CN102590432B - Detection method for medicine for curing cold nature yellow water disease - Google Patents
Detection method for medicine for curing cold nature yellow water disease Download PDFInfo
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Abstract
The invention discloses medicine for curing a cold nature yellow water disease, which comprises the following bulk pharmaceutical chemicals, parts by weight: 50-150 parts of radix pleurospermi tibetanici, 50-150 parts of himalaya mirabilis jalapa, 50-150 parts of caltrop, 50-150 parts of polygonatum and 50-150 parts of asparagus fern. Particle size of the medicine is 0.1-100 mu m. The medicine has high effective dissolution rate, infiltration capacity and bioavailability and is good in medicine effect. The invention further discloses a preparation method for the medicine for curing the cold nature yellow water disease and a special quality detecting method of the medicine. The quality detecting method effectively controls stability of the medicine and simultaneously effectively identifies specificity of the bulk pharmaceutical chemicals in the medicine.
Description
The application is that the application number submitted on July 20th, 2009 is 200910158074.7, denomination of invention is a kind of dividing an application of the medicine of cold grasserie and the application for a patent for invention of preparation and determination methods method thereof that be used for the treatment of.
Technical field
The present invention relates to a kind of detection method that is used for the treatment of cold grasserie medicine, belong to field of medicaments.
Background technology
In Tibetan medicine and pharmacology field, think that yellow water is one of important composition material of human organism; Human diet enters stomach, and after digestion and absorbing, its eliteization is raw is blood, and the waste matter of blood is attributed to courage internal organs becomes bile, and the elite of bile turns to again yellow water; Yellow water is present in whole body everywhere, more at skin and joint, and it plays the vital role that regulates human liquid, lubricated joint aspect physiology.
Although yellow water has healthy function for human body and has important effect, yellow water occurs that inclined to one side Sheng is also a kind of morbid state, and yellow water is partially contained and partially declined and all can cause grasserie.Tibetan medicine and pharmacology theory thinks, the person's character of yellow water neither belongs to heat, does not also belong to cold, be that fever and chills both sexes are various after pathology, so generation blood and the conversion person of Xi La institute combine with heat, becomes yellow sweating of heat syndrome, also claims black grasserie; For Ba Da does with conspicuous, according to the conversion person of institute, combine with cold, become cold grasserie, also claim white grasserie.Yellow sweating of heat syndrome is more common in young people, uncommon pull-up physique person and blood, uncommon some condition of drawing is not still not suitable with to person clinically; Cold grasserie is more common in children and the elderly, Ba Dagan, conspicuous according to type physique person with to Ba Da, dry and conspicuous some condition of complying with is not still not suitable with person.
In addition, the yellow water of pathology also can and then give rise to diseases with types such as merging, accumulations, as leucoderma, psoriasis, parasitosis, mange, numbness disease, diphtheria, anthrax, erysipelas, scar rash, edema, oedema etc.After yellow water pathology, although intersperse among whole body, show its peculiar symptom, mainly alter between row musculus cutaneus, the position such as abdominal cavity, joint.Grasserie is sent out in skin and is easily caused nettle rash; Send out and can cause arthritis in joint.
Grasserie is different from the exudate of the pathologies such as general skin eczema, scabies, malignant boil furuncle, and getting to the bottom of sb.'s illness, to be equivalent to the traditional Chinese medical science said be due to wet or damp and hot.For its pathogenesis, the doctor among the people of Tibetan cures certainly addendum according to < < Tibetan medicine and releases difficult > >, record in tetra-doctor's allusion quotation > > two books of < <, and in conjunction with practical experience, developed the classical Tibetan medicine and pharmacology proved recipe for the treatment of cold grasserie---five loose (Tibetan medicine name is called assorted A Ba), this proved recipe is recorded in first 280 pages of 95 years version Tibetan medicines of < < health drug standards > > promulgated by the ministries or commissions of the Central Government, its prescription is: Herba pleurospermi thomsonii 100g, himalayan four-o'clock root 100g, puncture vine 100g, sealwort 100g, asparagus fern 100g.For many years, because five loose treatment curative effects for cold grasserie have been subject to consistent approval, so all continue to use above-mentioned prescription all the time, all do not have it to carry out any further improvement research.
For above-mentioned five loose preparation methods, all adopt five loose preparation technologies of traditional Tibetan medicine always, first all raw medicinal materials are carried out to coarse crushing, sieve afterwards, mix and make powder; Above-mentioned preparation technology is simple, just raw medicinal material is carried out to simple coarse crushing.In above-mentioned traditional preparation technology, do not recognize for the relation between bulk drug particle diameter and curative effect of medication (be bulk drug particle diameter can not too greatly can not be too little), so the particle diameter of five loose medicines that it prepares has been subject to certain restriction, thereby cause that five loose drug dissolutions of tradition are low, Medicated Permeation ability, bioavilability be low, cannot give full play to the effect of medicine, affect curative effect.
In addition, in field of medicaments, for fear of the imitated production of medicine, strictly investigate the stability of medicine, with regard to above-mentioned five loose stability tests, available technology adopting be microscopic examination test mode; For adopting microscopic examination test mode, five loose standard types are: wood-parenchymatous cell's spindle-like, and wall is slightly thick, lignify, cinclides is obvious, diameter 12～19 μ m; Amylum body is numerous, and simple grain is circular or oval, and omphalion is obvious, is point-like or flying bird shape, diameter 4～10 μ m, and composite grain is comprised of 2～8 gradation; Endocarp fiber bunchy, faint yellow, several layers of criss-cross arrangement up and down, diameter 4～27 μ m, wall is thicker, lignify, pit is rare, and hole ditch is not obvious; In large-scale mucilage cell, contain needle-like calcium oxalate crystal bundle, long 40～99 μ m of needle; Lithocyte is extremely many, orange yellow, and rectangle or strip, diameter 32～88 μ m, wall thickness 10～37 μ m, pit is fine and closely woven, and hole ditch is thin and short.By above-mentioned fractographic means, realized the detection to five loose medicine stabilities, this detection mode can only realize the observation in macroscopic view, and in fact whether the essence of medicine change, this detection mode has no way of learning.
Summary of the invention
Summary of the invention part except beneficial effect
Primary technical matters to be solved by this invention is five loose weight portions of the bulk drug in original formulation that are always all confined to of the classical proved recipe of the Tibetan medicine for the treatment of grasserie, and then former five loose formulas are further developed, obtain having the medicine that is used for the treatment of cold grasserie of the bulk drug of weight portion after improving.
Second technical matters to be solved by this invention is in five loose preparation technologies, just raw medicinal material to be carried out to coarse crushing in prior art, thereby the effective dissolution rate that causes medicine is low, penetrating power is poor, bioavilability is low, cannot give full play to pharmaceutically-active problem, and then provide a kind of preparation method that can improve the penetrating power of medicine and the medicine that is used for the treatment of cold grasserie of bioavilability, and prepare the medicine having compared with the cold grasserie for the treatment of of high-dissolution, penetrating power and bioavilability.
The 3rd technical matters to be solved by this invention is in prior art, five loose stability property quantity measuring methods can only be rested on medicine is carried out on the level of macroscopic view observation, whether essence that can not testing drug stable, so provide a kind of can be fast, the stable medicine resistance to overturning of measuring the cold grasserie for the treatment of with and the quality determining method of the specificity discriminating of bulk drug.
In order to solve the problems of the technologies described above, the invention provides a kind of medicine for the treatment of cold grasserie, comprise the bulk drug of following weight portion:
Herba pleurospermi thomsonii 50-150 part, himalayan four-o'clock root 50-150 part, puncture vine 50-150 part, sealwort 50-150 part, asparagus fern 50-150 part; The particle diameter of described medicine is 0.1～100 μ m.
Wherein, the weight portion of preferred described bulk drug is: 100 parts of Herba pleurospermi thomsoniis, 100 parts of himalayan four-o'clock roots, 100 parts of puncture vines, 100 parts of sealworts, 100 parts of asparagus ferns.The particle diameter of described medicine is 0.1-60 μ m.
Most preferably the particle diameter of described medicine is 1-40 μ m.
The present invention also further discloses the preparation method of the medicine of the cold grasserie of above-mentioned treatment, and it comprises the steps:
(1) selected Herba pleurospermi thomsonii, himalayan four-o'clock root, puncture vine, sealwort, asparagus fern five tastes bulk drug, after removal of impurities, dry respectively or dry;
(2) above-mentioned five tastes bulk drug is ground into respectively to the micropowders that particle diameter is 0.1-100 μ m;
(3) according to the proportioning of above-mentioned raw materials medicine, above-mentioned raw materials medicine is fully mixed;
(4) the mixed bulk drug of step (3) packed or added again conventional auxiliary material to be prepared into arbitrary oral formulations in above-mentioned bulk drug.
Wherein, described auxiliary material is sweet mellow wine, HPMC, protein sugar, fragrant citrus powder, sodium glutamate and sodium carboxymethyl starch.
Described auxiliary material can also be one or more in microcrystalline cellulose, sodium carboxymethyl starch, starch, changeability starch.After adding above-mentioned auxiliary material, need first to granulate, then add talcum powder to carry out compressing tablet.
The present invention is being used for the treatment of described in disclosing on the medicine of cold grasserie and the basis of this process for preparing medicine, further discloses again the quality determining method of the described cold grasserie medicine for the treatment of, and it comprises the steps:
(1) get the drug sample 20g that is used for the treatment of cold grasserie to be measured, add chloroform 50ml, add hot reflux 4 hours, slough the free sapogenin of liposoluble constituent and part and filter, after filtrate is discarded, obtain the dregs of a decoction; To adding concentration in the described dregs of a decoction, be the hydrochloric acid 50ml hydrolysis 2 hours of 2mol/L, discard acid liquid; The dregs of a decoction are washed with water to neutral post-drying and obtain residue; In described residue, add chloroform 50ml, add afterwards hot reflux 4 hours, propose hydrolysis glucoside unit and filter, collect filtrate, naturally wave to 0.6～1ml as need testing solution;
Separately get puncture vine control medicinal material 2g, add chloroform 50ml, add hot reflux 4 hours, slough the free sapogenin of liposoluble constituent and part and filter, after filtrate is discarded, obtain the dregs of a decoction; To adding concentration in the described dregs of a decoction, be the hydrochloric acid 50ml hydrolysis 2 hours of 2mol/L, discard acid liquid; The dregs of a decoction are washed with water to neutral post-drying and obtain residue; In described residue, add chloroform 50ml, add afterwards hot reflux 4 hours, propose hydrolysis glucoside unit and also filters, collect filtrate, naturally wave to 0.6～1ml and make control medicinal material solution;
Get again the negative sample 20g that lacks puncture vine, add chloroform 50ml, add hot reflux 4 hours, slough the free sapogenin of liposoluble constituent and part and filter, after filtrate is discarded, obtain the dregs of a decoction; To adding concentration in the described dregs of a decoction, be the hydrochloric acid 50ml hydrolysis 2 hours of 2mol/L, discard acid liquid; The dregs of a decoction are washed with water to neutral post-drying and obtain residue; In described residue, add chloroform 50ml, add afterwards hot reflux 4 hours, propose hydrolysis glucoside unit and also filters, collect filtrate, naturally wave to 0.6～1ml and make negative control solution;
According to thin-layered chromatography, test, get described need testing solution, each 10 μ l of control medicinal material solution and negative control solution, put respectively in same and take on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is bonding agent, cyclohexane-ethyl acetate-chloroformic solution that the volume ratio of take is 5:2.5:1.5 is developping agent, launch, take out and dry, spray is with raw material anisaldehyde, the volume ratio of glacial acetic acid and sulfuric acid is the anisaldehyde sulfuric acid solution of 1:50:0.5, at 105 ℃, be heated to spot colour developing clear, in test sample chromatogram, with aobvious identical yellow spotting on the corresponding position of control medicinal material, and negative control is noiseless,
(2) get the drug sample 10g that is used for the treatment of cold grasserie to be measured, add wherein ethanol 30ml, through ultrasonic processing, after 30 minutes, filter; After filtration, filtrate is separated with residue, filtrate is collected, and add methyl alcohol 1ml to dissolve as need testing solution after flinging to ethanol;
Separately get Herba pleurospermi thomsonii control medicinal material 2g, add wherein ethanol 10ml, through ultrasonic processing, after 30 minutes, filter; After filtration, filtrate is separated with residue, filtrate is collected, and add methyl alcohol 1ml to dissolve medicinal material solution in contrast after flinging to ethanol;
Get again the negative sample 10g that lacks Herba pleurospermi thomsonii, add wherein ethanol 30ml, through ultrasonic processing, after 30 minutes, filter; After filtration, filtrate is separated with residue, filtrate is collected, and add methyl alcohol 1ml to dissolve as negative control solution after flinging to ethanol;
According to thin-layered chromatography, test, get each 5 μ l of described need testing solution, control medicinal material solution and negative control solution, put respectively in same and take on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is bonding agent, take volume ratio as 8:1.8:0.2 normal hexane-ethyl acetate-methanol solution be developping agent, launch, take out and dry, the phosphomolybdic acid test solution that quality percentage composition is 10% is take in spray, at 105 ℃, be heated to spot colour developing clear, in test sample chromatogram, with aobvious identical darkviolet spot on the corresponding position of control medicinal material, and negative control is noiseless;
(3) get the drug sample 10g that is used for the treatment of cold grasserie to be measured, add wherein ethanol 30ml, through ultrasonic processing, after 30 minutes, filter; After filtration, filtrate is separated with residue, collect filtrate, add methyl alcohol 1ml to dissolve as need testing solution after flinging to ethanol;
Separately get himalayan four-o'clock root control medicinal material 2g, add wherein ethanol 10ml, add wherein ethanol 30ml, through ultrasonic processing, after 30 minutes, filter; After filtration, filtrate is separated with residue, collect filtrate, add methyl alcohol 1ml to dissolve medicinal material solution in contrast after flinging to ethanol;
Get again the negative sample 10g that lacks himalayan four-o'clock root,, add wherein ethanol 30ml, through ultrasonic processing, after 30 minutes, filter; After filtration, filtrate is separated with residue, collect filtrate, add methyl alcohol 1ml to dissolve as negative control solution after flinging to ethanol;
According to thin-layered chromatography, test, each 5 μ l of described need testing solution, control medicinal material solution and negative control solution, put respectively on same silica GF254 thin layer plate, take volume ratio as 8:2:1.5 normal hexane-ethyl acetate-methyl alcohol be developping agent, launch, take out and dry, be placed under the uviol lamp that wavelength is 254nm and inspect, in test sample chromatogram, with aobvious identical crineous spot on the corresponding position of control medicinal material, and negative control is noiseless.
The medicine of the cold grasserie for the treatment of of the present invention, its bulk drug is Herba pleurospermi thomsonii 50-150 part, himalayan four-o'clock root 50-150 part, puncture vine 50-150 part, sealwort 50-150 part, asparagus fern 50-150 part; Compare with five that record in < < health drug standards > > promulgated by the ministries or commissions of the Central Government loose prescription Herba pleurospermi thomsonii 100g, himalayan four-o'clock root 100g, puncture vine 100g, sealwort 100g, asparagus fern 100g, it has further expanded the optional scope of the medicine Raw medicine that is used for the treatment of cold grasserie, through applicant's years of researches, find, within the scope of the weight portion of bulk drug of the present invention, can realize the effective treatment that is attributed to cold grasserie.Most importantly, the medicine that is used for the treatment of cold grasserie of the present invention has overcome Tibetan medicine field for many years and has continued to use five loose formulas of tradition always, and less than five powder formulas being carried out to the problem of any improvement Journal of Sex Research, it has carried out further research to five powder formulas of tradition, has enriched the medicine category for the treatment of cold grasserie.In addition, applicant also finds in above-mentioned extendability research, the particle diameter of the described medicine that is used for the treatment of cold grasserie has vital relation for the curative effect of its medicine, and find through years of researches, only have diameter of aspirin particle just can realize cold grasserie is effectively treated in the said medicine of 0.1～100 μ m, particle diameter too little (being less than 0.1 μ m) is easily because the medical surfaces after pulverizing is long-pending larger by the long-pending increase of the medical surfaces before former pulverizing, cause the hydroscopicity of medicine and chemical activity etc. also correspondingly to increase, the easier moisture absorption of medicine is rotten, the volatile ingredient of medicine inside more easily scatters and disappears, thereby affected the drug effect of medicine, the particle diameter of medicine is large (being greater than 100 μ m) too, and particle diameter too conference causes effective dissolution rate of medicine to reduce, and penetrating power is poor and bioavilability is also very low, so be also unfavorable for the performance of medicine effect.
The preparation method who is used for the treatment of the medicine of cold grasserie of the present invention, it is on the basis of selected bulk drug, bulk drug has been carried out to ultramicro grinding, and the particle diameter of restriction ultramicro grinding is 0.1～100 μ m, afterwards the raw material after ultramicro grinding is carried out the subsequent treatment such as sterilizing.This preparation method has abandoned the method for in five loose preparation methods of tradition, bulk drug being carried out to simple coarse crushing, by carrying out the ultramicro grinding of specified particle diameter, has guaranteed that the medicine preparing can bring into play the drug effect of himself more fully.In above-mentioned preparation process, the temperature of preferably bulk drug potpourri after crushed being carried out to sterilization treatment is 180 ℃, this temperature is set and has guaranteed on the one hand the effective sterilizing of bulk drug potpourri, be unlikely on the other hand to affect because sterilising temp is too high the property of medicine performance of bulk drug.For the medicine that is used for the treatment of cold grasserie of the present invention, can be designed to as required various formulation, such as tablet, suspending agent, electuary particle, capsule, the water-bindered pill, honeyed bolus etc., the variation of above-mentioned formulation can not produce any impact to the drug effect of medicine.
In addition, the quality determining method of the cold grasserie medicine for the treatment of of the present invention, object is to realize when medicine stability is tested and realizes the specificity of medicine Raw medicine is differentiated.This quality determining method, adopt the negative control solution of testing sample, control medicinal material and scarce puncture vine, scarce Herba pleurospermi thomsonii, scarce himalayan four-o'clock root to carry out thin layer test, thereby realized the stability test that is used for the treatment of cold grasserie medicine to of the present invention, also realized the specificity of puncture vine, Herba pleurospermi thomsonii and himalayan four-o'clock root in medicine is differentiated simultaneously.
The present invention has following advantage:
1. the medicine that is used for the treatment of cold grasserie of the present invention, on five loose bases of traditional Tibetan medicine, has carried out further expansion research to it, has expanded the optional scope of the medicine Raw medicine that is used for the treatment of cold grasserie; And find through research that to a deeper level diameter of aspirin particle is on treating the impact of the medicine effect of cold grasserie, only have diameter of aspirin particle just can realize the effective administration anti-inflammatory treatment of cold grasserie in the said medicine of 0.1～100 μ m, avoided the too little medicine moisture absorption that easily causes of particle diameter rotten, the volatile ingredient of medicine inside more easily scatters and disappears, thereby has affected the drug effect of medicine; Also avoided the particle diameter of medicine to cause too greatly effective dissolution rate of medicine to reduce, the poor and bioavilability of penetrating power is very low problem also; Further promoted the drug research of Tibetan medicine field for the cold grasserie for the treatment of.
2. preferred its particle diameter of medicine that is used for the treatment of cold grasserie of the present invention is 0.1-60 μ m, and most preferably particle diameter is 1-40 μ m, and effective dissolution rate and bioavilability that above-mentioned particle diameter can improve medicine are better set.
3. the medicine that is used for the treatment of cold grasserie of the present invention, by the effective selection to diameter of aspirin particle, does not need to add the stabilizing agent of any chemosynthesis, can improve in all directions effective dissolution rate and the bioavilability of medicine, uses safety.
4. the method for medicine for the preparation of the cold grasserie for the treatment of of the present invention, by the pulverizing of medicine Raw medicine being limited to its particle diameter, be 0.1-100 μ m, realize the ultramicro grinding to bulk drug, made the medicine that is used for the treatment of cold grasserie preparing can bring into play better its drug effect; The method is simple, and easily industrialization, has wide market outlook.
5. the quality determining method that is used for the treatment of the medicine of cold grasserie of the present invention, thereby abandoned, can only in macroscopic view, observe the test mode that medicine shape judges its stability, adopt physical and chemical testing means to realize the stability test to medicine essence, and also realized the discriminating to medicine specificity when realizing mensuration medicine stability, thereby guaranteed accurate, quick, stable, the sensitive detection to effective ingredient, more guarantee the quality of medicine, realized the high controllability to drug quality.
Embodiment
embodiment 1
Selected Herba pleurospermi thomsonii, himalayan four-o'clock root, puncture vine, sealwort, asparagus fern five tastes bulk drug, dry respectively after removal of impurities; Bulk drug after above-mentioned drying is ground into respectively to the micropowders that particle diameter is 1-40 μ m; Choosing 50 parts of 50 parts of above-mentioned Herba pleurospermi thomsoniis after crushed, 50 parts of himalayan four-o'clock roots, 50 parts of puncture vines, 50 parts of sealworts, asparagus fern fully mixes; To packing through mixed bulk drug, obtain powder afterwards.
embodiment 2
Selected Herba pleurospermi thomsonii, himalayan four-o'clock root, puncture vine, sealwort, asparagus fern five tastes bulk drug, after removal of impurities, dry respectively; Bulk drug after above-mentioned drying is ground into respectively to the micropowders that particle diameter is 1-10 μ m; Choosing 100 parts of 30 parts of above-mentioned Herba pleurospermi thomsoniis after crushed, 50 parts of himalayan four-o'clock roots, 60 parts of puncture vines, 80 parts of sealworts, asparagus fern fully mixes, then add microcrystalline cellulose to granulate, add again talcum powder, mix rear compressing tablet, finally pack.
embodiment 3
Selected Herba pleurospermi thomsonii, himalayan four-o'clock root, puncture vine, sealwort, asparagus fern five tastes bulk drug, after removal of impurities, dry respectively; Bulk drug after above-mentioned drying is ground into respectively to the micropowders that particle diameter is 10-30 μ m; Choose 100 parts of 80 parts of above-mentioned Herba pleurospermi thomsoniis after crushed, 100 parts of himalayan four-o'clock roots, 150 parts of puncture vines, 100 parts of sealworts, asparagus fern and fully mix, after mixing, make pill.
embodiment 4
Selected Herba pleurospermi thomsonii, himalayan four-o'clock root, puncture vine, sealwort, asparagus fern five tastes bulk drug, after removal of impurities, dry respectively; Above-mentioned dried bulk drug is ground into respectively to the micropowders that particle diameter is 0.1-1 μ m; Choosing 100 parts of 100 parts of above-mentioned Herba pleurospermi thomsoniis after crushed, 100 parts of himalayan four-o'clock roots, 150 parts of puncture vines, 100 parts of sealworts, asparagus fern fully mixes, then add sodium carboxymethyl starch to granulate, add again talcum powder, mix rear compressing tablet, finally pack.
embodiment 5
Selected Herba pleurospermi thomsonii, himalayan four-o'clock root, puncture vine, sealwort, asparagus fern five tastes bulk drug, after removal of impurities, dry respectively; Above-mentioned dried bulk drug is ground into respectively to the micropowders that particle diameter is 0.1-60 μ m; Choose 80 parts of 80 parts of above-mentioned Herba pleurospermi thomsoniis after crushed, 50 parts of himalayan four-o'clock roots, 150 parts of puncture vines, 50 parts of sealworts, asparagus fern and fully mix, then add sodium carboxymethyl starch to granulate, obtain granule.
embodiment 6
Selected Herba pleurospermi thomsonii, himalayan four-o'clock root, puncture vine, sealwort, asparagus fern five tastes bulk drug, after removal of impurities, dry respectively; Above-mentioned dried bulk drug is ground into respectively to the micropowders that particle diameter is 60-100 μ m; Choose 100 parts of 50 parts of above-mentioned Herba pleurospermi thomsoniis after crushed, 50 parts of himalayan four-o'clock roots, 100 parts of puncture vines, 100 parts of sealworts, asparagus fern and fully mix, then add microcrystalline cellulose to granulate, incapsulate, obtain capsule.
embodiment 7
Selected Herba pleurospermi thomsonii, himalayan four-o'clock root, puncture vine, sealwort, asparagus fern five tastes bulk drug, dry respectively after removal of impurities; Bulk drug after above-mentioned drying is ground into respectively to the medicinal powder that particle diameter is 60-100 μ m; Choosing 100 parts of 100 parts of above-mentioned Herba pleurospermi thomsoniis after crushed, 100 parts of himalayan four-o'clock roots, 100 parts of puncture vines, 100 parts of sealworts, asparagus fern fully mixes; Then mixed medicinal powder is incapsulated, obtain capsule.
In above-described embodiment 1-7, the auxiliary material adding is except microcrystalline cellulose and sodium carboxymethyl starch, can also add wherein starch or changeability starch, as the embodiment that can convert, the present invention also can add one or more in microcrystalline cellulose, sodium carboxymethyl starch, starch or changeability starch as the auxiliary material in the preparation medicine that is used for the treatment of cold grasserie of the present invention.
embodiment 8
Selected Herba pleurospermi thomsonii, himalayan four-o'clock root, puncture vine, sealwort, asparagus fern five tastes bulk drug, after removal of impurities, be placed in respectively in dryer and dry at 50 ℃; Bulk drug after above-mentioned drying is ground into respectively to the micropowders that particle diameter is 40-60 μ m; Choose 80 parts of 80 parts of above-mentioned Herba pleurospermi thomsoniis after crushed, 80 parts of himalayan four-o'clock roots, 80 parts of puncture vines, 80 parts of sealworts, asparagus fern and fully mix, and carry out sterilization treatment at 180 ℃; Afterwards to add in the bulk drug potpourri after sterilization treatment in appropriate sweet mellow wine, Hydroxypropyl methylcellulose, protein sugar, fragrant citrus powder, sodium glutamate and sodium carboxymethyl starch any and mix, finally pack.
embodiment 9
Selected Herba pleurospermi thomsonii, himalayan four-o'clock root, puncture vine, sealwort, asparagus fern five tastes bulk drug, after removal of impurities, be placed in respectively in dryer and dry at 60 ℃; Bulk drug after above-mentioned drying is ground into respectively to the micropowders that particle diameter is 10-40 μ m; Choose 100 parts of 100 parts of above-mentioned Herba pleurospermi thomsoniis after crushed, 100 parts of himalayan four-o'clock roots, 100 parts of puncture vines, 100 parts of sealworts, asparagus fern and fully mix, and carry out sterilization treatment at 180 ℃; In the bulk drug potpourri after sterilization treatment, add appropriate sweet mellow wine, Hydroxypropyl methylcellulose and mix afterwards, finally packing.
embodiment 10
Selected Herba pleurospermi thomsonii, himalayan four-o'clock root, puncture vine, sealwort, asparagus fern five tastes bulk drug, after removal of impurities, be placed in respectively in dryer and dry at 80 ℃; Bulk drug after above-mentioned drying is ground into respectively to the micropowders that particle diameter is 60-100 μ m; Choose 150 parts of 150 parts of above-mentioned Herba pleurospermi thomsoniis after crushed, 150 parts of himalayan four-o'clock roots, 150 parts of puncture vines, 150 parts of sealworts, asparagus fern and fully mix, and carry out sterilization treatment at 180 ℃; In the bulk drug potpourri after sterilization treatment, add appropriate protein sugar, fragrant citrus powder, sodium glutamate and sodium carboxymethyl starch and mix afterwards, finally packing.
embodiment 11
Selected Herba pleurospermi thomsonii, himalayan four-o'clock root, puncture vine, sealwort, asparagus fern five tastes bulk drug, after removal of impurities, be placed in respectively in dryer and dry at 60 ℃; Bulk drug after above-mentioned drying is ground into respectively to the micropowders that particle diameter is 1-60 μ m; Choose 150 parts of 100 parts of above-mentioned Herba pleurospermi thomsoniis after crushed, 50 parts of himalayan four-o'clock roots, 90 parts of puncture vines, 80 parts of sealworts, asparagus fern and fully mix, and carry out sterilization treatment at 180 ℃; In the bulk drug potpourri after sterilization treatment, add appropriate sweet mellow wine, Hydroxypropyl methylcellulose, protein sugar, fragrant citrus powder, sodium glutamate and sodium carboxymethyl starch and mix afterwards, finally packing.
In above-described embodiment 1-11, bulk drug is carried out to ultramicro grinding, adopt afterwards to be AccuSizer780/APS detector carry out particle diameter detection to bulk drug particle after crushed.
embodiment 12
The medicine that is used for the treatment of cold grasserie preparing in above-described embodiment 1-11 is entered to quality testing, and detecting step is as follows:
(1) get the drug sample 20g that is used for the treatment of cold grasserie to be measured, add chloroform 50ml, add hot reflux 4 hours, slough the free sapogenin of liposoluble constituent and part and filter, after filtrate is discarded, obtain the dregs of a decoction; To adding concentration in the described dregs of a decoction, be the hydrochloric acid 50ml hydrolysis 2 hours of 2mol/L, discard acid liquid; The dregs of a decoction are washed with water to neutral post-drying and obtain residue; In described residue, add chloroform 50ml, add afterwards hot reflux 4 hours, propose hydrolysis glucoside unit and filter, collect filtrate, naturally wave to 1ml as need testing solution;
Separately get puncture vine control medicinal material 2g, add chloroform 50ml, add hot reflux 4 hours, slough the free sapogenin of liposoluble constituent and part and filter, after filtrate is discarded, obtain the dregs of a decoction; To adding concentration in the described dregs of a decoction, be the hydrochloric acid 50ml hydrolysis 2 hours of 2mol/L, discard acid liquid; The dregs of a decoction are washed with water to neutral post-drying and obtain residue; In described residue, add chloroform 50ml, add afterwards hot reflux 4 hours, propose hydrolysis glucoside unit and also filters, collect filtrate, naturally wave to 1ml and make control medicinal material solution;
Get again the negative sample 20g that lacks puncture vine, add chloroform 50ml, add hot reflux 4 hours, slough the free sapogenin of liposoluble constituent and part and filter, after filtrate is discarded, obtain the dregs of a decoction; To adding concentration in the described dregs of a decoction, be the hydrochloric acid 50ml hydrolysis 2 hours of 2mol/L, discard acid liquid; The dregs of a decoction are washed with water to neutral post-drying and obtain residue; In described residue, add chloroform 50ml, add afterwards hot reflux 4 hours, propose hydrolysis glucoside unit and also filters, collect filtrate, naturally wave to 1ml and make negative control solution;
According to thin-layered chromatography, test, get described need testing solution, each 10 μ l of control medicinal material solution and negative control solution, put respectively in same and take on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is bonding agent, cyclohexane-ethyl acetate-chloroformic solution that the volume ratio of take is 5:2.5:1.5 is developping agent, launch, take out and dry, spray is with raw material anisaldehyde, the volume ratio of glacial acetic acid and sulfuric acid is the anisaldehyde sulfuric acid solution of 1:50:0.5, at 105 ℃, be heated to spot colour developing clear, in test sample chromatogram, with aobvious identical yellow spotting on the corresponding position of control medicinal material, and negative control is noiseless,
(2) get the drug sample 10g that is used for the treatment of cold grasserie to be measured, add wherein ethanol 30ml, through ultrasonic processing, after 30 minutes, filter; After filtration, filtrate is separated with residue, filtrate is collected, and add methyl alcohol 1ml to dissolve as need testing solution after flinging to ethanol;
Separately get Herba pleurospermi thomsonii control medicinal material 2g, add wherein ethanol 10ml, through ultrasonic processing, after 30 minutes, filter; After filtration, filtrate is separated with residue, filtrate is collected, and add methyl alcohol 1ml to dissolve medicinal material solution in contrast after flinging to ethanol;
Get again the negative sample 10g that lacks Herba pleurospermi thomsonii, add wherein ethanol 30ml, through ultrasonic processing, after 30 minutes, filter; After filtration, filtrate is separated with residue, filtrate is collected, and add methyl alcohol 1ml to dissolve as negative control solution after flinging to ethanol;
According to thin-layered chromatography, test, get each 5 μ l of described need testing solution, control medicinal material solution and negative control solution, put respectively in same and take on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is bonding agent, take volume ratio as 8:1.8:0.2 normal hexane-ethyl acetate-methanol solution be developping agent, launch, take out and dry, spray is with 10% phosphomolybdic acid test solution, at 105 ℃, be heated to spot colour developing clear, in test sample chromatogram, with aobvious identical darkviolet spot on the corresponding position of control medicinal material, and negative control is noiseless;
(3) get the drug sample 10g that is used for the treatment of cold grasserie to be measured, add wherein ethanol 30ml, through ultrasonic processing, after 30 minutes, filter; After filtration, filtrate is separated with residue, collect filtrate, add methyl alcohol 1ml to dissolve as need testing solution after flinging to ethanol;
Separately get himalayan four-o'clock root control medicinal material 2g, add wherein ethanol 10ml, add wherein ethanol 30ml, through ultrasonic processing, after 30 minutes, filter; After filtration, filtrate is separated with residue, collect filtrate, add methyl alcohol 1ml to dissolve medicinal material solution in contrast after flinging to ethanol;
Get again the negative sample 10g that lacks himalayan four-o'clock root,, add wherein ethanol 30ml, through ultrasonic processing, after 30 minutes, filter; After filtration, filtrate is separated with residue, collect filtrate, fling to and add methyl alcohol 1ml after ethanol and dissolve as negative control solution;
According to thin-layered chromatography, test, each 5 μ l of described need testing solution, control medicinal material solution and negative control solution, put respectively on same silica GF254 thin layer plate, take volume ratio as 8:2:1.5 normal hexane-ethyl acetate-methyl alcohol be developping agent, launch, take out and dry, be placed under the uviol lamp that wavelength is 254nm and inspect, in test sample chromatogram, with aobvious identical crineous spot on the corresponding position of control medicinal material, and negative control is noiseless.
After said method detects, testing result shows that the above-mentioned drug quality that is used for the treatment of cold grasserie preparing is stable.
dissolution rate test characterizes
The present invention further carries out the mensuration of effective dissolution rate to the medicine that is used for the treatment of cold grasserie preparing, this assay method is mainly to measure the effective dissolution rate of medicine by measuring the content of Siberian solomonseal rhizome polysaccharide in drug sample to be measured, and detailed method is as follows:
Get the medicine 1.0g that the present invention is used for the treatment of cold grasserie, accurately weighed, be placed in 100ml volumetric flask, and to add volumn concentration be 0.9% hydrochloric acid solution, place it in the water-bath of 37 ℃ and place 12h, after jolting, let cool slightly, add dissolution medium to scale.The sample liquid that takes a morsel, through filtering with microporous membrane, is used spectrophotometry and calculates, and this content is as the amount of 100% stripping.Measurement result is that the content of Siberian solomonseal rhizome polysaccharide in the medicine that is used for the treatment of cold grasserie of the present invention is 42.50%.
Spectrophotometry Siberian solomonseal rhizome polysaccharide content:
(1) preparation of reference substance solution: precision takes the anhydrous dextrose 16.635mg that is dried to constant weight through 105 ℃, is placed in 50ml measuring bottle, and adding distil water dissolves and is diluted to that shake up after scale can (in every 1ml containing anhydrous dextrose 0.3327mg).
(2) investigation of linear relationship: accurate reference substance solution 0ml, 0.1ml, 0.2ml, 0.3ml, 0.4ml, 0.5ml, the 0.6ml of drawing, be placed in respectively 10ml measuring bottle, add water to scale and shake up.Precision measures above-mentioned each solution 2.0ml respectively, be placed in tool plug test tube, and precision adds 4% phenol solution 1.0ml to shake up respectively, then precision drips concentrated sulphuric acid 7.0ml rapidly, solution after utilizing eddy current suspendible device to above-mentioned dropping sulfuric acid mixes fast, be placed in 40 ℃ of water-baths and be incubated 30min, take out to be placed on and in ice-water bath, place 5min; Separately get distilled water 2.0ml, with method, add 4% phenol solution and sulfuric acid with aforesaid operations, using this solution as blank.According to spectrophotometric method version < < Chinese Pharmacopoeia () > > appendix VB in 2005, at 582nm wavelength place, measure absorbance log, the absorbance log (Y) of take is ordinate, anhydrous dextrose content (X) is for horizontal ordinate returns processing, obtains regression equation to be
Y＝0.0419X-0.0101，r＝0.9997。
(3) preparation of need testing solution: adopt slurry method, rotating speed is 100r/min, and temperature is (37.0 ± 2) ℃, and the hydrochloric acid solution that dose volume percentage composition is 0.9% is made dissolution medium, gets each 6 parts of the above-mentioned dissolution mediums of 900ml; Get the medicine that the loose and the present invention of five of tradition is used for the treatment of cold grasserie appropriate, 6 parts every group, be placed in respectively dissolution medium and test.After on-test, these nine time points of 5min, 10min, 15min, 20min, 30min, 40min, 50min, 60min and 80min are got solution 8ml, supplement immediately synthermal fresh medium 8ml after taking-up; Accurate each point in time sampling solution 1ml that draws, is placed in 25ml measuring bottle, adds water to scale and shakes up; Precision measures the solution 2ml of the above-mentioned 25ml of adding water to, adds wherein ethanol 10ml and stirs, and afterwards it is carried out to centrifugal treating; To adding water 10ml in the precipitation after centrifugal treating, dissolve, precipitation precision after dissolving is measured to 2ml, be placed in tool plug test tube, according to operating under the preparation of typical curve, according to the content under the investigation item of (2) linear relationship, measure absorbance log in accordance with the law.
Assay method and result: accurate each 2ml of need testing solution that draws, be measured in the same method absorbance log, with 100% stripping quantity, make reference, each time point sample size with its relatively, calculate and add up stripping percent, the results are shown in Table 1.
Total polysaccharide accumulative total stripping percent in five powder preparations of table 1
It is to using the test data that the medicine of the cold grasserie for the treatment of for preparing in previous embodiment 1 obtains as test product to be measured that the test of above-mentioned dissolution rate characterizes.
From above-mentioned data, the medicine that is used for the treatment of cold grasserie of the present invention, carries out the ultramicro grinding of specified particle diameter scope to its raw medicinal material, after pulverizing, sporoderm-broken rate improves greatly, larger with the surface of contact of solvent, diffusingsurface is also larger, and the rate of propagation of medicine is also faster; In addition, miniaturization along with medicinal powder, granularity diminishes, specific surface area increases, and osmotic pressure raises, increased and dissolution medium between effective contact area, accelerate dissolving, the release of solid drugs, the dissolution rate of bulk drug effective constituent is accelerated, thereby improved bioavilability, to reach the object of better clinical efficacy.
the test of anti-inflammatory pharmacology
The medicine that is used for the treatment of cold grasserie of the present invention, it has good antiphlogistic effects, and pharmacological evaluation is as follows:
The medicament using when it is carried out to anti-inflammatory pharmacological evaluation is Freund's complete adjuvant, barium sulphide (A.R), five medicines that are used for the treatment of cold grasserie loose and the present invention prepares.The instrument adopting comprises electronic balance and biped balance pain sensation tester.
Experiment body is SD rat, body weight 220 ± 20g, 4 female mouse of monthly age (this experiment Ti You Lanzhou University Animal Lab. provides).
Through above-mentioned 70 the female mouse of thermalgesia test selection, be divided at random 7 groups, be set to respectively blank group, model group, five loose group, administration group I (0.1-60 μ m particle diameter low dosage), administration group II (0.1-100 μ m particle diameter), administration group III (0.1-60 μ m particle diameter high dose), administration group IV (1-40 μ m particle diameter).Injection Freund's complete adjuvant modeling after will rat left knee joint depilation, after modeling 12h, blank group and model group gavage equal-volume physiological saline, and five loose groups and administration group, respectively according to dosage gavage in table 1, adopt biped balance pain sensation tester to test after administration 6h.
Record biped △ m value, the variance analysis of SPSS11.5 software shows, each group of model group and other all has utmost point significant difference (P < 0.01), modeling be described successfully, and five loose group, administration group I, administration group II, administration group III and administration group IV all have antiinflammatory action.No difference of science of statistics between administration group I and five loose group, and between administration group II, there is significant difference (P < 0.05), and between administration group III, IV, all there is utmost point significant difference (P < 0.01); Between administration group III and administration group II, IV, all there is significant difference (P < 0.05), and administration group I and model group there is utmost point significant difference (P < 0.01).The antiinflammatory action of experimental result explanation administration group I and the effect of five loose groups of tradition approach; The antiinflammatory action of administration group III is obviously better than five loose and administration group I (P < 0.01) of conventional dosage forms, and is better than administration group II (P < 0.05).The antiphlogistic effects of administration group II is between administration group I and administration group III; The action effect of administration group IV is better than administration group III (P < 0.05), is obviously better than five loose group, administration group I and administration group II (P < 0.01).Result is as table 2.
Table 2 rat biped balance pain sensation test △ m value
(compare △ P < 0.05, △ △ P < 0.01 with model group; Compare * P < 0.05, * * P < 0.01 with administration group I; Compare ★ P < 0.05, ★ ★ P < 0.01 with administration group III)
From above-mentioned test figure, five loose dosage that use of organizing are greater than the dosage in described administration group I, but its rat biped balance pain sensation test △ m value is but greater than the △ m value of described administration group I.This just illustrates the cold grasserie medicine that is used for the treatment of of the present invention, and the dosage in use administration group I can realize the identical drug effect of larger dose in traditional five loose group.By test of many times, show, the medicine after ultramicro grinding that is used for the treatment of cold grasserie of the present invention is realized and five drug effects that loose medicine is identical of tradition, and its needed dosage is only 57.5% of five powder amounts of tradition.
Although the present invention elaborates it by above-mentioned embodiment; but; those skilled in the art should be understood that any form that does not exceed claim protection domain made on this basis and the variation of details, all belong to invention which is intended to be protected.
Claims (4)
1. treat a detection method for cold grasserie medicine, the medicine of the cold grasserie of described treatment comprises the bulk drug of following weight portion: Herba pleurospermi thomsonii 50-150 part, himalayan four-o'clock root 50-150 part, puncture vine 50-150 part, sealwort 50-150 part, asparagus fern 50-150 part; The particle diameter of described medicine is 0.1～100 μ m;
Described detection method comprises the steps:
(1) get the drug sample 20g that is used for the treatment of cold grasserie to be measured, add chloroform 50ml, add hot reflux 4 hours, slough the free sapogenin of liposoluble constituent and part and filter, after filtrate is discarded, obtain the dregs of a decoction; To adding concentration in the described dregs of a decoction, be the hydrochloric acid 50ml hydrolysis 2 hours of 2mol/L, discard acid liquid; The dregs of a decoction are washed with water to neutral post-drying and obtain residue; In described residue, add chloroform 50ml, add afterwards hot reflux 4 hours, propose hydrolysis glucoside unit and filter, collect filtrate, naturally wave to 0.6～1ml as need testing solution;
Separately get puncture vine control medicinal material 2g, add chloroform 50ml, add hot reflux 4 hours, slough the free sapogenin of liposoluble constituent and part and filter, after filtrate is discarded, obtain the dregs of a decoction; To adding concentration in the described dregs of a decoction, be the hydrochloric acid 50ml hydrolysis 2 hours of 2mol/L, discard acid liquid; The dregs of a decoction are washed with water to neutral post-drying and obtain residue; In described residue, add chloroform 50ml, add afterwards hot reflux 4 hours, propose hydrolysis glucoside unit and also filters, collect filtrate, naturally wave to 0.6～1ml and make control medicinal material solution;
Get again the negative sample 20g that lacks puncture vine, add chloroform 50ml, add hot reflux 4 hours, slough the free sapogenin of liposoluble constituent and part and filter, after filtrate is discarded, obtain the dregs of a decoction; To adding concentration in the described dregs of a decoction, be the hydrochloric acid 50ml hydrolysis 2 hours of 2mol/L, discard acid liquid; The dregs of a decoction are washed with water to neutral post-drying and obtain residue; In described residue, add chloroform 50ml, add afterwards hot reflux 4 hours, propose hydrolysis glucoside unit and also filters, collect filtrate, naturally wave to 0.6～1ml and make negative control solution;
According to thin-layered chromatography, test, get described need testing solution, each 10 μ l of control medicinal material solution and negative control solution, put respectively in same and take on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is bonding agent, cyclohexane-ethyl acetate-chloroformic solution that the volume ratio of take is 5:2.5:1.5 is developping agent, launch, take out and dry, spray is with raw material anisaldehyde, the volume ratio of glacial acetic acid and sulfuric acid is the anisaldehyde sulfuric acid solution of 1:50:0.5, at 105 ℃, be heated to spot colour developing clear, in test sample chromatogram, with aobvious identical yellow spotting on the corresponding position of control medicinal material, and negative control is noiseless,
(2) get the drug sample 10g that is used for the treatment of cold grasserie to be measured, add wherein ethanol 30ml, through ultrasonic processing, after 30 minutes, filter; After filtration, filtrate is separated with residue, filtrate is collected, and add methyl alcohol 1ml to dissolve as need testing solution after flinging to ethanol;
Separately get Herba pleurospermi thomsonii control medicinal material 2g, add wherein ethanol 10ml, through ultrasonic processing, after 30 minutes, filter; After filtration, filtrate is separated with residue, filtrate is collected, and add methyl alcohol 1ml to dissolve medicinal material solution in contrast after flinging to ethanol; Get again the negative sample 10g that lacks Herba pleurospermi thomsonii, add wherein ethanol 30ml, through ultrasonic processing, after 30 minutes, filter; After filtration, filtrate is separated with residue, filtrate is collected, and add methyl alcohol 1ml to dissolve as negative control solution after flinging to ethanol;
According to thin-layered chromatography, test, get each 5 μ l of described need testing solution, control medicinal material solution and negative control solution, put respectively in same and take on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is bonding agent, take volume ratio as 8:1.8:0.2 normal hexane-ethyl acetate-methanol solution be developping agent, launch, take out and dry, the phosphomolybdic acid test solution that quality percentage composition is 10% is take in spray, at 105 ℃, be heated to spot colour developing clear, in test sample chromatogram, with aobvious identical darkviolet spot on the corresponding position of control medicinal material, and negative control is noiseless;
(3) get the drug sample 10g that is used for the treatment of cold grasserie to be measured, add wherein ethanol 30ml, through ultrasonic processing, after 30 minutes, filter; After filtration, filtrate is separated with residue, collect filtrate, and add methyl alcohol 1ml dissolving as need testing solution after flinging to ethanol;
Separately get himalayan four-o'clock root control medicinal material 2g, add wherein ethanol 10ml, add wherein ethanol 30ml, through ultrasonic processing, after 30 minutes, filter; After filtration, filtrate is separated with residue, collect filtrate, and fling to and add methyl alcohol 1ml after ethanol and dissolve medicinal material solution in contrast;
Get again the negative sample 10g that lacks himalayan four-o'clock root, add wherein ethanol 30ml, through ultrasonic processing, after 30 minutes, filter; After filtration, filtrate is separated with residue, collect filtrate, fling to and add methyl alcohol 1ml after ethanol and dissolve as negative control solution;
According to thin-layered chromatography, test, each 5 μ l of described need testing solution, control medicinal material solution and negative control solution, put respectively on same silica GF254 thin layer plate, take volume ratio as 8:2:1.5 normal hexane-ethyl acetate-methyl alcohol be developping agent, launch, take out and dry, be placed under the uviol lamp that wavelength is 254nm and inspect, in test sample chromatogram, with aobvious identical crineous spot on the corresponding position of control medicinal material, and negative control is noiseless.
2. detection method according to claim 1, is characterized in that, the particle diameter of described medicine is 0.1-60 μ m.
3. detection method according to claim 1, is characterized in that, the particle diameter of described medicine is 1-40 μ m.
4. detection method according to claim 1, is characterized in that, the weight portion of described bulk drug is:
100 parts of Herba pleurospermi thomsoniis, 100 parts of himalayan four-o'clock roots, 100 parts of puncture vines, 100 parts of sealworts, 100 parts of asparagus ferns.
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