Summary of the invention
The objective of the invention is to: Chinese medicinal capsule agent and method for making and method of quality control that a kind of treatment apoplexy evident in efficacy is provided.
The present invention is achieved in that
One, prescription:
Radix Astragali 225g, Hirudo 100g, Rhizoma Chuanxiong 90g, Radix Angelicae Sinensis 90g, Flos Carthami 90g, Semen Persicae 113g, Radix Paeoniae Rubra 90g, Radix Aucklandiae 90g, Rhizoma Acori Graminei 90g, Pheretima 60g, Herba Taxilli 90g, Radix Et Caulis Acanthopanacis Senticosi extractum 35g.
Two, method for making:
More than 12 the flavor, except that Hirudo, Pheretima, Radix Et Caulis Acanthopanacis Senticosi dried cream powder are broken into the fine powder; Nine flavors such as all the other Radixs Astragali decoct with water secondary, 2 hours for the first time, 1.5 hours for the second time, filter, it is 1.1-1.2 (60 ℃) that collecting decoction, filtrate are concentrated into relative density, and spraying drying powder-forming adds Pheretima, Hirudo, Radix Et Caulis Acanthopanacis Senticosi powder mix homogeneously, incapsulate, make 1000, promptly.
Three, character:
This product is a capsule, and content is that yellowish-brown is to chocolate brown powder; The feeble QI raw meat, mildly bitter flavor.
Four, differentiate:
(1) gets this product content 2g, put in the conical flask, add 70% ethanol 30ml, reflux 30 minutes is put coldly, and evaporate to dryness in the evaporating dish is gone in filter, residue adds water 10ml, stirs to make dissolving, filters, filtrate is by strongly acidic cation-exchange (1.5g) post (long 15cm, internal diameter 1cm), and the water flushing is to colourless, use 1mol/L sodium hydroxide 10ml eluant solution then, collect eluent, transfer to neutrality with dilute hydrochloric acid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other trematodiasis control medicinal material 0.5g that fetches water shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw need testing solution 5 μ l, reference substance solution 10 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with 0.3% sodium carboxymethyl cellulose, be developing solvent with n-butyl alcohol-glacial acetic acid-water (4: 1: 1), launch, take out, dry, spray is with 0.2% ethanol solution of ninhydrin, about 5 minutes of 105 ℃ of bakings.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on show the speckle of same color.
(2) get this product content 1g, add chloroform 10ml, water-bath refluxed 30 minutes, filtered, and filtrate evaporate to dryness, residue add chloroform 0.5ml makes dissolving, as need testing solution.Other gets the isofraxidin reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B).Draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with 0.3% sodium carboxymethyl cellulose, be developing solvent with chloroform-methanol (95: 5), launch, taking-up is dried, and puts under the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(3) get this product content 3g, add 80% ethanol 30ml, heating in water bath refluxed 30 minutes, filter, filtrate evaporate to dryness, residue add water 15ml and heat and make dissolving, absorbent cotton filters, and collects filtrate, extracts 2 times with water-saturated n-butanol, each 10ml merges n-butanol extracting liquid, adds water 5ml washing, discard aqueous solution, n-butyl alcohol liquid evaporate to dryness, residue add that water 15ml is warm to make dissolving, and absorbent cotton filters, filtrate is transferred to D101 type macroporous adsorptive resins (long 3cm, internal diameter 1cm), the water flushing adds 70% ethanol 30ml eluting again to colourless, collect ethanol elution, evaporate to dryness, residue add methanol 0.5ml makes dissolving, as need testing solution.Other gets the peoniflorin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with 0.3% sodium carboxymethyl cellulose, with chloroform-methanol (5: 1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, 110 ℃ dry by the fire to the speckle colour developing clear.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on show the speckle of same color.
(4) get this product content 5g, add ethyl acetate-formic acid (9.5: 0.5) mixed liquor 20ml.Supersound process 25 minutes filters, and filtrate evaporate to dryness, residue add methanol 5ml makes dissolving, as need testing solution.Other gets Pheretima control medicinal material 0.5g, shines medical material solution in pairs with legal system.According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with toluene-ethyl acetate-formic acid (9: 1: 0.5) is developing solvent, saturated 30 minutes, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
Five, check:
Should meet every regulation relevant under the capsule item (an appendix I of Chinese Pharmacopoeia version in 2000 L).
Six, assay:
Get this product content 6g, the accurate title, decide, and puts in the conical flask, the accurate 2% potassium hydroxide methanol solution 50ml that adds claims to decide weight, heating and refluxing extraction 1 hour, put coldly, claim to decide weight, supply the weight that subtracts mistake with 2% potassium hydroxide methanol solution, shake up, filter, precision is measured subsequent filtrate 30ml, put in the evaporating dish, evaporate to dryness, residue add water 20ml makes dissolving, add chloroform-n-butyl alcohol (2: 1) mixed solution and extract 5 times, each 10ml, merge extractive liquid,, with ammonia solution washing 2 times, each 20ml discards ammoniacal liquor, chloroform-n-butyl alcohol liquid evaporate to dryness, the residue dissolve with methanol, and be transferred in the 2ml measuring bottle, add methanol and be diluted to scale, shake up, as need testing solution.It is an amount of that other gets the astragaloside reference substance, accurate claims surely, adds methanol and make solution that every 1ml contains 0.5mg product solution in contrast.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw need testing solution 4 μ l and 6 μ l, reference substance solution 3 μ l and 5 μ l, respectively the cross point in same be on the silica gel g thin-layer plate of adhesive with 0.3% sodium carboxymethyl cellulose, lower floor's solution with chloroform-methanol-water (65: 35: 10) (placing layering below 10 ℃) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear to dry by the fire to the speckle colour developing at 100 ℃, take out, on lamellae, cover onesize glass plate, use immobilization with adhesive tape on every side, scan according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B thin layer chromatography scanning), wavelength X S=530nm, λ R=650nm measures test sample trap integrated value and reference substance trap integrated value, calculate, promptly.
Every of this product contains the Radix Astragali with astragaloside (C
41H
68O
14) meter should be no less than 56 μ g.
Seven, function and curing mainly:
Inrigorating qi and promoting blood circulation, the removing blood stasis collateral dredging.Being used for the arteriosclerotic cerebral infarction convalescent period differential diagnosis in tcm is Qi deficiency blood stasis type apoplexy apoplex involving the channels and collaterals person, and disease is seen hemiplegia, hemianesthesia, distortion of commissure, dysphonia etc.
Eight, usage and dosage:
Oral, every 0.4g, one time 5,3 times on the one.
Results of pharmacodynamic test: observe the rheol influence of rabbit blood, can make hematocrit (%), blood plasma viscosity (ratio), whole blood height are cut viscosity (ratio), and whole blood is low cuts the remarkable decline of viscosity (ratio), make erythrocyte electrophoresis accelerate (P equal<0.05); To the influence of rat platelet aggregation function, but the inductive platelet aggregation of inhibition ADP (P<0.01) of highly significant: and the rabbit antithrombotic forms experiment, but the formation of the inhibition thrombosis of highly significant (P<0.01); To the influence of experimental anesthetized dog cerebral blood flow (ml/min) and cerebral vascular resistance (mmHg/ml/min), but the cerebral blood flow increasing amount of highly significant (P<0.01), and the highly significant low cerebral vascular resistance (P<0.001) of falling.