CN102614230B - Medicinal composition for treating rheumatoid arthritis and preparation method and application thereof - Google Patents
Medicinal composition for treating rheumatoid arthritis and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a medicinal composition for treating rheumatoid arthritis. The medicinal composition is the preparation which is prepared from the following active ingredients in parts by weight: 1 to 10 parts of pterocephalus hookeri heck total saponins extract and 1 to 10 parts of total iridoid glycoside extract. The invention also provides a preparation method and the application of the medicinal composition. According to the medicinal composition, the pterocephalus hookeri heck total saponins extract and the total iridoid glycoside extract are combined, so the medicinal composition is higher than each extract in the effects of resisting inflammation and rheumatoid arthritis, has a synergistic effect, is positive in the treatment effect and provides a new selection to clinical medication.
Description
Technical field
The present invention relates to a kind of pharmaceutical composition Preparation Method And The Use for the treatment of rheumatoid arthritis, belong to drug world.
Background technology
Rheumatoid arthritis (Rheumatiod Arthritis, be called for short RA) is a kind of common general immune disease that the chronic polyarthritis pathological changes is main manifestations of take, and the whole world has more than one hundred million patients.According to statistics, the external prevalence of RA is 1～2%, and indivedual areas are up to 5%; China's sickness rate is about 0.74%, existing patient 1,000 ten thousand people left and right.Show according to investigations, in normal population, the sickness rate of rheumatoid arthritis accounts for 0.35% left and right of normal population.The primary disease disability rate is high, and 50%, three year disability rate of 2 years disability rates of patient with rheumatoid arthritis of diagnosis and treatment does not in time reach 70%.And the patient who has suffered from rheumatoid arthritis, average life shortens 10～15 years, so RA has a strong impact on work capacity, the medicine of development RA, for the clinical symptoms of alleviating such disease, improve patient's life quality, ensure the productivity, there is positive meaning.
The Tibetan medicine Herba pterocephali, be the dry herb of Dipsacaceae plant spoon leaf Herba pterocephali Pterocephalus hookeri (C.B.Clarke) Hoeck, has heat-clearing and toxic substances removing, wind-damp dispelling, pain relieving effect.Herba pterocephali is Tibetan medicine's Tibetan medicine commonly used, have another name called " list appearance poison crow ", for the obvious typical national medicine of Tibetan medicine feature, medication is with a long history, the Tibetan medicine always is mainly used in it to treat the diseases such as rheumatic, except Tibetan medicine and closely-related Mongolian medicine thereof, Chinese medicine and other traditional medicine are not applied the history of Herba pterocephali substantially.Under the Tibetan medicine and pharmacology theoretical direction, the clinical practice of Herba pterocephali of take is foundation, Herba pterocephali extract resisting rheumatoid arthritis function and mechanism has been carried out to experimental study, result shows: the anti-RA effect of Herba pterocephali extract is sure, for adjuvant arthritis animal model constitutional inflammation and post-traumatic arthritis, antiphlogistic effects is preferably all arranged, and can alleviate the pathological change of synovial membrane, obvious analgesic activity is also arranged simultaneously, and this applies and matches with Herba pterocephali treatment rheumatism, rheumatoid arthritis with the Tibetan medicine is clinical.(Shen Peng, the resisting rheumatoid arthritis effect of Tibetan medicine Herba pterocephali and mechanism research, Chengdu University of Traditional Chinese Medicine, 2002 .)
Chemical constitution study to Herba pterocephali shows, mainly contains the compositions such as oleanane type triterpene saponins, iridoid glycoside compounds, alkaloid, polysaccharide in Herba pterocephali.Research to the Herba pterocephali effective ingredient shows, adopt rat acute foot swelling experiment, the experiment of mice granuloma induced by implantation of cotton pellets, the experiment of chmice acute ear swelling and chmice acute to ooze out the methods such as experiment, proved that Herba pterocephali n-butanol portion total saponin extracts has significant anti-inflammatory activity [Guan Xinlu, Deng. the antiinflammatory action of Herba pterocephali and anxious malicious experimentation. the journal .2004 of Beijing University of Chinese Medicine, 27 (2): 71～73].The main component meliatin of iridoid glycosides in Herba pterocephali, have obvious antiinflammatory pharmacological action, but its analog has immunological enhancement.[Pang Wei. the research of Tibetan medicine Herba pterocephali and application. National medicine magazine .2007, (5): 63-65].Number of patent application: 200910196870.x, Herba pterocephali total saponin extracts effective part extract is provided in this invention, its main component is the Triterpenoids sapogenins saponin, total saponin extracts content 50-90%, this total saponin extracts is inhibition tumor cell propagation significantly, in this total saponin extracts, directly adopt macroporous resin to separate and obtain, contain iridoid glycoside in extract.
Comprehensive existing document is known, only there are at present total saponin extracts and meliatin in Herba pterocephali to there is anti-inflammatory and analgesic effect and total saponin extracts antineoplastic report, yet there are no Herba pterocephali total saponin extracts and iridoid glycoside are combined to the report that uses the treatment rheumatoid arthritis.
Summary of the invention
The object of the present invention is to provide a kind of pharmaceutical composition for the treatment of rheumatoid arthritis and preparation method thereof.
The invention provides a kind of pharmaceutical composition for the treatment of rheumatoid arthritis, it is to be the preparation that active fraction preparation forms by Herba pterocephali total saponin extracts and total iridoid glucoside extract, wherein, the weight proportion of described total saponin extracts, total iridoid glucoside extract is:
Total saponin extracts 1-10 part, total iridoid glucoside extract 1-10 part.
Wherein, the weight proportion of described total saponin extracts, total iridoid glucoside extract is:
10 parts of total saponin extracts, 1 part of total iridoid glucoside extract; Or 5 parts of total saponin extracts, 5 parts of total iridoid glucoside extracts.
Further, in described Herba pterocephali total saponin extracts, saponin content is greater than 50%w/w; In described Herba pterocephali total iridoid glucoside extract, iridoid glycoside content is greater than 50%w/w.
Further, in described Herba pterocephali total saponin extracts, saponin content is greater than 80%w/w, is preferably 80-90%w/w; In described Herba pterocephali total iridoid glucoside extract, iridoid glycoside content is greater than 80%w/w, is preferably 80-90%w/w.
Wherein, the dry herb that described Herba pterocephali is Dipsacaceae plant spoon leaf Herba pterocephali Pterocephalus hookeri (C.B.Clarke) Hoeck.
The present invention also provides a kind of method for preparing aforementioned pharmaceutical compositions, and it comprises the steps:
(1) prepare the Herba pterocephali total saponin extracts
A, get Herba pterocephali, extracting in water, filter, and after filtrate is concentrated, adopts nonpolar or low pole purification with macroreticular resin, first, with after the washing decontamination, discards eluent; With the 60-85% ethanol elution, after collecting ethanol elution;
B, get the ethanol elution of step a, after decompression and solvent recovery, add lead acetate solution, stir, filter, filtrate for later use, get precipitation, and after deleading, drying, obtain the Herba pterocephali total saponin extracts;
(2) prepare Herba pterocephali total iridoid glucoside extract
Get in step b the filtrate added after lead acetate solution, concentrated after, use n-butanol extraction, get n-butyl alcohol liquid, after the recovery solvent, drying, obtain Herba pterocephali total iridoid glucoside extract;
(3) preparation of pharmaceutical composition
Take Herba pterocephali total saponin extracts and total iridoid glucoside extract by the prescription proportioning, add adjuvant pharmaceutically commonly used to be prepared into preparation.
Wherein, select D101, AB-8 or HPD-300 type macroporous adsorbent resin in step a; With the 65-75%v/v ethanol elution; In step b, get the ethanol elution of step a, after decompression and solvent recovery, redissolve in 30-95%v/v ethanol, add saturated neutral lead acetate solution, stir, filter, filtrate for later use, get precipitation, be suspended in 30-95%v/v ethanol, with hydrogen sulfide gas or cation exchange resin deleading, filter, get filtrate concentrating, drying, obtain the Herba pterocephali total saponin extracts.
Further, select D101 type macroporous adsorbent resin in step a; With the 70%v/v ethanol elution; In step b, concentration of alcohol is 60-85%v/v.
Further, in step b, concentration of alcohol is preferably 65-75%v/v.
Further, in step a, the concrete operation step of purification with macroreticular resin is as follows:
The concentration of sample solution is formulated as to 0.1-0.2g crude drug/ml, adopts D101 type purification with macroreticular resin, the loading flow velocity is 1-3BV/h, applied sample amount is counted medical material with medical material: resin=(0.5-1.5): 1w/w, with the 3-5BV water elution, flow velocity is 1-3BV/h, discards eluent; With 70% ethanol elution of 2-4BV, elution flow rate is 2-4BV/h.
Further preferably, the concentration of sample solution is formulated as to 0.1g crude drug/ml medicinal liquid, adopts purification under D101 type macroporous adsorbent resin room temperature, the loading flow velocity is 2BV/h, and applied sample amount is counted medical material with medical material: resin=1: 1, with the 4BV water elution, flow velocity is 2BV/h, discards eluent; With 70% ethanol elution of 3BV, elution flow rate is 3BV/h.
The present invention also provides the purposes of aforementioned pharmaceutical compositions in the medicine for preparing antiinflammatory, analgesia or treatment rheumatoid arthritis.
Pharmaceutical composition of the present invention, Herba pterocephali total saponin extracts and total iridoid glucoside extract compatibility are used, its antiinflammatory resisting rheumatoid disease effect is better than each single extract, there is synergistic function, especially with the Herba pterocephali total saponin extracts: Herba pterocephali total iridoid glucoside extract (10: 1) effect is best, curative effect is more stable, for clinical application provides new selection.
Obviously, according to foregoing of the present invention, according to ordinary skill knowledge and the customary means of this area, not breaking away under the above-mentioned basic fundamental thought of the present invention prerequisite, can also make modification, replacement or the change of other various ways.
The specific embodiment of form, be described in further detail foregoing of the present invention again by the following examples.But this should be interpreted as to the scope of the above-mentioned theme of the present invention only limits to following example.All technology realized based on foregoing of the present invention all belong to scope of the present invention.
The accompanying drawing explanation
Figure 1A A rat hindlimb constitutional swelling symptom, a left side is Normal group, the right side is model control group;
Fig. 2 AA rat forelimb performance Secondary cases swelling symptom, a left side is Normal group, the right side is model control group.
The specific embodiment
The preparation of embodiment 1 Herba pterocephali total saponin extracts of the present invention
Get Herba pterocephali crude drug 1000g cutting, add the 1600ml water-wet, then use the 6000ml water boiling and extraction 2 times, each 1.5h, filter, after filtrate is concentrated, the centrifugal precipitation of removing, water extract is diluted to 0.1g crude drug/ml medicinal liquid, adopts loading under D101 type macroporous adsorbent resin room temperature, and the loading flow velocity is 2BV/h, 1 times of (medical material: resin=1: 1) that applied sample amount is resin demand, with the 4BV water elution, flow velocity is 2BV/h, discards eluent; With the 70%v/v ethanol elution of 3BV, elution flow rate is 3BV/h, the eluent decompression recycling ethanol, be dissolved in 60%v/v ethanol, add excessive saturated neutral lead acetate solution, stir, make the Herba pterocephali total saponin extracts precipitate fully, filter, get precipitation and be suspended in 70%v/v ethanol, pass into excess hydrogen sulfide gas deleading, filter, get filtrate and pass into air again and slough hydrogen sulfide gas, decompression recycling ethanol is to the thick paste shape, drying, obtain total saponin extracts.
Take oleanolic acid as reference substance, adopt total saponin extracts content in the colorimetric method for determining extract, the results are shown in Table 1.
Table 1
In the Herba pterocephali total saponin extracts, saponin content, in oleanolic acid, should, lower than 50%w/w, not select saponin content to be not less than the Herba pterocephali total saponin extracts of 80%w/w in the present invention.Simultaneously, do not detect in the Herba pterocephali total saponin extracts and contain iridoid glycoside, with the regulation of " blank assay being disturbed and being allowed below 5% " in the study of tcm new drug guide, setting total iridoid glycoside extractive content in the Herba pterocephali total saponin extracts is 0-5%w/w.
The preparation of embodiment 2 Herba pterocephali total iridoid of the present invention glucoside extract
Get Herba pterocephali crude drug 1000g cutting, add the 1600ml water-wet, then add the 6000ml water boiling and extraction 2 times, each 1.5h, filter, and filtrate is concentrated, the centrifugal precipitation of removing, water extract is diluted to 0.1g crude drug/ml medicinal liquid, adopts loading under D101 type macroporous adsorbent resin room temperature, and the loading flow velocity is 2BV/h, 1 times of (medical material: resin=1: 1) that applied sample amount is resin demand, with the 4BV water elution, flow velocity is 2BV/h, discards eluent; With 70% ethanol elution of 3BV, elution flow rate is 3BV/h, the eluent decompression recycling ethanol, be dissolved in 80%v/v ethanol, add excessive saturated neutral lead acetate solution, stir, make the Herba pterocephali total saponin extracts precipitate fully, filter, get filtrate, decompression recycling ethanol, to the thick paste shape, is dissolved in water, n-butanol extraction three times, get n-butyl alcohol liquid, decompression and solvent recovery is to the thick paste shape, and drying, obtain the total iridoid glucoside extract.
Take loganin as reference substance, adopt the content of total iridoid glucoside extract in the colorimetric method for determining extract, the results are shown in Table 2.
Table 2
In Herba pterocephali total iridoid glucoside extract, iridoid glycoside content, in loganin, should, lower than 50%w/w, not select iridoid glycoside content to be not less than the Herba pterocephali total iridoid glucoside extract of 80%w/w in the present invention.
In the present invention, utilize lead acetate that the Herba pterocephali triterpene saponin is separated with iridoid glycoside, principle is referring to " Chemistry for Chinese Traditional Medicine ", the Xiao Chonghou chief editor, Shanghai science tech publishing house, 1997 the 1st edition, 389 pages, 440 pages.
The preparation of embodiment 3 pharmaceutical compositions of the present invention
Get the total saponin extracts 100g of embodiment 1 preparation, the total iridoid glucoside extract 10g of embodiment 2 preparations, and add proper starch, after wet granulation, drying, obtain medicament composition granule agent of the present invention.
The preparation of embodiment 4 pharmaceutical compositions of the present invention
Get the total saponin extracts 50g of embodiment 1 preparation, the total iridoid glucoside extract 50g of embodiment 2 preparations, and add suitable microcrystalline Cellulose, and after mixing, encapsulated, obtain medicament composition capsule agent of the present invention.
Below by the beneficial effect of pharmacology, test of pesticide effectiveness proof pharmaceutical composition of the present invention.
The drug efficacy study of test example 1 pharmaceutical composition of the present invention and Herba pterocephali total saponin extracts, iridoid glucoside extract
1.1 laboratory animal
Healthy Sprague-Dawley (SD) rat, clean level, complete male, body weight 180～220g; The healthy animal quality certification number: SCXK (river) 2008-24, produce and provide by Sichuan Academy of Medical Sciences institute of lab animals; Experimental animal feeding, at 24+2 ℃, in environment that night and daytime respectively replace in 12 hours, freely absorbs clean food and drinking-water, and animal is tested after conforming 3 days; Animal feeding and experimental implementation process strictly observe the dependency rule (NIH guide for the care and use of laboratory animals) of laboratory animal ethics and welfare.
1.2 the preparation of test medication
According to the Pharmacopoeia of the People's Republic of China 2010 editions and " Ministry of Health of the People's Republic of China's Tibetan medicine ministry standard " record, Coming-of-Age Day, consumption was 3g/60kg (in crude drug), therefore, by various Herba pterocephali extracts: Herba pterocephali total saponin extracts A (embodiment 1 preparation), iridoid glycoside B (embodiment 2 preparations), pharmaceutical composition C of the present invention (total saponin extracts: total iridoid glucoside extract=10: 1, embodiment 3 preparations), pharmaceutical composition D of the present invention (total saponin extracts: total iridoid glucoside extract=5: 5, embodiment 4 preparations) rat dosage is adjusted into 1250mg crude drug in whole/kg.
1.3 medicine and reagent
Nimesulide dispersible tablet (Nimesulide), Nanchang City Fei Hong pharmaceutcal corporation, Ltd, the accurate word of traditional Chinese medicines: H20020196, lot number: 091010, specification: 0.1g/ sheet, Coming-of-Age Day is used dosage: 0.2g/60kg, and dosage: 33.33mg/kg use in test, and during experiment, to be mixed with the medicinal liquid of 3.33mg/ml standby for the employing distilled water diluting;
Indometacin enteric-coated tablet (Indomethacin), Chongqing Ke Rui pharmaceutical Co. Ltd, the accurate word of traditional Chinese medicines: H50020263, lot number: 310001, specification: 25mg/ sheet, Coming-of-Age Day is used dosage: 75mg/60kg, and dosage: 12.5mg/kg use in test, and during experiment, the employing distilled water diluting is mixed with respectively 2.5, the medicinal liquid of 1.25mg/ml is standby;
Complete Freund's adjuvant (Freund ' s Adjuvant Complete), Sigma Chemical, lot number: 016K8900, specification: every milliliter of adjuvant is containing 1mg deactivation tubercule bacillus; The bacillus calmette-guerin vaccine lyophilized powder, Beijing Biological Product Inst., lot number: 20100413, specification: 60mg/ props up; Again add the bacill calmette-guerin of doses deactivation in the complete Freund's adjuvant of 1mg/ml, be prepared into every milliliter of complete Freund's adjuvant containing 10mg deactivation tubercule bacillus, 4 ℃ of stored refrigerated are standby.
Carrageenin (Carrageenin), Sigma Chemical, lot number: 073K0051.
1.4 statistical method
Adopt SPSS 11.5 statistical softwares to carry out statistical analysis.Measurement data means result with Mean ± SD, and between being organized with single factor variance analysis relatively, variance adopts the LSD check to data together, and heterogeneity of variance adopts Tamhane ' s T2 check; Ranked data employing non parametric tests is compared between being organized; P<0.05 o'clock, think that its group difference has significance.
2. on Carrageenan causes the impact of rat paw edema
2.1 experimental technique
60 of healthy male SD rats, be divided into 5 groups at random by body weight, is respectively model control group, positive controls (indomethacin) and Herba pterocephali extract A, B, C, D group.Each organizes rat every day by setting the continuous gastric infusion of dosage 7 days, and model control group gives the equal-volume solvent.
Mark in right back ankle joint before test, by sufficient volumetric method, measure sufficient volume twice, average as normal foot volume before administration; 30min after the last administration, in Rat Right metapedes sole of the foot section, subcutaneous injection 1% carrageenin solution 0.1ml causes inflammation, and respectively at cause scorching after 60,120,180, during 240min, be measured in the same method and respectively organize Rat Right metapedes volume, mean the anti-inflammatory effect of medicine with paw swelling (administration metapedes volume-administration front foot volume).
2.2 experimental result
After the carrageenin of Rat Right metapedes injection 1%, obvious swelling appears in sufficient pawl; With model control group, compare, Herba pterocephali extract A and B and compositions C, D can suppress carrageenin and cause rat paw edema, point out various Herba pterocephali extracts, to acute inflammation, certain inhibitory action is arranged, but wherein especially obvious with the effect of compositions C group, its effect is suitable with indomethacin, and therapeutic effect is more stable.The results are shown in Table 3.
Table 3 Herba pterocephali extract on Carrageenan causes the impact of rat paw edema
Annotate: with model control group, compare,
*p<0.05,
*p<0.01.
3 Herba pterocephali extracts cause the impact of rat assist agent arthritis (AA) model on complete Freund's adjuvant
3.1AA the foundation of rat model and dosage regimen
Get 70 of healthy male SD rats, by body weight, be divided at random 7 groups, be respectively Normal group, model control group, positive controls (nimesulide) and Herba pterocephali extract A, B, C, D group, every group of 10 rats.
The modeling of reference literature method, toes intradermal injection 0.1ml Freund's complete adjuvant after every Rat Right (every milliliter of adjuvant is containing 10mg deactivation tubercule bacillus), set up model of adjuvant arthritis in rats; The right back toes intradermal injection of rats in normal control group 0.1ml normal saline.
After rat intradermal injection complete Freund's adjuvant, obvious tumefaction appears in right back foot, approximately after 24h, peaks, and continues detumescence gradually after 3～5 days, is acute inflammatory reaction; What after modeling, after 8～9 days, occur once again causes scorching side joint and pedal swelling, engender non-joint and the pedal swelling that causes scorching side and two forelimbs after 12 days, the symptoms such as weight loss, color of the leather is unglazed, for the reaction of Secondary cases immune inflammation, and be considered as the index of adjuvant-induced arthritis model modeling success, concrete See Figure 1, Fig. 2.
After causing inflammation, each organizes rat according to setting dosage successive administration 30 days, and Normal group and model control group rat give the equal-volume distilled water.
3.2 the impact on the arthroncus of AA rat primary
3.2.1 experimental technique
Each organizes rat in causing scorching first 3 days by setting the dosage gastric infusion, normally reaches model control group and gives the equal-volume distilled water.Adopt volumetric method to measure to cause scorching before whole volume (ml) 2 times after Rat Right, get its meansigma methods as cause scorching before the normal foot volume; Simultaneously in cause scorching after 6,12,24,36,48,72h measurements cause scorching sufficient volume so that before and after scorching, difference means its swelling, the impact of observation Herba pterocephali extract on AA rat acute constitutional inflammation.
3.2.2. experimental result
With Normal group, compare, after Rat Right metapedes injection complete Freund's adjuvant, right back foot produces obvious tumefaction, and when causing scorching rear 12～36h, swelling reaches peak value; With model control group, compare, Herba pterocephali extract A, B and compositions C, D all can obviously suppress AA rat primary arthroncus due to complete Freund's adjuvant, show that all arthroncus has obvious inhibitory action to constitutional for Herba pterocephali total saponin extracts, total iridoid glucoside extract and both compositionss, but the most obvious with the effect of compositions C group, the effect of D group is taken second place, and the results are shown in Table 4.
The impact of table 4 Herba pterocephali extract on the foot swelling of AA rat primary
Annotate: with model control group, compare,
*p<0.05,
*p<0.01.
3.3 the impact on the arthroncus of AA rat Secondary cases
3.3.1 experimental technique
Adopt volumetric method to measure and cause the front left back foot of rat of inflammation (the non-inflammation foot that causes) sufficient volume (ml) 2 times, get its meansigma methods, as causing scorching front normal foot volume; And measure the non-sufficient volume-variation that causes scorching foot (left foot) respectively at causing scorching latter the 12nd, 18,24,30 days, to observe the impact of Herba pterocephali extract on the arthroncus of AA rat Secondary cases.
3.3.2 experimental result
With Normal group, compare, after Rat Right metapedes injection complete Freund's adjuvant 12d, left back foot produces obvious Secondary cases swelling, and when causing scorching rear 24d, swelling reaches peak value; With model group, compare, Herba pterocephali extract A, B and compositions C, D all can obviously suppress the foot swelling of AA rat Secondary cases, show that various Herba pterocephali extracts have stronger inhibitory action to the secondary inflammation due to the complete Freund's adjuvant immune stimulating, wherein, with compositions C group action effect the best, and curative effect is more stable, the effect of D group is taken second place, and the results are shown in Table 5.
The impact of table 5 Herba pterocephali extract on the foot swelling of AA rat Secondary cases
Annotate: with model control group, compare,
*p<0.05,
*p<0.01.
4. conclusion
Herba pterocephali total saponin extracts, Herba pterocephali total iridoid glucoside extract and compositions by a certain percentage thereof all can obviously suppress that carrageenin causes rat paw edema, can obviously reduce the AA rat primary, Secondary cases swollen joint expansibility.Wherein, by after total saponin extracts and the use of total iridoid glucoside extract compatibility, brought into play synergistic function, its antiinflammatory resisting rheumatoid disease effect is better than each single extract, especially with the Herba pterocephali total saponin extracts: Herba pterocephali total iridoid glucoside extract (10: 1) effect is best, and curative effect is more stable.
In sum, pharmaceutical composition of the present invention, Herba pterocephali total saponin extracts and total iridoid glucoside extract compatibility are used, its antiinflammatory resisting rheumatoid disease effect is better than each single extract, there is synergistic function, especially with the Herba pterocephali total saponin extracts: Herba pterocephali total iridoid glucoside extract (10: 1) effect is best, and curative effect is more stable, for clinical application provides new selection.
Claims (5)
1. one kind prepares the method for the treatment of the medicine for treating rheumatoid arthritis compositions, and it comprises the steps:
(1) prepare the Herba pterocephali total saponin extracts
A, get Herba pterocephali, extracting in water, filter, after filtrate is concentrated, the concentration of sample solution is formulated as to 0.1-0.2g crude drug/ml, adopt D101 type purification with macroreticular resin, the loading flow velocity is 1-3BV/h, and applied sample amount is counted medical material with medical material: resin=(0.5-1.5): 1w/w, with the 3-5BV water elution, flow velocity is 1-3BV/h, discards eluent; With 70% ethanol elution of 2-4BV, elution flow rate is 2-4BV/h.
Collect ethanol elution;
B, get the ethanol elution of step a, after decompression and solvent recovery, redissolve in 60-85%v/v ethanol, add saturated neutral lead acetate solution, stir, filter, filtrate for later use, get precipitation, be suspended in 60-85%v/v ethanol, with hydrogen sulfide gas or cation exchange resin deleading, filter, get filtrate concentrated, drying, obtain the Herba pterocephali total saponin extracts;
(2) prepare Herba pterocephali total iridoid glucoside extract
Get in step b the filtrate added after lead acetate solution, concentrated after, use n-butanol extraction, get n-butyl alcohol liquid, after the recovery solvent, drying, obtain Herba pterocephali total iridoid glucoside extract;
(3) preparation of pharmaceutical composition
Take Herba pterocephali total saponin extracts and total iridoid glucoside extract by the prescription proportioning, add adjuvant pharmaceutically commonly used to be prepared into preparation, wherein, the weight proportion of described total saponin extracts, total iridoid glucoside extract is:
Total saponin extracts 1-10 part, total iridoid glucoside extract 1-10 part.
2. method according to claim 1, it is characterized in that: the weight proportion of described total saponin extracts, total iridoid glucoside extract is:
10 parts of total saponin extracts, 1 part of total iridoid glucoside extract; Or 5 parts of total saponin extracts, 5 parts of total iridoid glucoside extracts.
3. method according to claim 1 and 2, it is characterized in that: in described Herba pterocephali total saponin extracts, saponin content is greater than 50%w/w; In described Herba pterocephali total iridoid glucoside extract, the total iridoid glycoside extractive content is greater than 50%w/w.
4. method according to claim 3, it is characterized in that: in described Herba pterocephali total saponin extracts, saponin content is greater than 80%w/w; In described Herba pterocephali total iridoid glucoside extract, iridoid glycoside content is greater than 80%w/w.
5. method according to claim 1, it is characterized in that: described Herba pterocephali is Dipsacaceae plant spoon leaf Herba pterocephali
pterocephalus hookeri(C.B.Clarke) the dry herb of Hoeck.
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| CN201310432934.8A CN103479688B (en) | 2011-03-09 | 2012-03-09 | A kind of pharmaceutical composition Preparation Method And The Use for the treatment of rheumatoid arthritis |
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| CN 201210061157 Expired - Fee Related CN102579519B (en) | 2011-03-09 | 2012-03-09 | Extracts of total saponins of pterocephalus hookeri and preparation method and application thereof |
| CN2012100611542A Expired - Fee Related CN102579518B (en) | 2011-03-09 | 2012-03-09 | Pterocephalus hookeri (C.B.Clarke) Hoeck total saponin extract and preparation method and application thereof |
| CN201210061163.1A Expired - Fee Related CN102614230B (en) | 2011-03-09 | 2012-03-09 | Medicinal composition for treating rheumatoid arthritis and preparation method and application thereof |
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| CN 201210061157 Expired - Fee Related CN102579519B (en) | 2011-03-09 | 2012-03-09 | Extracts of total saponins of pterocephalus hookeri and preparation method and application thereof |
| CN2012100611542A Expired - Fee Related CN102579518B (en) | 2011-03-09 | 2012-03-09 | Pterocephalus hookeri (C.B.Clarke) Hoeck total saponin extract and preparation method and application thereof |
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| CN103977044B (en) * | 2014-05-20 | 2017-11-14 | 上海中医药大学 | Hooker winghead root n-butanol portion extract and its production and use |
| CN104237446B (en) * | 2014-08-15 | 2015-10-28 | 山东金诃药物研究开发有限公司 | A kind of detection method of hooker winghead root |
| CN109771083B (en) * | 2019-03-28 | 2021-02-26 | 福建农林大学金山学院 | Method for realizing plantar injection by applying knee jerk reflex |
| CN110885385B (en) * | 2019-11-19 | 2020-09-25 | 西南大学 | Pterocephalus hookeri toxin A, application thereof and preparation method of pterocephalus hookeri extract with low liver injury toxicity |
| CN114276405B (en) * | 2021-12-06 | 2023-03-03 | 上海诗丹德标准技术服务有限公司 | Pentacyclic triterpenoid, preparation method and application thereof |
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| JP3887596B2 (en) * | 2002-11-05 | 2007-02-28 | 株式会社ノエビア | Skin preparation for moisturizing and skin preparation for improving rough skin |
| CN1292765C (en) * | 2003-12-26 | 2007-01-03 | 甘孜藏族自治州藏医药研究所 | Pharmaceutical composition, its preparation process and usage |
| CN102028722B (en) * | 2009-09-30 | 2012-08-29 | 上海中医药大学 | Extract of effective parts of total saponins in pterocephalus hookeri as well as preparation method and application thereof |
| CN101843630B (en) * | 2010-06-11 | 2012-07-18 | 首都医科大学宣武医院 | Composition containing iridoid and application thereof |
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| 关昕璐等.翼首草的抗炎作用与急毒实验研究.《北京中医药大学学报》.2004,第27卷(第2期),第71页左栏第1-2段、第72页右栏第1段. |
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| Publication number | Publication date |
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| CN103479688B (en) | 2015-12-23 |
| CN102579519B (en) | 2013-08-21 |
| CN103479688A (en) | 2014-01-01 |
| CN102579518A (en) | 2012-07-18 |
| CN102526141A (en) | 2012-07-04 |
| CN102614230A (en) | 2012-08-01 |
| CN102526141B (en) | 2013-07-10 |
| CN102579519A (en) | 2012-07-18 |
| CN102579518B (en) | 2013-11-27 |
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