powder 261g.
By uv-spectrophotometric instrument, the content of polysaccharide and polyphenol in above-mentioned Echinacea extract is detected, result, for containing polysaccharide 16.92%, contains polyphenol 5.43%; By high performance liquid chromatograph, chicoric acid content in above-mentioned Echinacea extract is detected, result is for containing chicoric acid 1.24%.
Can find out by five experiment comparative examples of embodiment tri-.1-5.:
1) reflux, extract, in 10～60% alcoholic solution that are 12 at pH by Echinacea medical material that the present invention is selected, filtering residue soaks with 1% Lysozyme in Aqueous Solution the two step extracting method that extract again, the Echinacea extract that more current conventional extracting method obtains, yield is high, and the content of effective ingredient polysaccharide, polyphenol, chicoric acid all significantly increases.
2) reflux, extract, in 30% alcoholic solution that is 12 at pH by Echinacea that the present invention is selected, the amount of the Echinacea extract that filtering residue obtains with the two step extracting method that 1% Lysozyme in Aqueous Solution immersion is extracted again, for 1.6 times of existing 30% alcoholic solution extracting method, the content of effective ingredient chicoric acid
For the more than 4 times of existing 30% alcoholic solution extracting method; Effect is remarkable.
3) technique of comprehensive embodiment mono-.1-3. and associated score are according to analysing, can confirm, reflux, extract, in 30% alcoholic solution that is 12 at pH described in embodiment mono-.1., filtering residue soaks with 1% Lysozyme in Aqueous Solution the technical scheme of extracting again and should be the optimal technical solution of preparing Echinacea extract.
By above 5 experiments, illustrate that the more current conventional extracting method of the present invention's extracting method used extracts the Echinacea extract obtaining, quality is many, and the content of the effective ingredient such as polysaccharide, polyphenol, chicoric acid all significantly increases.
Claims (3)
1. a compound recipe Echinacea preparation, is characterized in that described preparation is made up of Echinacea extract, lysozyme, sucrose, dextrin; The usage ratio of Echinacea extract and lysozyme is 3: 1, and the mass fraction of each component is Echinacea extract 15%, lysozyme 5%, sucrose 64%, dextrin 16%; In described preparation, selected Echinacea extract is to adopt reflux, extract, in the alcoholic solution that is first 12 by Echinacea medical material at pH, again filtering residue is obtained with the two step extracting method that 1% Lysozyme in Aqueous Solution immersion is extracted, its concrete process for extracting is: get the alcoholic solution that 8 parts of concentration are 30%, with Ca (OH)
2regulate pH value to 12; By 1 part of Echinacea medical material, decontamination, pulverizing, be soaked in above-mentioned alkaline ethanol solution 1 hour, and reflux, extract, 3 times, and each 2 hours, filter, merging filtrate, obtains filtrate and filtering residue two parts; Filtering residue adds 1% Lysozyme in Aqueous Solution that weight is 10 times of Echinacea medical material weight, and 37 DEG C are soaked 12 hours, filter, and discard precipitation, and filtrate merges with alcohol extract before, obtains Echinacea extracting solution; The Echinacea extracting solution of upper step gained is regulated to pH to 4 ~ 6 with HCl, leave standstill 3 hours, filter, precipitation drying and crushing, obtains Echinacea precipitated powder; Filtrate recycling ethanol is to without alcohol taste, and to be concentrated into density be 1.15g/ml, and spraying is dry, and gained Echinacea powder mixes with Echinacea precipitated powder, acquisition Echinacea extract; Wherein, polyoses content>=21.50%, polyphenol content>=8.10%, chicoric acid content>=5.00%.
2. the preparation method of compound recipe Echinacea preparation as claimed in claim 1, is characterized in that concrete operations processing step is as follows:
Get the Echinacea extract that two step extracting method described in claim 1 and concrete extraction process thereof obtain, mix with lysozyme, add the purified water of 1.2 times of mixture qualities, stir, obtain Echinacea extract-lysozyme mixed liquor; Get dextrin and sucrose, mix homogeneously, drops into fluid bed, then under 50 DEG C of conditions, Echinacea extract-lysozyme mixed liquor is sprayed onto on the mixture of dextrin and sucrose, obtains effective ingredient and be 20% compound recipe Echinacea granular preparation again.
3. the application of compound recipe Echinacea preparation as claimed in claim 1, is characterized in that as preparation prevention and treats the medicine because of the fowl disease of coli-infection initiation.
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| CN106389788B (en) * | 2016-11-14 | 2019-09-13 | 青岛农业大学 | It is a kind of for enhancing the drug extract, preparation and preparation method of immunologic function of livestock and birds and anti-virus ability |
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Inventor after: Wang Haiting Inventor after: Cui Jin Inventor after: Li Youzhi Inventor after: Li Baohua Inventor after: Li Chengying Inventor after: Ran Rong Inventor after: Wang Yaqi Inventor after: Wu Lianyong Inventor after: Kong Mei Inventor after: Tian Yuzhu Inventor before: Wang Haiting Inventor before: Li Chengying Inventor before: Ran Rong Inventor before: Wang Yaqi Inventor before: Wu Lianyong Inventor before: Kong Mei Inventor before: Tian Yuzhu Inventor before: Cui Jin |
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Effective date of registration: 20171127 Address after: Industrial Road Licheng District, Ji'nan city of Shandong Province, No. 243 250100 Co-patentee after: SHANDONG PROVINCE VETERINARY DRUG QUALITY INSPECTION Patentee after: Qilu Animal Health Products Co., Ltd. Address before: No. 234, industrial North Road, Ji'nan City, Shandong, Shandong Patentee before: Qilu Animal Health Products Co., Ltd. |