CN100438886C - Chrysanthem pain relieving medicinal preparation - Google Patents
Chrysanthem pain relieving medicinal preparation Download PDFInfo
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- CN100438886C CN100438886C CNB031304788A CN03130478A CN100438886C CN 100438886 C CN100438886 C CN 100438886C CN B031304788 A CNB031304788 A CN B031304788A CN 03130478 A CN03130478 A CN 03130478A CN 100438886 C CN100438886 C CN 100438886C
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- flos chrysanthemi
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- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 208000002193 Pain Diseases 0.000 title claims abstract description 17
- 230000036407 pain Effects 0.000 title claims abstract description 13
- 239000003814 drug Substances 0.000 claims abstract description 105
- 239000007788 liquid Substances 0.000 claims abstract description 92
- 239000000284 extract Substances 0.000 claims abstract description 81
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 78
- 238000000605 extraction Methods 0.000 claims abstract description 52
- 239000000341 volatile oil Substances 0.000 claims abstract description 39
- 239000000203 mixture Substances 0.000 claims abstract description 30
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 29
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- 238000000034 method Methods 0.000 claims abstract description 12
- 241000628997 Flos Species 0.000 claims description 92
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- Medicinal Preparation (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The present invention relates to chrysanthemum pain relieving medicinal preparation medicine which is characterized in that the medicine has the components: 86% to 98.2% of chrysanthemum and 1.8% to 14% of auxiliary materials. The present invention has the manufacture method that the chrysanthemum is weighed and put in a reaction tank; 12 times amount of water is added; an oil extractor is arranged; volatile oil is extracted for 5h and obtained; extract is filtered to obtain filter liquid; medicinal residue is boiled by adding 8 times amount of water and extracted for 1h; extract is filtered to obtain filter liquid; the filter liquid is combined, decompressed and concentrated to the state that the inventory rating of the filter liquid to the chrysanthemum is 1:1; the filter liquid is put in a separatory funnel and extracted by capryl acetate for 4 times; the rate of the dosage to the original medicinal materials each time is 1:1; extraction liquid is combined, decompressed and concentrated to be dried; 80% of ethanol is added, and the rate of the dosage to the original medicinal materials is 1:1; the mixture is dissolved, decompressed and concentrated to no ethanol flavor, and (1) is obtained; the pH of residue liquid after extraction of the capryl acetate is regulated into 2 to 3; the residue liquid is extracted by normal butyl alcohol for 4 times, and the rate of the dosage to the original medicinal materials each time is 1:1; extraction liquid is combined, the pH is regulated invention relates to into 6 to 7, and the extraction liquid is decompressed and concentrated to be dried; 80% of ethanol is added, and the rate of the dosage to the original medicinal materials is 1:1; the mixture is dissolved, decompressed and concentrated to be dried; water is added, and the rate of the dosage to the original medicinal materials is 1:1; the mixture is dissolved out to obtain (2); the (2) and the (1) are combined and homogeneously mixed by adding the volatile oil, and.
Description
Technical field
The present invention relates to a kind of Flos Chrysanthemi analgesic preparation, particularly relating to a kind of is the Flos Chrysanthemi analgesic preparation that raw material is made with the vegetable Chinese herbal medicine.
Background technology
Flos Chrysanthemi is medicine, the dual-purpose Chinese medicine of food, is mainly used in cold anemopyretic, headache, conjunctival congestion, laryngopharynx swelling and pain, dizziness, tinnitus, diseases such as furuncle swelling toxin.Past people is combined into compound preparation with its water decoction or with other Chinese crude drug, but it has bioavailability not high, and dosage is big, takes inconvenient shortcoming.
Recently, Tianjin P﹠G biological product company limited has been declared the patent of " extracting the method and the extract of chrysanthemum medicinal component ", the method and the extract that provide the Flos Chrysanthemi medicinal ingredient to extract, but extract Flos Chrysanthemi analgesia preparation medicine is not provided as yet.
Summary of the invention
The object of the present invention is to provide a kind of bioavailability height, solid dispersion is good, absorbs fully eutherapeutic analgesic preparation.
The present invention adopts following technical scheme for this reason: a kind of Flos Chrysanthemi analgesic preparation is characterized in that this medicine is the tablet that raw material is made with the extract of Flos Chrysanthemi:
A prescription: Flos Chrysanthemi 5000g starch 200g cane sugar powder 100g sweetener 4g
Citric acid 5g Mentholum 1g magnesium stearate 2g
B, preparation method:
A) the Flos Chrysanthemi medicinal ingredient is extracted: take by weighing Flos Chrysanthemi 5000g, put and add 12 times of amounts of entry in the retort, oil extractor is installed, extract volatile oil 5h, volatile oil, extracting liquid filtering, filtrate; Medicinal residues add 8 times of amounts of entry and boil extraction 1h, and extracting liquid filtering gets filtrate, merging filtrate, be evaporated to and Flos Chrysanthemi inventory 1: 1 o'clock, put in the separatory funnel, with ethyl acetate extraction 4 times, each consumption and crude drug 1: 1, combining extraction liquid is evaporated to driedly, adds 80% ethanol consumption and 1: 1 amount of crude drug, make its dissolving, be evaporated to no alcohol distinguish the flavor of (1);
Debris behind the ethyl acetate extraction is transferred pH=2-3, with n-butanol extraction 4 times, each consumption and crude drug 1: 1, it is dried that combining extraction liquid transfers pH=6-7 to be evaporated to, and adds 80% ethanol consumption and 1: 1 amount of crude drug, make its dissolving, be evaporated to driedly, add water consumption and 1: 1 amount of crude drug, making its stripping get (2) will (2) and (1) merging, add the volatile oil mix homogeneously, both got Flos Chrysanthemi extract;
B) with the said extracted thing, add starch 200g, cane sugar powder 100g, sweetener 4g, citric acid 5g, fully stir and make its mix homogeneously, to put then in the vacuum drying oven, 60 ℃ of baking temperatures after the thick paste drying to be extracted, are ground into fine powder, cross 100 mesh sieves;
C) get above-mentioned fine powder with 95% ethanol system granule, granule is treated to add Mentholum 1g behind the particle drying in 60 ℃ of dryings of temperature, fully mixes, and makes it evenly, adds magnesium stearate 2g mix homogeneously;
D) tabletting: with above-mentioned fine powder send into tablet machine process Flos Chrysanthemi analgesia sheet.
A kind of Flos Chrysanthemi analgesic preparation is characterized in that this medicine is the granule that raw material is made with the extract of Flos Chrysanthemi:
A, prescription: Flos Chrysanthemi 5000g dextrin 350g cane sugar powder 450g
Sweetener 7g citric acid 7g Mentholum 1g
B, preparation method:
A) the Flos Chrysanthemi medicinal ingredient extracts: take by weighing Flos Chrysanthemi 5000g, put and add 12 times of amounts of entry in the retort, oil extractor is installed, extract volatile oil 5h, volatile oil, extracting liquid filtering, filtrate; Medicinal residues add 8 times of amounts of entry and boil extraction 1h, and extracting liquid filtering gets filtrate, merging filtrate, be evaporated to and Flos Chrysanthemi inventory 1: 1 o'clock, put in the separatory funnel, with ethyl acetate extraction 4 times, each consumption and crude drug 1: 1, combining extraction liquid is evaporated to driedly, adds 80% ethanol consumption and 1: 1 amount of crude drug, make its dissolving, be evaporated to no alcohol distinguish the flavor of (1);
Debris behind the ethyl acetate extraction is transferred pH=2-3, with n-butanol extraction 4 times, each consumption and crude drug 1: 1, it is dried that combining extraction liquid transfers pH=6-7 to be evaporated to, and adds 80% ethanol consumption and 1: 1 amount of crude drug, make its dissolving, be evaporated to driedly, add water consumption and 1: 1 amount of crude drug, making its stripping get (2) will (2) and (1) merging, add the volatile oil mix homogeneously, both got Flos Chrysanthemi extract;
B) get the extract of said extracted, add dextrin 350g, cane sugar powder 450g, sweetener 7g, citric acid 7g, fully stir and make its mix homogeneously, put then in the vacuum drying oven, 60 ℃ of baking temperatures are after the thick paste drying to be extracted, be ground into fine powder, cross 100 mesh sieves;
C) get above-mentioned fine powder with 95% ethanol system granule, granule is treated to add Mentholum 1g behind the particle drying in 60 ℃ of dryings of temperature, fully mixes, and makes it evenly, and granule both must ease pain.
A kind of Flos Chrysanthemi analgesic preparation is characterized in that this medicine is the capsule that raw material is made with the extract of Flos Chrysanthemi:
A, prescription: Flos Chrysanthemi 5000g starch 250g Mentholum 1g
B, preparation method:
A), the Flos Chrysanthemi medicinal ingredient extracts: take by weighing Flos Chrysanthemi 5000g, put and add 12 times of amounts of entry in the retort, oil extractor is installed, extract volatile oil 5h, volatile oil, extracting liquid filtering, filtrate; Medicinal residues add 8 times of amounts of entry and boil extraction 1h, and extracting liquid filtering gets filtrate, merging filtrate, be evaporated to and Flos Chrysanthemi inventory 1: 1 o'clock, put in the separatory funnel, with ethyl acetate extraction 4 times, each consumption and crude drug 1: 1, combining extraction liquid is evaporated to driedly, adds 80% ethanol consumption and 1: 1 amount of crude drug, make its dissolving, be evaporated to no alcohol distinguish the flavor of (1);
Debris behind the ethyl acetate extraction is transferred pH=2-3, with n-butanol extraction 4 times, each consumption and crude drug 1: 1, it is dried that combining extraction liquid transfers pH=6-7 to be evaporated to, and adds 80% ethanol consumption and 1: 1 amount of crude drug, make its dissolving, be evaporated to driedly, add water consumption and 1: 1 amount of crude drug, making its stripping get (2) will (2) and (1) merging, add the volatile oil mix homogeneously, both got Flos Chrysanthemi extract;
B), get the extract of said extracted, add starch 250g and fully stir and make its mix homogeneously, put then in the vacuum drying oven, 60 ℃ of baking temperatures after the thick paste drying to be extracted, are ground into fine powder, cross 60 mesh sieves.Add Mentholum 1g then, fully mix, make it evenly to incapsulate, capsule both must ease pain.
A kind of Flos Chrysanthemi analgesic preparation is characterized in that this medicine is the oral liquid that raw material is made with the extract of Flos Chrysanthemi:
A, prescription: Flos Chrysanthemi 5000g cane sugar powder 85g sweetener 5g citric acid 5g
B, preparation method:
A) the Flos Chrysanthemi medicinal ingredient extracts: take by weighing Flos Chrysanthemi 5000g, put and add 12 times of amounts of entry in the retort, oil extractor is installed, extract volatile oil 5h, volatile oil, extracting liquid filtering, filtrate; Medicinal residues add 8 times of amounts of entry and boil extraction 1h, and extracting liquid filtering gets filtrate, merging filtrate, be evaporated to and Flos Chrysanthemi inventory 1: 1 o'clock, put in the separatory funnel, with ethyl acetate extraction 4 times, each consumption and crude drug 1: 1, combining extraction liquid is evaporated to driedly, adds 80% ethanol consumption and 1: 1 amount of crude drug, make its dissolving, be evaporated to no alcohol distinguish the flavor of (1);
Debris behind the ethyl acetate extraction is transferred pH=2-3, with n-butanol extraction 4 times, each consumption and crude drug 1: 1, it is dried that combining extraction liquid transfers pH=6-7 to be evaporated to, and adds 80% ethanol consumption and 1: 1 amount of crude drug, makes its dissolving, be evaporated to dried, add water consumption and 1: 1 amount of crude drug, making its stripping get (2) will (2) and (1) merging, is evaporated to relative density and is 1.15～1.20 clear paste;
B) get the clear paste of said extracted, add cane sugar powder 85g, sweetener 5g, citric acid 5g, add volatile oil, fully stir and make its mix homogeneously, adding pure water to solution total amount then is 1000ml, both pain-relieving oral liquid.
Contained main effective ingredient is volatile oil, aminoacid, galuteolin (being dissolved in ethyl acetate), chlorogenic acid (being dissolved in n-butyl alcohol) and vitamin etc. in the Flos Chrysanthemi, has effects such as antibiotic, antiinflammatory, analgesic, spasmolytic, inhibition infection, blood pressure lowering.Treatment Common Cold, dizzy, the conjunctival congestion and swelling pain symptom of headache there is better curative effect.
Through to the oral acute toxicity of chrysanthemum extract liquid mice-maximum dosage-feeding test do not see any dead toxic reaction (seeing that " the oral acute toxicity of chrysanthemum extract liquid mice-maximum dosage-feeding test " report that Tianjin Inst. of Materia Medica new drug assessment centers done is attached) chrysanthemum extract liquid cough-relieving that causes, analgesic activity (seeing that " the oral acute toxicity of chrysanthemum extract liquid mice-maximum dosage-feeding test " report that Tianjin Inst. of Materia Medica new drug assessment centers done is attached) prove that chrysanthemum extract liquid has tangible cough-relieving (see " the oral acute toxicity of chrysanthemum extract liquid mice-maximum dosage-feeding test " that Tianjin Inst. of Materia Medica new drug assessment centers is done report attached) chrysanthemum extract liquid antitussive action, show certain analgesic activity, and the analgesic that we provide is the medicine of monarch drug preparation with the chrysanthemum extract liquid, therefore has the bioavailability height, solid dispersion is good, absorb fully eutherapeutic beneficial effect.
The specific embodiment
Embodiment 1 preparation Flos Chrysanthemi analgesia sheet
1, prescription: Flos Chrysanthemi 5000g starch 200g cane sugar powder 100g sweetener 4g
Citric acid 5g Mentholum 1g magnesium stearate 2g
1000
2, preparation method:
1) the Flos Chrysanthemi medicinal ingredient is extracted: take by weighing Flos Chrysanthemi 5000g, put and add 12 times of amounts of entry in the retort, oil extractor is installed, extract volatile oil 5h, volatile oil, extracting liquid filtering, filtrate.Medicinal residues add 8 times of amounts of entry and boil extraction 1h, and extracting liquid filtering gets filtrate, merging filtrate, be evaporated to and Flos Chrysanthemi inventory 1: 1 o'clock, put in the separatory funnel, with ethyl acetate extraction 4 times, each consumption and crude drug 1: 1, combining extraction liquid is evaporated to driedly, adds 80% ethanol consumption and 1: 1 amount of crude drug, make its dissolving, be evaporated to no alcohol distinguish the flavor of (1).
Debris behind the ethyl acetate extraction is transferred pH=2-3, with n-butanol extraction 4 times, each consumption and crude drug 1: 1, combining extraction liquid accent pH=6-7 is evaporated to dried, add 80% ethanol consumption and 1: 1 amount of crude drug, make its dissolving, be evaporated to dried, add water consumption and 1: 1 amount of crude drug, make its stripping get (2) (2) and (1) are merged, add the volatile oil mix homogeneously, both got Flos Chrysanthemi extract.
2) with the said extracted thing, add starch 200g, cane sugar powder 100g, sweetener 4g, citric acid 5g, fully stir and make its mix homogeneously, to put then in the vacuum drying oven, 60 ℃ of baking temperatures after the thick paste drying to be extracted, are ground into fine powder, cross 100 mesh sieves.
3) get above-mentioned fine powder with 95% ethanol system granule, granule is treated to add Mentholum 1g behind the particle drying in 60 ℃ of dryings of temperature, fully mixes, and makes it evenly, adds magnesium stearate 2g mix homogeneously.
4) tabletting: with above-mentioned fine powder send into tablet machine process 1000 of Flos Chrysanthemi analgesia sheets, every heavy 0.5g is grown up three times on the one, one time 2
Embodiment 2 preparation analgesia granules
1, prescription: Flos Chrysanthemi 5000g dextrin 350g cane sugar powder 450g
Sweetener 7g citric acid 7g Mentholum 1g
1000g
2, preparation method:
1) the Flos Chrysanthemi medicinal ingredient extracts: take by weighing Flos Chrysanthemi 5000g, put and add 12 times of amounts of entry in the retort, oil extractor is installed, extract volatile oil 5h, volatile oil, extracting liquid filtering, filtrate.Medicinal residues add 8 times of amounts of entry and boil extraction 1h, and extracting liquid filtering gets filtrate, merging filtrate, be evaporated to and Flos Chrysanthemi inventory 1: 1 o'clock, put in the separatory funnel, with ethyl acetate extraction 4 times, each consumption and crude drug 1: 1, combining extraction liquid is evaporated to driedly, adds 80% ethanol consumption and 1: 1 amount of crude drug, make its dissolving, be evaporated to no alcohol distinguish the flavor of (1).
Debris behind the ethyl acetate extraction is transferred pH=2-3, with n-butanol extraction 4 times, each consumption and crude drug 1: 1, combining extraction liquid accent pH=6-7 is evaporated to dried, add 80% ethanol consumption and 1: 1 amount of crude drug, make its dissolving, be evaporated to dried, add water consumption and 1: 1 amount of crude drug, make its stripping get (2) (2) and (1) are merged, add the volatile oil mix homogeneously, both got Flos Chrysanthemi extract.
2) get the extract of said extracted, add dextrin 350g, cane sugar powder 450g, sweetener 7g, citric acid 7g, fully stir and make its mix homogeneously, put then in the vacuum drying oven, 60 ℃ of baking temperatures are after the thick paste drying to be extracted, be ground into fine powder, cross 100 mesh sieves.
3) get above-mentioned fine powder with 95% ethanol system granule, granule is treated to add Mentholum 1g behind the particle drying in 60 ℃ of dryings of temperature, fully mixes, and makes it evenly, and the granule 1000g that both must ease pain is grown up a 2g three times on the one.
Embodiment 3 preparation analgesia capsules
1, prescription: Flos Chrysanthemi 5000g starch 250g Mentholum 1g
1000
2, preparation method:
1) the Flos Chrysanthemi medicinal ingredient extracts: take by weighing Flos Chrysanthemi 5000g, put and add 12 times of amounts of entry in the retort, oil extractor is installed, extract volatile oil 5h, volatile oil, extracting liquid filtering, filtrate.Medicinal residues add 8 times of amounts of entry and boil extraction 1h, and extracting liquid filtering gets filtrate, merging filtrate, be evaporated to and Flos Chrysanthemi inventory 1: 1 o'clock, put in the separatory funnel, with ethyl acetate extraction 4 times, each consumption and crude drug 1: 1, combining extraction liquid is evaporated to driedly, adds 80% ethanol consumption and 1: 1 amount of crude drug, make its dissolving, be evaporated to no alcohol distinguish the flavor of (1).
Debris behind the ethyl acetate extraction is transferred pH=2-3, with n-butanol extraction 4 times, each consumption and crude drug 1: 1, combining extraction liquid accent pH=6-7 is evaporated to dried, add 80% ethanol consumption and 1: 1 amount of crude drug, make its dissolving, be evaporated to dried, add water consumption and 1: 1 amount of crude drug, make its stripping get (2) (2) and (1) are merged, add the volatile oil mix homogeneously, both got Flos Chrysanthemi extract.
2) get the extract of said extracted, add starch 250g and fully stir and make its mix homogeneously, put then in the vacuum drying oven, 60 ℃ of baking temperatures after the thick paste drying to be extracted, are ground into fine powder, cross 60 mesh sieves.Add Mentholum 1g then, fully mix, make it evenly to incapsulate, 1000 of the capsules of both must having eased pain are grown up three times on the one, one time 2.
Embodiment 4 preparation pain-relieving oral liquids
1, prescription: Flos Chrysanthemi 5000g cane sugar powder 85g
Sweetener 5g citric acid 5g
1000ml
2, preparation method:
1) the Flos Chrysanthemi medicinal ingredient extracts: take by weighing Flos Chrysanthemi 5000g, put and add 12 times of amounts of entry in the retort, oil extractor is installed, extract volatile oil 5h, volatile oil, extracting liquid filtering, filtrate.Medicinal residues add 8 times of amounts of entry and boil extraction 1h, and extracting liquid filtering gets filtrate, merging filtrate, be evaporated to and Flos Chrysanthemi inventory 1: 1 o'clock, put in the separatory funnel, with ethyl acetate extraction 4 times, each consumption and crude drug 1: 1, combining extraction liquid is evaporated to driedly, adds 80% ethanol consumption and 1: 1 amount of crude drug, make its dissolving, be evaporated to no alcohol distinguish the flavor of (1).
Debris behind the ethyl acetate extraction is transferred pH=2-3, with n-butanol extraction 4 times, each consumption and crude drug 1: 1, it is dried that combining extraction liquid transfers pH=6-7 to be evaporated to, and adds 80% ethanol consumption and 1: 1 amount of crude drug, make its dissolving, be evaporated to dried,, add water consumption and 1: 1 amount of crude drug, make its stripping get (2) (2) and (1) are merged, be evaporated to relative density and be 1.15～1.20 clear paste.
2) get the clear paste of said extracted, add cane sugar powder 85g, sweetener 5g, citric acid 5g, add volatile oil, fully stir and make its mix homogeneously, adding pure water to solution total amount then is 1000ml, both pain-relieving oral liquid, the twice-daily of being grown up, a 10ml.
Chrysanthemum extract liquid
The oral acute toxicity of mice-maximum dosage-feeding test
Test unit: Tianjin Inst. of Materia Medica new drug assessment centers
Project leader: Liu Changxiao
Test participant: Gao Jing, a moral is wide
Protocol is preserved: Tianjin Inst. of Materia Medica new drug assessment centers
Date of test: 4～May in 2003
Contact person: Liu Changxiao
Phone: 022-23006863
Chrysanthemum extract liquid
The oral acute toxicity of mice-maximum dosage-feeding test
Flos Chrysanthemi is the Chinese medicine of medicine-food two-purpose, is mainly used in cold anemopyretic, headache, and conjunctival congestion, laryngopharynx swelling and pain, dizziness, tinnitus, furuncle swelling toxin etc., the compound preparation made from each 30g of Flos Lonicerae can be used for hypertension, arteriosclerosis [1].Tianjin P﹠G biological product company limited extracts through two kinds of different process Flos Chrysanthemi, makes the extracting solution of cough-relieving, two kinds of technologies of analgesia, declares patent with this.Our spy has carried out the chmice acute toxicity research to the extract of two kinds of technologies.
1, test material
1.1 be subjected to the reagent thing
1.1.1 cough-relieving extracting solution
Be green brown (being called stock solution-1), the heavy 1.13g of every ml stock solution-1 (for the Cmax extracting solution of producer's preparation), every g stock solution-1 contains the 6.66g crude drug, lot number: 0423, provide by Tianjin P﹠G biological product company limited.Warm stirring back is for the administration of mice oral administration gavage during test.
1.1.2 analgesia extracting solution
Be brown (being called stock solution-2), the heavy 1.10g of every ml stock solution-2 (for the Cmax extracting solution of producer's preparation), every g stock solution-2 contains the 8.58g crude drug, lot number: 0527, provide by Tianjin P﹠G biological product company limited.Warm stirring back is for the administration of mice oral administration gavage during test.
1.2 animal
Kunming mouse, body weight 18 ~ 21g, male and female half and half are provided by the court animal housing.The Laboratory Animal Facility certificate of competency " No. the 013rd, the real moving facility in Tianjin ", administration commission issues by the Tianjin medical faunae, and animal meets primary standard.
2, test method and result
Select 20 of mices for use, each 10 of male and female, fasting gave oral administration gavage Flos Chrysanthemi of mice with maximum dosage-feeding (0.8ml/20g body weight) respectively and extracts stock solution-1 and stock solution-2 after 16 hours.Poisoning symptom after the observation administration comprises autonomic activities, hair, and the eye face, respiratory frequencys etc. are carried out gross anatomy to dead animal, and perusal stolen goods device surface has or not pathological changes, and surviving animals continues to observe one week of body weight, and all body weight are added up.
After about 20 minutes of the mice oral administration gavage stock solution-1, autonomic activities occurs and reduce, abdomen crouches, the eye blepharoptosis, and exaggerated respiration etc., above-mentioned symptom disappears after about 2 hours, recovers normal subsequently, the no phenomena of mortality.Observe body weight gain all normal (see Table 1 and growth curve) through continuous one all body weight.
After about 10 minutes of the mice oral administration gavage stock solution-2, autonomic activities increase in the short time occurs, jump; then occur on foot waving; myasthenia of limbs, 80% mice is sleeping after about 20 minutes, righting reflex loss; rapid breathing etc.; most of mice begins to revive after about 4 hours, and indivedual mices do not revive fully, and mice is all clear-headed after 6 hours; recover normal activity, the no phenomena of mortality.Observe body weight gain all normal (see Table 2 and growth curve) through continuous one all body weight.
Table 1 cough-relieving chrysanthemum extract liquid (stock solution-1) is to the influence of mice body weight (n=10, X ± S.D)
Table 2 analgesia chrysanthemum extract liquid (stock solution-2) is to the influence of mice body weight (n=10, X ± S.D)
After result of the test showed oral administration gavage stock solution-1 of mice and stock solution-2, visible toxic reaction was not seen dead mouse in the short time, and all endosome weight averages increase normal.Therefore, the maximum dosage-feeding of an oral administration gavage cough-relieving of mice chrysanthemum extract liquid (stock solution-1) and analgesia chrysanthemum extract liquid (stock solution-2) is respectively 301g crude drug/kg and 377.5g crude drug/kg.
3, conclusion
The maximum dosage-feeding of an oral administration gavage cough-relieving of mice chrysanthemum extract liquid (stock solution-1) and analgesia chrysanthemum extract liquid (stock solution-2) is respectively 301g crude drug/kg and 377.5g crude drug/kg, be equivalent to 702 and 880 times of clinical every day of maximum consumption (30g crude drug/people/sky, everyone is in 70kg).
Therefore when mice oral administration gavage cough-relieving chrysanthemum extract liquid 301g crude drug/kg and analgesia chrysanthemum extract liquid 377.5g crude drug/kg, do not see any dead toxic reaction that causes.
Chrysanthemum extract liquid cough-relieving, analgesic activity
Test unit: Tianjin Inst. of Materia Medica new drug assessment centers
Project leader: Liu Changxiao
Test participant: Gao Jing, a moral is wide
Protocol is preserved: Tianjin Inst. of Materia Medica new drug assessment centers
Date of test: 4～May in 2003
Contact person: Liu Changxiao
Phone: 022-23006863
Chrysanthemum extract liquid cough-relieving, analgesic activity
Flos Chrysanthemi is medicine, the dual-purpose Chinese medicine of food, is mainly used in cold anemopyretic, headache, conjunctival congestion, laryngopharynx swelling and pain, dizziness, tinnitus, furuncle swelling toxin etc., dosage be the 6-18 gram/time
[1]Tianjin P﹠G biological product company limited extracts through two kinds of different process Flos Chrysanthemi, makes the extracting solution of cough-relieving, two kinds of technologies of analgesia, declares patent with this.Our spy has carried out cough-relieving, analgesic activity research to the extracting solution of two kinds of technologies.
1, test material
1.1 be subjected to the reagent thing
1.1.1 cough-relieving extracting solution
For green brown, the heavy 1.15g of every ml stock solution, every g stock solution contains the 5.98g crude drug, lot number: 0506, provide by Tianjin P﹠G biological product company limited.The warm stirring of extracting solution back is with the 0.5%CMC suspendible, for the administration of mice oral administration gavage during test.
1.1.2 analgesia extracting solution
For brown, the heavy 1.10g of every ml stock solution, every g stock solution contains the 8.58g crude drug, lot number: 0507, provide by Tianjin P﹠G biological product company limited.The warm stirring of extracting solution back is with the 0.5%CMC suspendible, for the administration of mice oral administration gavage during test.
1.1.3 codeine phosphate tablets
For cough-relieving test positive control drug, commercially available, every 30mg produces along pharmaceutical Co. Ltd in Beijing.With the 0.5%CMC suspendible, supply the administration of mice oral administration gavage during test.
1.1.4 Buprenorphine Hydrochloride Sublingual Tablets
For analgesic test positive control (potent analgesic), commercially available, every 0.2mg, lot number: 021204 is produced by Tianjin Inst. of Materia Medica pharmaceutcal corporation, Ltd.With the 0.5%CMC suspendible, supply the administration of mice oral administration gavage during test.
1.2 reagent
Ammonia: the emerging magnificent chemical reagent in Tianjin factory produces.
Sodium carboxymethyl cellulose (CMC): lot number 930628, viscosity 800 ~ 1200 centipoises, Beijing chemical reagents corporation sells.
1.3 animal
Kunming mouse, body weight 18～22.5g, male and female half and half are provided by the court animal housing.The Laboratory Animal Facility certificate of competency " No. the 013rd, the real moving facility in Tianjin ", administration commission issues by the Tianjin medical faunae, and animal meets primary standard.
2, test method and result
2.1 antitussive action (ammonia draws the method for coughing) to mice
Select 40 of mices for use, be divided into 4 groups by body weight, 10 every group, the male and female dual-purpose.Two groups of mice difference oral administration gavage cough-relieving chrysanthemum extract liquids (0.4ml/20g body weight), dosage is 10g crude drug/kg and 20g crude drug/kg, every day 1 time, continuous 7 days, the blank group gives equal-volume 0.5%CMC, another group while oral administration gavage codeine phosphate tablets 30mg/kg during the last administration, after 1 hour each group mice is placed respectively to put into simultaneously in the 500ml beaker and contains 0.2ml strong aqua ammonia cotton balls, timing, the record mice is from putting into beaker to time incubation period that begins to cough, and writing down the cough number of times that mice is put into beaker 3min, result and blank relatively carry out statistical disposition with the t inspection technique.
Result of the test shows, mice oral administration gavage cough-relieving chrysanthemum extract liquid 10g crude drug/kg and 20g crude drug/kg, every day 1 time, continuous 7 days, cough latent period is not seen prolongation, the cough number of times is obviously reduced, two dosage are compared with the blank group, and the P value less than 0.05 and 0.01, the results are shown in Table 3 respectively
The oral cough-relieving chrysanthemum extract liquid of table 3 is to the antitussive action of mice
| Group | Dosage (the g crude drug/kg) | Animal (only) | Incubation period (second, X ± S.D) | The cough number of times (X ± S.D) |
| Blank | - | 10 | 44.1±14.8 | 53.5±10.4 |
| The codeine sheet | 0.03 | 10 | 61.7±14.5* | 42.3±8.7* |
| Flos Chrysanthemi | 10 | 10 | 53.3±11.5 | 43.8±10.0 * |
| 20 | 10 | 53.6±18.1 | 39.2±9.2* * |
Annotate: compare * P＜0.05, * * P＜0.01 with the blank group.
2.2 analgesic activity (hot plate method) to mice
Screening, get female mice number, place on the preheating metallic plate (55 ± 0.5 ℃) record mice from being placed on the hot plate every mice to the pain threshold of sufficient required time occurring adding as this Mus, allly add the foot time less than 5 seconds or give it up greater than 30 seconds or leaper, the mice of pain threshold between 5 seconds～30 seconds is used for test.
Test: qualified mice is divided into 4 groups, 10 every group.Two groups of mice difference oral administration gavage pain relieving chrysanthemum extract liquids (0.4ml/20g body weight), dosage is 10g crude drug/kg and 20g crude drug/kg, every day 1 time, continuous 7 days, the blank group gives equal-volume 0.5%CMC, and another group while oral administration gavage Buprenorphine Hydrochloride Sublingual Tablets 10mg/kg placed each group mice respectively on 55 ± 0.5 ℃ of hot plates after 1 hour during the last administration, measure the mice pain threshold response time, the result carries out statistical disposition with the t method of inspection.
Result of the test shows, mice oral administration gavage analgesia chrysanthemum extract liquid 10g crude drug/kg and 20g crude drug/kg, and every day 1 time, continuous 7 days, pain threshold there is in various degree raising, two dosage are compared with the blank group, and P value is equal＜and 0.05, the results are shown in Table 4
The oral analgesia chrysanthemum extract liquid of table 4 is to the analgesic activity of mice
| Group | Dosage (the g crude drug/kg) | Animal (only) | Pain threshold (second, X ± S.D) |
| Blank | - | 10 | 16.4±4.6 |
| Buprenorphine Hydrochloride Sublingual Tablets | 0.01 | 10 | 33.6±9.7** |
| Flos Chrysanthemi | 10 | 10 | 20.5±3.7* |
| 20 | 10 | 25.2±10.4* |
Annotate: compare * P＜0.05, * * P＜0.01 with the blank group.
3, conclusion
Mice oral administration gavage cough-relieving chrysanthemum extract liquid 10g crude drug/kg and 20g crude drug/kg have tangible antitussive action
Mice oral administration gavage analgesia chrysanthemum extract liquid 10g crude drug/kg and 20g crude drug/kg show certain analgesic activity.
Claims (4)
1, a kind of Flos Chrysanthemi analgesic preparation is characterized in that this medicine is the tablet that raw material is made with the extract of Flos Chrysanthemi:
A prescription: Flos Chrysanthemi 5000g starch 200g cane sugar powder 100g sweetener 4g
Citric acid 5g Mentholum 1g magnesium stearate 2g
B, preparation method:
A) the Flos Chrysanthemi medicinal ingredient is extracted: take by weighing Flos Chrysanthemi 5000g, put and add 12 times of amounts of entry in the retort, oil extractor is installed, extract volatile oil 5h, volatile oil, extracting liquid filtering, filtrate; Medicinal residues add 8 times of amounts of entry and boil extraction 1h, and extracting liquid filtering gets filtrate, merging filtrate, be evaporated to and Flos Chrysanthemi inventory 1: 1 o'clock, put in the separatory funnel, with ethyl acetate extraction 4 times, each consumption and crude drug 1: 1, combining extraction liquid is evaporated to driedly, adds 80% ethanol consumption and 1: 1 amount of crude drug, make its dissolving, be evaporated to no alcohol distinguish the flavor of (1);
Debris behind the ethyl acetate extraction is transferred pH=2-3, with n-butanol extraction 4 times, each consumption and crude drug 1: 1, combining extraction liquid accent pH=6-7 concentrating under reduced pressure as for, add 80% ethanol consumption and 1: 1 amount of crude drug, make its dissolving, be evaporated to driedly, add water consumption and 1: 1 amount of crude drug, making its stripping get (2) will (2) and (1) merging, add the volatile oil mix homogeneously, both got Flos Chrysanthemi extract;
B) with the said extracted thing, add starch 200g, cane sugar powder 100g, sweetener 4g, citric acid 5g, fully stir and make its mix homogeneously, to put then in the vacuum drying oven, 60 ℃ of baking temperatures after the thick paste drying to be extracted, are ground into fine powder, cross 100 mesh sieves;
C) get above-mentioned fine powder with 95% ethanol system granule, granule is treated to add Mentholum 1g behind the particle drying in 60 ℃ of dryings of temperature, fully mixes, and makes it evenly, adds magnesium stearate 2g mix homogeneously;
D) tabletting: with above-mentioned fine powder send into tablet machine process Flos Chrysanthemi analgesia sheet.
2, a kind of Flos Chrysanthemi analgesic preparation is characterized in that this medicine is the granule that raw material is made with the extract of Flos Chrysanthemi:
A, prescription: Flos Chrysanthemi 5000g dextrin 350g cane sugar powder 450g
Sweetener 7g citric acid 7g Mentholum 1g
B, preparation method:
A) the Flos Chrysanthemi medicinal ingredient extracts: take by weighing Flos Chrysanthemi 5000g, put and add 12 times of amounts of entry in the retort, oil extractor is installed, extract volatile oil 5h, volatile oil, extracting liquid filtering, filtrate; Medicinal residues add 8 times of amounts of entry and boil extraction 1h, and extracting liquid filtering gets filtrate, merging filtrate, be evaporated to and Flos Chrysanthemi inventory 1: 1 o'clock, put in the separatory funnel, with ethyl acetate extraction 4 times, each consumption and crude drug 1: 1, combining extraction liquid is evaporated to driedly, adds 80% ethanol consumption and 1: 1 amount of crude drug, make its dissolving, be evaporated to no alcohol distinguish the flavor of (1);
Debris behind the ethyl acetate extraction is transferred pH=2-3, with n-butanol extraction 4 times, each consumption and crude drug 1: 1, it is dried that combining extraction liquid transfers pH=6-7 to be evaporated to, and adds 80% ethanol consumption and 1: 1 amount of crude drug, make its dissolving, concentrating under reduced pressure as for, add water consumption and 1: 1 amount of crude drug, making its stripping get (2) will (2) and (1) merging, add the volatile oil mix homogeneously, both got Flos Chrysanthemi extract;
B) get the extract of said extracted, add dextrin 350g, cane sugar powder 450g, sweetener 7
G, citric acid 7g fully stir and make its mix homogeneously, put then in the vacuum drying oven, and 60 ℃ of baking temperatures after the thick paste drying to be extracted, are ground into fine powder, cross 100 mesh sieves;
C) get above-mentioned fine powder with 95% ethanol system granule, granule is treated to add Mentholum 1g behind the particle drying in 60 ℃ of dryings of temperature, fully mixes, and makes it evenly, and granule both must ease pain.
3, a kind of Flos Chrysanthemi analgesic preparation is characterized in that this medicine is the capsule that raw material is made with the extract of Flos Chrysanthemi:
A, prescription: Flos Chrysanthemi 5000g starch 250g Mentholum 1g
B, preparation method:
A), the Flos Chrysanthemi medicinal ingredient extracts: take by weighing Flos Chrysanthemi 5000g, put and add 12 times of amounts of entry in the retort, oil extractor is installed, extract volatile oil 5h, volatile oil, extracting liquid filtering, filtrate; Medicinal residues add 8 times of amounts of entry and boil extraction 1h, and extracting liquid filtering gets filtrate, merging filtrate, be evaporated to and Flos Chrysanthemi inventory 1: 1 o'clock, put in the separatory funnel, with ethyl acetate extraction 4 times, each consumption and crude drug 1: 1, combining extraction liquid is evaporated to driedly, adds 80% ethanol consumption and 1: 1 amount of crude drug, make its dissolving, be evaporated to no alcohol distinguish the flavor of (1);
Debris behind the ethyl acetate extraction is transferred pH=2-3, with n-butanol extraction 4 times, each consumption and crude drug 1: 1, it is dried that combining extraction liquid transfers pH=6-7 to be evaporated to, and adds 80% ethanol consumption and 1: 1 amount of crude drug, make its dissolving, be evaporated to driedly, add water consumption and 1: 1 amount of crude drug, making its stripping get (2) will (2) and (1) merging, add the volatile oil mix homogeneously, both got Flos Chrysanthemi extract;
B), get the extract of said extracted, add starch 250g and fully stir and make its mix homogeneously, put then in the vacuum drying oven, 60 ℃ of baking temperatures after the thick paste drying to be extracted, are ground into fine powder, cross 60 mesh sieves.Add Mentholum 1g then, fully mix, make it evenly to incapsulate, capsule both must ease pain.
4, a kind of Flos Chrysanthemi analgesic preparation is characterized in that this medicine is the oral liquid that raw material is made with the extract of Flos Chrysanthemi:
A, prescription: Flos Chrysanthemi 5000g cane sugar powder 85g sweetener 5g citric acid 5g
B, preparation method:
A) the Flos Chrysanthemi medicinal ingredient extracts: take by weighing Flos Chrysanthemi 5000g, put and add 12 times of amounts of entry in the retort, oil extractor is installed, extract volatile oil 5h, volatile oil, extracting liquid filtering, filtrate; Medicinal residues add 8 times of amounts of entry and boil extraction 1h, and extracting liquid filtering gets filtrate, merging filtrate, be evaporated to and Flos Chrysanthemi inventory 1: 1 o'clock, put in the separatory funnel, with ethyl acetate extraction 4 times, each consumption and crude drug 1: 1, combining extraction liquid is evaporated to driedly, adds 80% ethanol consumption and 1: 1 amount of crude drug, make its dissolving, be evaporated to no alcohol distinguish the flavor of (1);
Debris behind the ethyl acetate extraction is transferred pH=2-3, with n-butanol extraction 4 times, each consumption and crude drug 1: 1, it is dried that combining extraction liquid transfers pH=6-7 to be evaporated to, and adds 80% ethanol consumption and 1: 1 amount of crude drug, makes its dissolving, be evaporated to dried, add water consumption and 1: 1 amount of crude drug, making its stripping get (2) will (2) and (1) merging, is evaporated to relative density and is 1.15～1.20 clear paste;
B) get the clear paste of said extracted, add cane sugar powder 85g, sweetener 5g, citric acid 5g, add volatile oil, fully stir and make its mix homogeneously, adding pure water to solution total amount then is 1000ml, both pain-relieving oral liquid.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031304788A CN100438886C (en) | 2003-07-29 | 2003-07-29 | Chrysanthem pain relieving medicinal preparation |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031304788A CN100438886C (en) | 2003-07-29 | 2003-07-29 | Chrysanthem pain relieving medicinal preparation |
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| Publication Number | Publication Date |
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| CN1513507A CN1513507A (en) | 2004-07-21 |
| CN100438886C true CN100438886C (en) | 2008-12-03 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1413642A (en) * | 2002-08-14 | 2003-04-30 | 天津市小瑀保健食品有限公司 | Method for extracting chrysanthemum medicinal component and extract |
| CN1413643A (en) * | 2002-08-14 | 2003-04-30 | 天津市小瑀保健食品有限公司 | Method for extracting chrysanthemum medicinal component and extract |
| CN1425413A (en) * | 2002-12-27 | 2003-06-25 | 中山大学 | Xiasangju effervescent tablet and its preparing process |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1413642A (en) * | 2002-08-14 | 2003-04-30 | 天津市小瑀保健食品有限公司 | Method for extracting chrysanthemum medicinal component and extract |
| CN1413643A (en) * | 2002-08-14 | 2003-04-30 | 天津市小瑀保健食品有限公司 | Method for extracting chrysanthemum medicinal component and extract |
| CN1425413A (en) * | 2002-12-27 | 2003-06-25 | 中山大学 | Xiasangju effervescent tablet and its preparing process |
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