CN104587026A - Cortex zanthoxyli total alkaloid extract and preparations as well as application thereof - Google Patents
Cortex zanthoxyli total alkaloid extract and preparations as well as application thereof Download PDFInfo
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Abstract
The invention provides a cortex zanthoxyli total alkaloid extract and preparations as well as application thereof. The cortex zanthoxyli total alkaloid extract is obtained by extraction from the traditional Chinese medicine cortex zanthoxyli, and refining, wherein the total alkaloid content is basically more than 50%, and is up to 100% in maximum. The invention further provides preparations and medical application of the cortex zanthoxyli total alkaloid extract, wherein the preparations include powder injection, dropping pills, tablets, capsules, granules, and so on. Pharmacodynamic and toxicology tests prove that the cortex zanthoxyli total alkaloid extrac can remarkably restrain proliferation of CIA (Collagen Induced Arthritis) rat joint synovial cells, and has low toxic and side effects.
Description
Technical field
The present invention relates to field of medicaments, be specifically related to a kind of Cortex Zanthoxyli podocarpi total alkaloids extract and preparation thereof and purposes.
Background technology
The autoimmune disease of rheumatoid arthritis (rheumatoid arthritis, RA) to be a kind of with articular synovitis be feature, global incidence is 0.5% ~ 1%.Its pathological change mainly synovial cell proliferation, backing layer thickens.IA fibroblast-like synoviocyte is the important composition composition of synovial tissue, by secreting various cytokine, protease, arachidonic acid metabolite etc., being destroyed in process playing a significant role in joint.Meanwhile, autoimmune disease is the morbid state because body immune system causes self component generation immunoreation, has the feature such as recurrent exerbation and chronic migration, therefore, needs long-term treatment and monitoring.
Specific treatment medicine is there is no clinically at present for rheumatoid arthritis, usual employing be control the inflammation that causes of autoimmune disease and use the medicine suppressing immune response, as prednisone, methotrexate, cyclophosphamide, azathioprine, ciclosporin A etc., but, these medicines are while the inflammatory reaction suppressing immune response to cause and tissue injury, also inhibits immune anti-infection ability, a series of untoward reaction can be produced thus.
Cortex Zanthoxyli podocarpi is the very famous local medication in Hunan Province, record in " Hunan Province's Chinese crude drug standard " (version in 1993), it is dry dried bark and the branch skin of rutaceae Zanthoxylum podocarpum Zanthoxylum simulansHance var.podocarpum Hemsl., there is expelling wind and cold, removing toxic substances analgesic effect, bones and muscles pain due to rheumatism, traumatic injury, toothache and venom can be treated.Cortex Zanthoxyli podocarpi is at Hunan Province's aboundresources, distribution is wide, various places, Hunan are all in use, be mainly used in wind-damp dispelling, its treatment rheumatic arthritis and rheumatoid arthritis respond well, leading portion applicant in period has found that in Cortex Zanthoxyli podocarpi, total lignans extract has good treatment of arthritis effect, and has applied for patent (one is used for the treatment of arthritic Cortex Zanthoxyli podocarpi total lignans extract, the patent No.: ZL 201110030813.1).On this basis, we continue further investigation, the effective site of Cortex Zanthoxyli podocarpi is followed the trail of, with the Cortex Zanthoxyli podocarpi total alkaloids extract of different content for medicine is tested, result confirms that Cortex Zanthoxyli podocarpi total alkaloids extract suppresses the effect of articular synovial cells propagation, and is " multicomponent, multipath, Mutiple Targets " onset.
Summary of the invention
The first object of the present invention is to provide a kind of extract of a kind of Cortex Zanthoxyli podocarpi total alkaloids of high-efficiency low-toxicity, and wherein total alkaloid content is more than 50%; This Cortex Zanthoxyli podocarpi total alkaloids extract is by following three kinds of methods, any one therefrom extracts in medicine Cortex Zanthoxyli podocarpi obtained:
Method I, comprises the steps:
(1) prepare crude extract: get Cortex Zanthoxyli podocarpi medical material, be ground into coarse granule, the aqueous hydrochloric acid solution adding 0.5% ~ 2.0% wherein carries out seepage pressure effects, collects percolate, filters, and adds alkali adjust ph to neutral, this filtrate is concentrated, obtain crude extract;
(2) refining extract: the crude extract adding distil water that step (1) is obtained makes into suspension, add alkali adjust ph to alkalescence, add the dichloromethane extraction 3 ~ 4 times relative to suspension 4 ~ 6 times amount, reclaim under reduced pressure dichloromethane at every turn, drying, to obtain final product.
Method II, comprises the steps:
(1) prepare crude extract: get Cortex Zanthoxyli podocarpi medical material, be ground into coarse granule, the hydrochloric acid alcoholic solution adding 0.5% ~ 2.0% wherein carries out seepage pressure effects, collect percolate, filter, add alkali adjust ph to neutral, decompression recycling ethanol, concentrated, obtain crude extract;
(2) refining extract: the crude extract that step (1) is obtained adds anhydrous alcohol solution, after adding decolorizing with activated carbon, be added on D101 macroporous adsorptive resins, first wash with water, eluent discards, then uses the ethanol elution of 70% ~ 95%, collect eluent, decompression recycling ethanol, dry, to obtain final product;
Method III, comprises the steps:
Get Cortex Zanthoxyli podocarpi medical material, be ground into coarse granule, add lime cream wherein and carry out seepage pressure effects, collect percolate, filter, be evaporated to relative density 1.01 ~ 1.02 (50 DEG C of surveys), add the dichloromethane extraction 3 ~ 4 times relative to concentrated solution 4 ~ 6 times amount at every turn, reclaim under reduced pressure dichloromethane after merge extractive liquid, dry, to obtain final product.Wherein, in the step preparing crude extract, for obtaining better extraction effect, the coarse grained size of described Cortex Zanthoxyli podocarpi is for crossing No. 1 sieve and can not crossing No. 3 sieves.
The extract of Cortex Zanthoxyli podocarpi total alkaloids of the present invention, described method I prepare in the step of crude extract, described aqueous hydrochloric acid solution is 10 ~ 12 times relative to the consumption of granule.
For obtaining better extraction effect, adding aqueous hydrochloric acid solution in Cortex Zanthoxyli podocarpi coarse granule after, soaking and carrying out seepage pressure effects after 12 hours.
Afterwards, filter, by filtrate adjust ph to neutral, filtrate is concentrated into paste.
The method of the invention I, in the step of refining extract, adds the distilled water of 2 ~ 3 times amount, makes suspension in crude extract;
The method of the invention I is in the step of refining extract, and in suspension, add alkali adjust ph to alkalescence, pH value is 8 ~ 9.
In the step (1) of the method for the invention II, described hydrochloric acid alcoholic solution is 10 ~ 12 times relative to the consumption of granule.
In the step (1) of the method for the invention II, concrete activated carbon decolorizing and ethanol elution are ordinary skill in the art means, and the present invention is not particularly limited this.
The extract of Cortex Zanthoxyli podocarpi total alkaloids of the present invention, wherein, content >=70% of the total alkaloids extracted, content >=90% of the total alkaloids of preferred extraction, further preferred, gained can be refined extract dichloromethane and be further purified process, the high Cortex Zanthoxyli podocarpi total alkaloids extract of total alkaloid content (total alkaloid content can up to 100%) can be obtained.
The present invention's second object is to provide the preparation of described Cortex Zanthoxyli podocarpi total alkaloids extract, can be the acceptable various common dosage forms of pharmaceutical field such as powder pin, drop pill, tablet, capsule, granule.
The present invention's the 3rd object is to provide above-mentioned Cortex Zanthoxyli podocarpi total alkaloids extract and the application of preparation in preparation treatment medicine for treating rheumatoid arthritis thereof.
In above-mentioned embody rule, the alkaloid in described extract can suppress articular synovial cells proliferation activity well, and high-efficiency low-toxicity.
The invention has the advantages that:
Pharmacodynamics and toxicology test prove, Cortex Zanthoxyli podocarpi total alkaloids extract of the present invention can significantly suppress rat synovial cell to be bred, and toxic and side effects is little.Described extract not only effective ingredient (alkaloids) is clear and definite, and the content of total alkaloids is higher, and impurity is fewer, effect is better, so can reduce dose, also can reduce toxic and side effects to a certain extent, Drug safety and effectiveness can be ensured further.And this Cortex Zanthoxyli podocarpi total alkaloids extract is different from the onset of chemicals single component, but the onset effect of " multicomponent, multipath, Mutiple Targets ", and toxic and side effects is little.
Detailed description of the invention
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.If do not specialize, the conventional means that technological means used in embodiment is well known to those skilled in the art, is raw materials usedly commercial goods.
Embodiment 1 prepares Cortex Zanthoxyli podocarpi total alkaloids extract
Employing method I, comprises the following steps:
(1) crude extract is prepared: get Cortex Zanthoxyli podocarpi medical material 100kg, be ground into coarse granule, the aqueous hydrochloric acid solution adding 10 times amount 0.5% wherein soaks after 12 hours and carries out seepage pressure effects, collect percolate, filter, hydro-oxidation sodium liquid adjust ph is extremely neutral, concentrating under reduced pressure, filtrate is concentrated into paste, obtains crude extract;
(2) refining extract: the crude extract that step (1) is obtained is added appropriate distilled water and makes into suspension, hydro-oxidation sodium liquid adjust ph to 8, add the dichloromethane extraction 3 times relative to suspension 4 times amount at every turn, reclaim under reduced pressure dichloromethane, spraying dry, obtains the Cortex Zanthoxyli podocarpi total alkaloids extract that total alkaloid content is 50%.
Embodiment 2
Identical with embodiment 1 technical scheme, difference is only:
In step (1), the aqueous hydrochloric acid solution adding 1.0% of 11 times amount in Cortex Zanthoxyli podocarpi coarse granule carries out seepage pressure effects;
In step (2), add the dichloromethane extraction 4 times relative to suspension 5 times amount, hydro-oxidation sodium liquid adjust ph to 9 in suspension, final total alkaloid content is the Cortex Zanthoxyli podocarpi total alkaloids extract of 60% at every turn.
Embodiment 3
Identical with embodiment 1 technical scheme, difference is only:
In step (1), the aqueous hydrochloric acid solution adding 2.0% of 12 times amount in Cortex Zanthoxyli podocarpi coarse granule carries out seepage pressure effects;
In step (2), add the dichloromethane extraction 4 times relative to suspension 6 times amount in suspension, final total alkaloid content is the Cortex Zanthoxyli podocarpi total alkaloids extract of 70% at every turn.
Embodiment 4
Identical with embodiment 1 technical scheme, difference is only:
The present embodiment also comprises step (3):
The refining extract obtained by step (2), add 5 times of water gagings wherein and make into suspension, with with the isopyknic dichloromethane extraction of sample 4 times, combined dichloromethane layer, then add 5 times of water gagings make suspendible in suspension, then with the isopyknic dichloromethane extraction of sample 3 times, combined dichloromethane layer, reclaim dichloromethane, lyophilization, namely obtains the Cortex Zanthoxyli podocarpi total alkaloids extract that total alkaloid content is 100%.
Embodiment 5
Employing method II, comprises the following steps:
(1) crude extract is prepared: get Cortex Zanthoxyli podocarpi medical material 100kg, be ground into coarse granule, the hydrochloric acid alcoholic solution adding 10 times amount 1.0% wherein soaks after 12 hours and carries out seepage pressure effects, collect percolate, filter, hydro-oxidation sodium liquid adjust pH is to neutral, and decompression recycling ethanol is also concentrated, filtrate is concentrated into paste, obtains crude extract;
(2) refining extract: the crude extract that step (1) is obtained adds appropriate anhydrous alcohol solution, add decolorizing with activated carbon, mix thoroughly with the D101 macroporous adsorbent resin of same weight, add the water of more than 10 times dehydrated alcohol amounts, stir, be added on processed D101 macroporous adsorptive resins, first wash with water, eluent discards, be washed till colourless with the ethanol of 80% again, collect this 80% ethanol elution, decompression recycling ethanol is also condensed into the clear paste that relative density is 1.20, vacuum drying, obtain the Cortex Zanthoxyli podocarpi total alkaloids extract that total alkaloid content is 70%.
Embodiment 6
Identical with embodiment 5 technical scheme, difference is only:
In step (1), the hydrochloric acid alcoholic solution adding 11 times amount 0.5% in Cortex Zanthoxyli podocarpi coarse granule soaks after 12 hours and carries out seepage pressure effects;
In step (2), then eluent is washed till colourless with the ethanol of 90%, collects this 90% ethanol elution, obtain the Cortex Zanthoxyli podocarpi total alkaloids extract containing total alkaloids 60%.
The present embodiment also comprises step (3): the refining extract obtained by step (2), add 5 times of water gagings wherein and make suspendible, with with the isopyknic dichloromethane extraction of sample 4 times, combined dichloromethane layer, then add 5 times of water gagings make suspendible in suspension, then with the isopyknic dichloromethane extraction of sample 3 times, combined dichloromethane layer, reclaim dichloromethane, lyophilization, namely obtains the Cortex Zanthoxyli podocarpi total alkaloids extract that total alkaloid content is 100%.
Embodiment 7
Identical with embodiment 5 technical scheme, difference is only:
In step (1), the hydrochloric acid alcoholic solution adding 12 times amount 2.0% in Cortex Zanthoxyli podocarpi coarse granule soaks after 12 hours and carries out seepage pressure effects;
In step (2), then eluent is washed till colourless with the ethanol of 95%.
Embodiment 8
Employing method III:
Get Cortex Zanthoxyli podocarpi medical material 100kg, be ground into coarse granule, add 8 times amount lime cream wherein to soak after 8 hours and carry out seepage pressure effects, collect percolate, filter, be evaporated to relative density 1.01 (50 DEG C of surveys), add the dichloromethane extraction 3 times relative to concentrated solution 6 times amount at every turn, reclaim under reduced pressure dichloromethane, vacuum drying, obtains the Cortex Zanthoxyli podocarpi total alkaloids extract that total alkaloid content is 90%.
Embodiment 9
Identical with the technical scheme of embodiment 8, difference is only:
In Cortex Zanthoxyli podocarpi coarse granule, add 12 times amount lime cream soak after 8 hours and carry out seepage pressure effects; Add the dichloromethane extraction 4 times of 5 times amount after concentrating under reduced pressure at every turn, obtain the Cortex Zanthoxyli podocarpi total alkaloids extract that total alkaloid content is 80%.
Embodiment 10
Identical with the technical scheme of embodiment 8, difference is only:
Add the dichloromethane extraction 4 times of 4 times amount after concentrating under reduced pressure at every turn, obtain the Cortex Zanthoxyli podocarpi total alkaloids extract that total alkaloid content is 70%.
Embodiment 11 ~ 13 prepares Cortex Zanthoxyli podocarpi total alkaloids extract preparation
The Cortex Zanthoxyli podocarpi total alkaloids extract 200g that Example 1,5 and 8 is obtained respectively, dextrin 800g, mix homogeneously, adopts existing hard capsule preparation technology, i.e. the obtained hard capsule containing Cortex Zanthoxyli podocarpi total alkaloids extract.
Embodiment 14 ~ 16
The Cortex Zanthoxyli podocarpi total alkaloids extract 2kg that Example 2,7 and 10 is obtained respectively, vegetable oil 8kg, mix homogeneously, makes capsule casing material with gelatin, adopts existing soft capsule preparation technology, i.e. the obtained soft capsule containing Cortex Zanthoxyli podocarpi total alkaloids extract.
Embodiment 17 ~ 19
The Cortex Zanthoxyli podocarpi total alkaloids extract 200g that Example 3,6 and 9 is obtained respectively, polyethylene glycol-800 g, mix homogeneously, adopts existing drop pill preparation technology, i.e. the obtained drop pill containing Cortex Zanthoxyli podocarpi total alkaloids extract.
Embodiment 20 ~ 22
The Cortex Zanthoxyli podocarpi total alkaloids extract 200g that Example 4,6,9 is obtained respectively, soluble starch 600g, sucrose 200g, mix homogeneously, granulates, sieves, dry, i.e. the obtained granule containing Cortex Zanthoxyli podocarpi total alkaloids extract.By the obtained further tabletting of granule, i.e. the obtained tablet containing Cortex Zanthoxyli podocarpi total alkaloids extract.
Embodiment 23 ~ 25
The Cortex Zanthoxyli podocarpi total alkaloids extract 200g that Example 3,7 and 10 is obtained respectively, be dissolved in 10000ml water for injection and (add a little ethanol and make dissolving), adopt injectable powder freeze-drying preparation technology, i.e. the obtained injectable powder type containing Cortex Zanthoxyli podocarpi total alkaloids extract.
For investigating the effectiveness of Cortex Zanthoxyli podocarpi total alkaloids extract of the present invention and safety, applicant respectively with the extract of above-mentioned section Example gained for trial drug, carried out pharmacodynamics test and toxicology test is investigated.
Pharmacodynamics test (suppressing the sliding born of the same parents' cell proliferation test of CIA rat articular):
Laboratory animal: Wistar rat, cleaning grade, body weight 160 ~ 180g, purchases in Shanghai Experimental Animal Center.
Experimental subject:
1, the Cortex Zanthoxyli podocarpi total alkaloids extract that embodiment 1 is obtained;
2, the Cortex Zanthoxyli podocarpi total alkaloids extract that embodiment 5 is obtained;
3, the Cortex Zanthoxyli podocarpi total alkaloids extract that embodiment 8 is obtained.
The foundation of experimental model
Purchase from Shanghai Experimental Animal Center the Wistar rat that body weight is 160-180g, 6-8 week, raise in room temperature, the Animal House in 12-12 hour day-night cycle cycle with the Mus feedstuff of standard and water, adaptability is randomized in mouse cage after raising 1 week, 5, every cage.All zooperies are carried out in strict accordance with the regulation of People's Republic of China's relevant laws and regulations and Hunan University of Traditional Chinese Medicine's animal experimental center.Chicken II-type collagen is dissolved in 0.1% glacial acetic acid, stirring and evenly mixing is mixed with the solution of 2mg/ml, it is become emulsifying agent with cold Freund's complete adjuvant in 1:1 ratio stirring and evenly mixing, in the vola of rat, root of the tail portion and back portion 3 intradermal injection 0.25ml, strengthens once after 7 days.After about 2 weeks, rheumatoid arthritis in rats model is set up.
The separation and ientification of experimental model articular synovial cells
After model of rheumatoid arthritis rat anesthesia, the kneed synovial tissue of aseptic separation, 3 times are washed with the PBS solution of not calcium ions and magnesium ion, shred into the fritter of 1-2mm3 with shears in 10cm aseptic plastic plate, piece of tissue is gone in the DMEM culture medium containing 10% hyclone, 100 units/ml penicillin and streptomycin and 0.4% collagenase II, put 37 DEG C, 5%CO
2digestion 2-3 hour is cultivated in incubator.The upper strata cell suspension that cancellationization is good proceeds in 50ml centrifuge tube, through the centrifugal 10min of 400 × g, reject supernatant, adds the mixed solution of isopyknic 0.25% pancreatin and 0.02%EDTA in cell precipitation, under similarity condition, continue digestion 1 hour, period every 15min concussion mixing once.Collect suspension in centrifuge tube, obtain individual cells suspension with the sieved filter of the aseptic steel of 200 object, through the centrifugal 10min of 400 × g, reject supernatant, adds PBS solution centrifuge washing 3 times, reject supernatant fluid.In sediment, add the DMEM complete medium containing 10% hyclone, 100 units/ml penicillin and streptomycin, piping and druming mixing cell, being transferred to diameter is in the sterilized petri dishes of 10cm, puts 37 DEG C, 5%CO
2cultivate 24 hours in incubator.Reject culture medium solution, adds aseptic PBS solution and washs 3 times, adds fresh DMEM culture medium, continues to cultivate 8-10 days.Collect the articular synovial cells of normal Wistar rats as stated above.
One, rat synovial cell Proliferation Ability test
Rat model articular synovial cells to go down to posterity after 3 generations collecting cell after the mixed solution digestion of 0.25% pancreatin and 0.02%EDTA, and adjustment cell quantity is 3 × 105/ml, joins in 96 orifice plates, every hole 100 μ l.The numb mouth leather total alkaloids extract of 3 kinds of variable concentrations is added in 96 orifice plates, every hole 100 μ l, makes hole Chinese medicine final concentration be respectively 0.2mg/ml, 0.4mg/ml, 0.8mg/ml, 1.0mg/ml, 1.5mg/ml, 2.0mg/ml, 2.5mg/ml and 5.0mg/ml, often kind of concentration establishes 6 multiple holes, not add the normal rat articular synovial cells of medicine as negative control, to add the model articular synovial cells of sinomenine for cell inhibitory effect positive control.96 orifice plates are put 37 DEG C, 5%CO
2cultivate 44 hours in incubator, add 20 μ l MTT solution (5mg/ml), continue cultivation 4 hours, reject supernatant, adds the DMSO liquid of 150 μ l in hole, after concussion mixing 10min, microplate reader measures the absorbance OD value under 490nm.The inhibit activities of cell proliferation calculates according to the following equation.
OD
n: the OD value of negative control cell; ODT: the OD value of rat model articular synovial cells to be measured
Experimental result: in table 1
Table 1 suppresses articular synovial cells proliferation results (IC50)
| Sample | IC50 |
| Embodiment 1 gained Cortex Zanthoxyli podocarpi total alkaloids extract | 0.62mg/ml |
| Embodiment 5 gained Cortex Zanthoxyli podocarpi total alkaloids extract | 0.38mg/ml |
| Embodiment 8 gained Cortex Zanthoxyli podocarpi total alkaloids extract | 0.27mg/ml |
Result shows: Cortex Zanthoxyli podocarpi total alkaloids extract obviously can suppress the sliding born of the same parents' cell proliferation of CIA rat articular, and in dose-effect relationship, and along with increasing of wherein total alkaloid content, its effect strengthens.
Two, acute toxicity test:
In order to investigate the safety of Cortex Zanthoxyli podocarpi total alkaloids extract, spy has carried out acute toxicity to it and has investigated, and test method result is as follows:
Experimental agents: the Cortex Zanthoxyli podocarpi total alkaloids extract (containing total alkaloids 70%) obtained by embodiment 2.
Laboratory animal: ICR mice, one-level, 8 ~ 9 weeks ages of Mus, body weight 18 ~ 22g.
Experimental technique: because of the impact by Cortex Zanthoxyli podocarpi total alkaloids extract concentration and volume, single administration cannot measure its LD
50by " herbal pharmacology research methodology " (People's Health Publisher, 1st edition, Qi Chen edits) requirement, dose according to animal tolerant Cmax, maximum volume gives the regulation of 2-3 time in once or one day continuously, choose healthy ICR mice 40, be divided into matched group and medicine group, often organize 20 animals.Before experiment, water be can't help 12 hours to mice fasting, the Cortex Zanthoxyli podocarpi total alkaloids extract medicinal liquid 0.4ml/10g body weight that it is 106.4% that medicine group every mouse stomach gives concentration (containing extract 106.4g in every 100ml medicinal liquid)/time, administration 2 times in 24 hours, control group mice gavage gives distilled water 0.4ml/10g body weight, same 2 times, then mice is raised routinely, observe 7 days.
Result shows: after mouse stomach administration, compare with matched group, Symptoms without exception, and during breeding observing, appetite, activity, defecation are all normal, and raising the body weight of all animals after 7 days all normally increases, and Mouse Weight is 25.12 ± 3.01g.As calculated, the maximum dosage-feeding of administration is 1520g (crude drug in whole)/Kg/ day, is 3040 times of adult's (60Kg) clinical consumption per day (0.5g/Kg/ day).
Result shows: Cortex Zanthoxyli podocarpi total alkaloids extract Acute toxicity of the present invention is little, and degree of safety is large.
Can be drawn by the result of above-mentioned pharmacodynamics and toxicology test: Cortex Zanthoxyli podocarpi total alkaloids extract has the effect suppressing articular synovial cells propagation preferably, and toxicity is very low.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (9)
1. an extract for Cortex Zanthoxyli podocarpi total alkaloids, is characterized in that, wherein total alkaloid content is more than 50%; This Cortex Zanthoxyli podocarpi total alkaloids extract is by following three kinds of methods, any one therefrom extracts in medicine Cortex Zanthoxyli podocarpi obtained:
Method I, comprises the steps:
(1) prepare crude extract: get Cortex Zanthoxyli podocarpi medical material, be ground into coarse granule, the aqueous hydrochloric acid solution adding 0.5% ~ 2.0% wherein carries out seepage pressure effects, collects percolate, filters, and adds alkali adjust ph to neutral, this filtrate is concentrated, obtain crude extract;
(2) refining extract: the crude extract adding distil water that step (1) is obtained makes into suspension, add alkali adjust ph to alkalescence, add the dichloromethane extraction 3 ~ 4 times relative to suspension 4 ~ 6 times amount, reclaim under reduced pressure dichloromethane at every turn, drying, to obtain final product;
Method II, comprises the steps:
(1) prepare crude extract: get Cortex Zanthoxyli podocarpi medical material, be ground into coarse granule, the hydrochloric acid alcoholic solution adding 0.5% ~ 2.0% wherein carries out seepage pressure effects, collect percolate, filter, add alkali adjust ph to neutral, decompression recycling ethanol, concentrated, obtain crude extract;
(2) refining extract: the crude extract that step (1) is obtained adds anhydrous alcohol solution, after adding decolorizing with activated carbon, be added on D101 macroporous adsorptive resins, first wash with water, eluent discards, then uses the ethanol elution of 70% ~ 95%, collect eluent, decompression recycling ethanol, dry, to obtain final product;
Method III, comprises the steps:
Get Cortex Zanthoxyli podocarpi medical material, be ground into coarse granule, add lime cream wherein and carry out seepage pressure effects, collect percolate, filter, be evaporated to relative density 1.01 ~ 1.02 (50 DEG C of surveys), add the dichloromethane extraction 3 ~ 4 times relative to concentrated solution 4 ~ 6 times amount at every turn, reclaim under reduced pressure dichloromethane after merge extractive liquid, dry, to obtain final product.
2. extract according to claim 1, is characterized in that, in the step (1) of described method I and method II, described aqueous hydrochloric acid solution and hydrochloric acid alcoholic solution are 10 ~ 12 times relative to the consumption of granule.
3. extract according to claim 1 and 2, is characterized in that, in the step (2) of described method I, add alkali adjust ph to alkalescence in suspension, described weakly alkaline pH value range is 8 ~ 9.
4. the extract according to any one of claims 1 to 3, is characterized in that, total alkaloid content >=70%.
5. the extract according to any one of claims 1 to 3, is characterized in that, total alkaloid content >=90%.
6. the extract according to any one of Claims 1 to 5, is characterized in that, gained is refined extract dichloromethane and is further purified process.
7. the pharmaceutical preparation containing the Cortex Zanthoxyli podocarpi total alkaloids extract described in any one of claim 1 ~ 6.
8. pharmaceutical preparation according to claim 7, is characterized in that, described preparation is powder pin, drop pill, tablet, capsule and granule.
9. Cortex Zanthoxyli podocarpi total alkaloids extract described in any one of claim 1 ~ 6 or the application of the pharmaceutical preparation described in any one of claim 7 ~ 8 in preparation treatment medicine for treating rheumatoid arthritis.
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Application publication date: 20150506 |