CN105816769A - Lung benefiting tablets prepared from bulbus fritillariae ussuriensis and milkvetch roots and identification and content determination methods - Google Patents

Lung benefiting tablets prepared from bulbus fritillariae ussuriensis and milkvetch roots and identification and content determination methods Download PDF

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CN105816769A
CN105816769A CN201610332340.3A CN201610332340A CN105816769A CN 105816769 A CN105816769 A CN 105816769A CN 201610332340 A CN201610332340 A CN 201610332340A CN 105816769 A CN105816769 A CN 105816769A
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solution
adds
methanol
ethanol
radix
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杨静
陈贻焕
李春娥
郭奕
罗晓萍
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TONGHUA JITONG PHARMACEUTICAL CO Ltd
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TONGHUA JITONG PHARMACEUTICAL CO Ltd
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
    • A61K36/481—Astragalus (milkvetch)
    • A—HUMAN NECESSITIES
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    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/25—Araliaceae (Ginseng family), e.g. ivy, aralia, schefflera or tetrapanax
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    • A61K36/88—Liliopsida (monocotyledons)
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    • A61K9/2004—Excipients; Inactive ingredients
    • A61K9/2022—Organic macromolecular compounds
    • A61K9/205—Polysaccharides, e.g. alginate, gums; Cyclodextrin
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Abstract

The invention relates to a traditional Chinese medicine detection method, and discloses lung benefiting tablets prepared from bulbus fritillariae ussuriensis and milkvetch roots and identification and content determination methods .The lung benefiting tablets prepared from bulbus fritillariae ussuriensis and milkvetch roots are used for phthisis and are specially applicable to secondary pulmonary tuberculosis qi consuming and yin injuring syndrome .Radix stemonae, herba houttuyniae, rhizoma bletillae and radix notoginseng are selected as identification items, testing and screening are conducted through parameters, and the advantages of being good in chromatographic condition, good in specificity and reproducibility, rapid, economical and practical are achieved .A milkvetch root content determination method is selected, so that the method is high in specificity, high in accuracy and capable of effectively improving the product quality and better ensuring the curative effect of a product .The technology and detection method are reasonable, applicable and effective.

Description

Shellfish stilbene lung benefiting sheet and discriminating and content assaying method
Technical field
The present invention relates to the detection method of a kind of Chinese medicine, i.e. shellfish stilbene lung benefiting sheet and discriminating and content assaying method.For the Chinese medicine composition shellfish stilbene lung benefiting sheet of pulmonary tuberculosis, it is particularly well-suited to secondary pulmonary tuberculosis gas the moon consumption wound card.
Background technology
It is common for classifying according to doctor trained in Western medicine with " secondary pulmonary tuberculosis " clinically, secondary pulmonary tuberculosis is also known as adult type pulmonary tuberculosis, for infecting child lungy, the most static at primary affection or even recovery from illness one time after date, there occurs again active tuberculosis, its morbidity have two kinds may: one be that tubercule bacillus the most heavily becomes activity in outmoded primary tumor, causes focus resume combustion, claims endogenous to recur；One cure for primary infection after again by the external world infect tubercule bacillus and fall ill, claim exogenous redying.Secondary pulmonary tuberculosis is more common in more than 12 years old older children and teenager, and main sick type is infiltrative pulmonary tuberculosis.
Tuberculosis is with chemotherapeutic drugs such as Rimactazid, pyrazinamide, ethambutols as main treatment, determined curative effect, for legal treatment medicine, weak point is to be not less than the drug withdrawal of nine to ten two months ability the continuous use time, period causes a part of patient can not adhere to taking the full course for the treatment of or take because certain medicine in chemotherapy regimen is not suitable for individuality and frequently changes therapeutic scheme due to the inevitable toxic and side effects of this type of chemotherapeutic drugs, cause can not get effectively controlling, disease progression, some cases gives surgery pneumonectomy operative treatment.
Summary of the invention
It is an object of the invention to provide a kind of toxic and side effects little for above-mentioned deficiency, curative effect is reliable, detects rational shellfish stilbene lung benefiting sheet and discriminating and content assaying method.
The technical solution of the present invention is: a kind of shellfish stilbene lung benefiting sheet and discriminating and content assaying method, and step is as follows:
One, prepared by shellfish stilbene lung benefiting sheet: shellfish stilbene lung benefiting sheet by Radix Astragali 200g, Bulbus Lilii 100g, Radix Ophiopogonis 100g, Bulbus Fritillariae Ussuriensis 80g, Radix Stemonae (processed) 150 g, Radix Platycodonis 100g, Rhizoma Picrorhizae 150g, Radix Ranunculi Ternati 120g, Herba Houttuyniae 150g, Pseudobulbus Bletillae (Rhizoma Bletillae) 100g, Radix Notoginseng 50g make；Above ten simply, and Radix Notoginseng, Rhizoma Bletillae powder are broken into fine powder, cobalt-60 x ray irradiation x sterilizing；Bulbus Fritillariae Ussuriensis, the Radix Stemonae, Herba Houttuyniae add 70 ethanol extraction 2 times, 2 hours for the first time, 1 hour for the second time, united extraction liquid, and vacuum decompression reclaims ethanol, is concentrated into the clear paste of relative density 1.25～1.28；Medicinal residues and remaining Radix Astragali Six-element crude drug boiling secondary altogether, each 1 hour, collecting decoction, filtering, filtrate merges with above-mentioned clear paste, is concentrated into the thick paste that relative density is 1.30～1.32, add Radix Notoginseng, Pseudobulbus Bletillae (Rhizoma Bletillae) fine powder, mixing, be dried, it is ground into fine powder, adds starch, make granule, it is dried, adds magnesium stearate 4g, be pressed into 1000, film coating, to obtain final product.
Two, differentiate
(1) discriminating of Pseudobulbus Bletillae (Rhizoma Bletillae):
Take this product 10, finely ground, add methanol 20ml, supersound process 30 minutes, filters, and filtrate is evaporated, the residue 20ml that adds water makes dissolving, then adds hydrochloric acid 2ml, is heated to reflux 30 minutes, cool down immediately, with ether shaking extraction twice, each 40ml, merge ether solution, volatilizing, residue adds chloroform 1ml makes dissolving, as need testing solution.
Separately take Pseudobulbus Bletillae (Rhizoma Bletillae) control medicinal material 2g, be made in the same way of control medicinal material solution.
Testing according to thin layer chromatography, draw each 5 l of above two solution, put respectively on the same silica gel g thin-layer plate with sodium carboxymethyl cellulose as adhesive, with toluene-ethyl acetate=15:1 as developing solvent, launch, take out, dry, spray is with 5% vanillin-sulfuric acid test solution；In test sample chromatograph on position corresponding with control medicinal material chromatograph, the speckle of aobvious same color.
(2) discriminating of Herba Houttuyniae:
Take this product 10, finely ground, add ethyl acetate 20ml, supersound process 20 minutes, filter, filtrate is evaporated, and residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution.
Separately take Herba Houttuyniae control medicinal material 3g, be made in the same way of control medicinal material solution；Test according to thin layer chromatography, draw each 10 l of above two solution, put respectively on same silica gel g thin-layer plate, with n-hexane-ethyl acetate=9:1 as developing solvent, launch, take out, dry, put and inspect under uviol lamp；In test sample chromatograph, on position corresponding with control medicinal material chromatograph, aobvious identical blue fluorescence speckle.
(3) discriminating of the Radix Stemonae:
Take this product 8, finely ground, add 90 ethanol 20ml and 2 hydrochloric acid 1ml, it is heated to reflux 20 minutes, stands overnight, filter, being evaporated, the residue 10ml that adds water makes dissolving, adds strong ammonia solution and adjusts pH value to more than 10, with chloroform extraction three times, 10ml every time, merges chloroform liquid, is evaporated, residue adds 90% ethanol 1ml makes dissolving, as need testing solution.
Separately take Radix Stemonae control medicinal material 2g, be made in the same way of control medicinal material solution.
Test according to thin layer chromatography, draw need testing solution 15 l, control medicinal material solution 3 l, put respectively on the same silica gel G plate with sodium carboxymethyl cellulose as adhesive, with chloroform-methanol=10:1 as developing solvent, launch, taking out, dry, spray is with bismuth potassium iodide test solution；In test sample chromatograph, on position corresponding with control medicinal material, aobvious identical punctation.
(4) discriminating of Radix Notoginseng: take this product 8, finely ground, add methanol 30ml, supersound process 30 minutes, filter, filtrate is evaporated；The residue 20ml that adds water makes dissolving, extracts 4 times with the shaking of water saturated n-butyl alcohol, each 30ml, merge n-butanol extracting liquid, wash 2 times with ammonia solution, each 30ml, discarding ammoniacal liquor, n-butyl alcohol liquid is evaporated, and the residue 10ml that adds water makes dissolving, let cool, by neutral alumina column, with water 50ml eluting, discard water liquid, then with 70% ethanol 80ml eluting, collect eluent, being evaporated, residue adds methanol 1ml makes dissolving, as need testing solution.
Separately take Panax Notoginseng saponin R1Reference substance, ginsenoside Rg1Reference substance, adds methanol and makes every 1ml mixed solution respectively containing 0.5mg, as reference substance solution.
Test according to thin layer chromatography, draw need testing solution 15 l, reference substance solution 2 l, puts respectively on same silica gel g thin-layer plate, with chloroform-acetate-methanol-water=15:40:22:10,10 DEG C of lower floor's solution overnight arranged below are developing solvent, launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot development at 110 DEG C clear；In test sample chromatograph, on position corresponding with reference substance chromatograph, aobvious same color speckle.
Three, assay
Take this product 15, finely ground, accurately weighed, to put in apparatus,Soxhlet's, add methanol, heating and refluxing extraction 4 hours in water-bath, extracting solution reclaims methanol to dry；The residue 20ml that adds water makes dissolving, it is transferred in separatory funnel, extract 4 times with the shaking of water saturated n-butyl alcohol, 30ml every time, merge n-butanol extracting liquid, wash 2 times with ammonia solution, 30ml every time, discard ammoniacal liquor, n-butyl alcohol liquid is evaporated, the residue 10ml that adds water makes dissolving, let cool, by D101 type macroporous adsorptive resins, internal diameter 1.5cm, long 12cm, with water 50ml eluting, discard water liquid, again with 40% ethanol 50ml eluting, discard 40% ethanol elution, continue with 70% ethanol 50ml eluting, collect eluent, it is evaporated, residue adds methanol makes dissolving, and be transferred in 5ml measuring bottle, add methanol to scale, shake up, as need testing solution.
Separately take astragaloside reference substance, add methanol and make every 1ml solution containing 1mg, as reference substance solution.
Thin layer chromatography is tested, and draws need testing solution 10 l, reference substance solution 2 l and 4 l, cross point is on same silica gel g thin-layer plate respectively, and with chloroform-methanol-water=65:35:10,10 DEG C of lower floor's solution overnight arranged below are developing solvent, launch, take out, dry, spray with 10% ethanol solution of sulfuric acid, be heated to spot development at 100 DEG C clear, take out, lamellae covers an equal amount of glass plate, surrounding adhesive tape is fixed, and is scanned according to thin layer chromatography, wavelength:S=530nm,R=700nm, measures test sample trap integrated value and reference substance trap integrated value, calculates, to obtain final product.
The invention have the advantage that 1, through clinic, can improve rapidly tuberculosis symptoms, improve body's immunity, alleviate chemical therapy toxic side effect, promote sputum conversion, focus absorbs and void closing, and toxic and side effects is little, and curative effect is reliable, has the value of popularization and application.2, antitussive, eliminate the phlegm, stop blooding, antiinflammatory, several broad aspect such as regulation immunity have more satisfactory effect.3, choose the Radix Stemonae, Herba Houttuyniae, Pseudobulbus Bletillae (Rhizoma Bletillae), Radix Notoginseng, for differentiating item, is screened by parameter experiment, it is achieved chromatographic condition preferably, specificity and repeatability good, quick, economical and practical.Have chosen Radix Astragali content assaying method so that this method specificity is strong, accuracy is high, is effectively increased product quality, preferably ensure that the curative effect of product.Technique, detection method are reasonable, applicable, effectively.
Below in conjunction with embodiment, experimental example, embodiments of the present invention are described in further detail.
Detailed description of the invention
Shellfish stilbene lung benefiting sheet and discriminating and content assaying method:
Prescription: Radix Astragali 200g, Bulbus Lilii 100g, Radix Ophiopogonis 100g, Bulbus Fritillariae Ussuriensis 80g, Radix Stemonae (processed) 150 g, Radix Platycodonis 100g, Rhizoma Picrorhizae 150g, Radix Ranunculi Ternati 120g, Herba Houttuyniae 150g, Pseudobulbus Bletillae (Rhizoma Bletillae) 100g, Radix Notoginseng 50g.
Character: this product is Film coated tablets, aobvious brown color after removing coating；Mildly bitter flavor.
Preparation method: above ten simply, Radix Notoginseng, Rhizoma Bletillae powder are broken into fine powder, cobalt-60 x ray irradiation x sterilizing (6kGy)；Bulbus Fritillariae Ussuriensis, the Radix Stemonae, Herba Houttuyniae add 70 ethanol (volume fraction) and extract 2 times, 2 hours for the first time, 1 hour for the second time, united extraction liquid, and vacuum decompression reclaims ethanol, are concentrated into relative density 1.25～1.28(50 DEG C) clear paste；The Six-element boiling secondaries such as medicinal residues and remaining Radix Astragali, each 1.0 hours, collecting decoction, filter, filtrate merges with above-mentioned clear paste, be concentrated into relative density be 1.30～1.32(50 DEG C) thick paste, add Radix Notoginseng, Pseudobulbus Bletillae (Rhizoma Bletillae) fine powder, mixing, be dried, it is ground into fine powder, adds appropriate amount of starch, make granule, it is dried, adds magnesium stearate 4g, be pressed into 1000, film coating, to obtain final product.
Differentiate:
(1) discriminating of Pseudobulbus Bletillae (Rhizoma Bletillae): take this product 10, finely ground, add methanol 20ml, supersound process 30 minutes, filters, and filtrate is evaporated, the residue 20ml that adds water makes dissolving, then adds hydrochloric acid 2ml, is heated to reflux 30 minutes, cool down immediately, with ether shaking extraction twice, each 40ml, merge ether solution, volatilizing, residue adds chloroform 1ml makes dissolving, as need testing solution.Separately take Pseudobulbus Bletillae (Rhizoma Bletillae) control medicinal material 2g, be made in the same way of control medicinal material solution.According to thin layer chromatography (Chinese Pharmacopoeia one annex VI of version in 2010B) test, to draw each 5 l of above two solution, put respectively on the same silica gel g thin-layer plate with sodium carboxymethyl cellulose as adhesive, with toluene-ethyl acetate (15:1) as developing solvent, launch, take out, dry, spray is with 5% vanillin-sulfuric acid test solution.In test sample chromatograph on position corresponding with control medicinal material chromatograph, the speckle of aobvious same color.
(2) discriminating of Herba Houttuyniae: take this product 10, finely ground, add ethyl acetate 20ml, supersound process 20 minutes, filter, filtrate is evaporated, and residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution.Separately take Herba Houttuyniae control medicinal material 3g, be made in the same way of control medicinal material solution.Test according to thin layer chromatography (Chinese Pharmacopoeia one annex VI B of version in 2010), draw each 10 l of above two solution, put respectively on same silica gel g thin-layer plate, with n-hexane-ethyl acetate (9:1) as developing solvent, launch, take out, dry, put and inspect under uviol lamp (365nm).In test sample chromatograph, on position corresponding with control medicinal material chromatograph, aobvious identical blue fluorescence speckle.
(3) discriminating of the Radix Stemonae: take this product 8, finely ground, add 90 ethanol 20ml(volume fractions) and 2 hydrochloric acid 1ml(volume fractions), it is heated to reflux 20 minutes, stands overnight, filter, being evaporated, the residue 10ml that adds water makes dissolving, adds strong ammonia solution and adjusts pH value to more than 10, with chloroform extraction three times, 10ml every time, merges chloroform liquid, is evaporated, residue adds 90% ethanol 1ml makes dissolving, as need testing solution.Separately take Radix Stemonae control medicinal material 2g, be made in the same way of control medicinal material solution.Test according to thin layer chromatography (Chinese Pharmacopoeia one annex VI B of version in 2010), draw need testing solution 15 l, control medicinal material solution 3 l, put respectively on the same silica gel G plate with sodium carboxymethyl cellulose as adhesive, with chloroform-methanol (10:1) as developing solvent, launch, take out, drying, spray is with bismuth potassium iodide test solution.In test sample chromatograph, on position corresponding with control medicinal material, aobvious identical punctation.
(4) discriminating of Radix Notoginseng: take this product 8, finely ground, add methanol 30ml, supersound process 30 minutes, filter, filtrate is evaporated.The residue 20ml slight fever that adds water makes dissolving, extracts 4 times with the shaking of water saturated n-butyl alcohol, each 30ml, merge n-butanol extracting liquid, wash 2 times with ammonia solution, each 30ml, discard ammoniacal liquor, n-butyl alcohol liquid is evaporated, the residue 10ml slight fever that adds water makes dissolving, lets cool, by neutral alumina column (neutral alumina 100～120 mesh, 3g, internal diameter 1cm, long 10cm), with water 50ml eluting, discard water liquid, again with 70% ethanol 80ml eluting (volume fraction), collect eluent, be evaporated, residue adds methanol 1ml makes dissolving, as need testing solution.Separately take Panax Notoginseng saponin R1Reference substance, ginsenoside Rg1Reference substance, adds methanol and makes every 1ml mixed solution respectively containing 0.5mg, as reference substance solution.Test according to thin layer chromatography (Chinese Pharmacopoeia one annex VI B of version in 2010), draw need testing solution 15 l, reference substance solution 2 l, put respectively on same silica gel g thin-layer plate, with chloroform-10 DEG C of acetate-methanol-water (15:40:22:10) lower floor's solution overnight arranged below as developing solvent, launch, take out, drying, spray, with 10% ethanol solution of sulfuric acid (volume fraction), is heated to spot development at 110 DEG C clear.In test sample chromatograph, on position corresponding with reference substance chromatograph, aobvious same color speckle.
Inspection should meet every regulation (Chinese Pharmacopoeia one annex I D of version in 2010) relevant under tablet item.
Assay: take this product 15, finely ground, accurately weighed, to put in apparatus,Soxhlet's, add methanol appropriate, heating and refluxing extraction 4 hours in water-bath, extracting solution reclaims methanol to dry.The residue 20ml slight fever that adds water makes dissolving, it is transferred in separatory funnel, extract 4 times with the shaking of water saturated n-butyl alcohol, 30ml every time, merge n-butanol extracting liquid, wash 2 times with ammonia solution, 30ml every time, discard ammoniacal liquor, n-butyl alcohol liquid is evaporated, the residue 10ml slight fever that adds water makes dissolving, let cool, by D101 type macroporous adsorptive resins (internal diameter 1.5cm, long 12cm), with water 50ml eluting, discard water liquid, again with 40% ethanol 50ml eluting (volume fraction), discard 40% ethanol elution, continue with 70% ethanol 50ml eluting (volume fraction), collect eluent, it is evaporated, residue adds methanol makes dissolving in right amount, and be transferred in 5ml measuring bottle, add methanol to scale, shake up, as need testing solution.Separately take astragaloside reference substance, add methanol and make every 1ml solution containing 1mg, as reference substance solution.Test according to thin layer chromatography (Chinese Pharmacopoeia one annex VI B of version in 2010), draw need testing solution 10 l, reference substance solution 2 l and 4 l, cross point is on same silica gel g thin-layer plate respectively, with chloroform-methanol-water (65:35:10) 10 DEG C lower floor's solution overnight arranged below as developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid (volume fraction), it is heated to spot development clear at 100 DEG C, take out, lamellae covers an equal amount of glass plate, surrounding adhesive tape is fixed, according to thin layer chromatography (Chinese Pharmacopoeia one annex VI of version in 2010BThin layer chromatography scanning) it is scanned, wavelength:S=530nm,R=700nm, measures test sample trap integrated value and reference substance trap integrated value, calculates, to obtain final product.
This product every contains the Radix Astragali with astragaloside (C41H68O14) meter, 0.04mg must not be less than.

Claims (1)

1. the discriminating of a shellfish stilbene lung benefiting sheet and content assaying method, it is characterised in that step is as follows:
One, prepared by shellfish stilbene lung benefiting sheet: shellfish stilbene lung benefiting sheet by Radix Astragali 200g, Bulbus Lilii 100g, Radix Ophiopogonis 100g, Bulbus Fritillariae Ussuriensis 80g, Radix Stemonae (processed) 150 g, Radix Platycodonis 100g, Rhizoma Picrorhizae 150g, Radix Ranunculi Ternati 120g, Herba Houttuyniae 150g, Pseudobulbus Bletillae (Rhizoma Bletillae) 100g, Radix Notoginseng 50g make；Above ten simply, and Radix Notoginseng, Rhizoma Bletillae powder are broken into fine powder, cobalt-60 x ray irradiation x sterilizing；Bulbus Fritillariae Ussuriensis, the Radix Stemonae, Herba Houttuyniae add 70 ethanol extraction 2 times, 2 hours for the first time, 1 hour for the second time, united extraction liquid, and vacuum decompression reclaims ethanol, is concentrated into the clear paste of relative density 1.25～1.28；Medicinal residues and remaining Radix Astragali Six-element crude drug boiling secondary altogether, each 1 hour, collecting decoction, filtering, filtrate merges with above-mentioned clear paste, is concentrated into the thick paste that relative density is 1.30～1.32, add Radix Notoginseng, Pseudobulbus Bletillae (Rhizoma Bletillae) fine powder, mixing, be dried, it is ground into fine powder, adds starch, make granule, it is dried, adds magnesium stearate 4g, be pressed into 1000, film coating, to obtain final product；
Two, differentiate
(1) discriminating of Pseudobulbus Bletillae (Rhizoma Bletillae):
Take this product 10, finely ground, add methanol 20ml, supersound process 30 minutes, filters, and filtrate is evaporated, the residue 20ml that adds water makes dissolving, then adds hydrochloric acid 2ml, is heated to reflux 30 minutes, cool down immediately, with ether shaking extraction twice, each 40ml, merge ether solution, volatilizing, residue adds chloroform 1ml makes dissolving, as need testing solution；
Separately take Pseudobulbus Bletillae (Rhizoma Bletillae) control medicinal material 2g, be made in the same way of control medicinal material solution；
Testing according to thin layer chromatography, draw each 5 l of above two solution, put respectively on the same silica gel g thin-layer plate with sodium carboxymethyl cellulose as adhesive, with toluene-ethyl acetate=15:1 as developing solvent, launch, take out, dry, spray is with 5% vanillin-sulfuric acid test solution；In test sample chromatograph on position corresponding with control medicinal material chromatograph, the speckle of aobvious same color；
(2) discriminating of Herba Houttuyniae:
Take this product 10, finely ground, add ethyl acetate 20ml, supersound process 20 minutes, filter, filtrate is evaporated, and residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution；
Separately take Herba Houttuyniae control medicinal material 3g, be made in the same way of control medicinal material solution；Test according to thin layer chromatography, draw each 10 l of above two solution, put respectively on same silica gel g thin-layer plate, with n-hexane-ethyl acetate=9:1 as developing solvent, launch, take out, dry, put and inspect under uviol lamp；In test sample chromatograph, on position corresponding with control medicinal material chromatograph, aobvious identical blue fluorescence speckle；
(3) discriminating of the Radix Stemonae:
Take this product 8, finely ground, add 90 ethanol 20ml and 2 hydrochloric acid 1ml, it is heated to reflux 20 minutes, stands overnight, filter, being evaporated, the residue 10ml that adds water makes dissolving, adds strong ammonia solution and adjusts pH value to more than 10, with chloroform extraction three times, 10ml every time, merges chloroform liquid, is evaporated, residue adds 90% ethanol 1ml makes dissolving, as need testing solution；
Separately take Radix Stemonae control medicinal material 2g, be made in the same way of control medicinal material solution；
Test according to thin layer chromatography, draw need testing solution 15 l, control medicinal material solution 3 l, put respectively on the same silica gel G plate with sodium carboxymethyl cellulose as adhesive, with chloroform-methanol=10:1 as developing solvent, launch, taking out, dry, spray is with bismuth potassium iodide test solution；In test sample chromatograph, on position corresponding with control medicinal material, aobvious identical punctation；
(4) discriminating of Radix Notoginseng: take this product 8, finely ground, add methanol 30ml, supersound process 30 minutes, filter, filtrate is evaporated；The residue 20ml that adds water makes dissolving, extracts 4 times with the shaking of water saturated n-butyl alcohol, each 30ml, merge n-butanol extracting liquid, wash 2 times with ammonia solution, each 30ml, discarding ammoniacal liquor, n-butyl alcohol liquid is evaporated, and the residue 10ml that adds water makes dissolving, let cool, by neutral alumina column, with water 50ml eluting, discard water liquid, then with 70% ethanol 80ml eluting, collect eluent, being evaporated, residue adds methanol 1ml makes dissolving, as need testing solution；
Separately take Panax Notoginseng saponin R1Reference substance, ginsenoside Rg1Reference substance, adds methanol and makes every 1ml mixed solution respectively containing 0.5mg, as reference substance solution；
Test according to thin layer chromatography, draw need testing solution 15 l, reference substance solution 2 l, puts respectively on same silica gel g thin-layer plate, with chloroform-acetate-methanol-water=15:40:22:10,10 DEG C of lower floor's solution overnight arranged below are developing solvent, launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot development at 110 DEG C clear；In test sample chromatograph, on position corresponding with reference substance chromatograph, aobvious same color speckle；
Three, assay
Take this product 15, finely ground, accurately weighed, to put in apparatus,Soxhlet's, add methanol, heating and refluxing extraction 4 hours in water-bath, extracting solution reclaims methanol to dry；The residue 20ml that adds water makes dissolving, it is transferred in separatory funnel, extract 4 times with the shaking of water saturated n-butyl alcohol, 30ml every time, merge n-butanol extracting liquid, wash 2 times with ammonia solution, 30ml every time, discard ammoniacal liquor, n-butyl alcohol liquid is evaporated, the residue 10ml that adds water makes dissolving, let cool, by D101 type macroporous adsorptive resins, internal diameter 1.5cm, long 12cm, with water 50ml eluting, discard water liquid, again with 40% ethanol 50ml eluting, discard 40% ethanol elution, continue with 70% ethanol 50ml eluting, collect eluent, it is evaporated, residue adds methanol makes dissolving, and be transferred in 5ml measuring bottle, add methanol to scale, shake up, as need testing solution；
Separately take astragaloside reference substance, add methanol and make every 1ml solution containing 1mg, as reference substance solution；
Thin layer chromatography is tested, and draws need testing solution 10 l, reference substance solution 2 l and 4 l, cross point is on same silica gel g thin-layer plate respectively, and with chloroform-methanol-water=65:35:10,10 DEG C of lower floor's solution overnight arranged below are developing solvent, launch, take out, dry, spray with 10% ethanol solution of sulfuric acid, be heated to spot development at 100 DEG C clear, take out, lamellae covers an equal amount of glass plate, surrounding adhesive tape is fixed, and is scanned according to thin layer chromatography, wavelength:S=530nm,R=700nm, measures test sample trap integrated value and reference substance trap integrated value, calculates, to obtain final product.
CN201610332340.3A 2016-05-19 2016-05-19 Lung benefiting tablets prepared from bulbus fritillariae ussuriensis and milkvetch roots and identification and content determination methods Pending CN105816769A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108426955A (en) * 2018-03-11 2018-08-21 安徽省食品药品检验研究院 The discrimination method of tuber of stemona genunie medicinal materials
CN109692291A (en) * 2019-03-05 2019-04-30 贵州健兴药业有限公司 Lung power cough mixture medicinal extract and application thereof and method of quality control
CN110702833A (en) * 2019-09-27 2020-01-17 石家庄平安医院有限公司 Rapid thin-layer identification method for six medicinal materials in Jinling Changan capsule

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101417100A (en) * 2008-12-09 2009-04-29 通化永仓药业有限公司 Medicine for treating secondary lung tuberculosis and preparation method thereof
CN101530601A (en) * 2009-03-24 2009-09-16 吉林万通药业集团梅河药业股份有限公司 Astragalus edge tablets and its quality control method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101417100A (en) * 2008-12-09 2009-04-29 通化永仓药业有限公司 Medicine for treating secondary lung tuberculosis and preparation method thereof
CN101530601A (en) * 2009-03-24 2009-09-16 吉林万通药业集团梅河药业股份有限公司 Astragalus edge tablets and its quality control method

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108426955A (en) * 2018-03-11 2018-08-21 安徽省食品药品检验研究院 The discrimination method of tuber of stemona genunie medicinal materials
CN109692291A (en) * 2019-03-05 2019-04-30 贵州健兴药业有限公司 Lung power cough mixture medicinal extract and application thereof and method of quality control
CN110702833A (en) * 2019-09-27 2020-01-17 石家庄平安医院有限公司 Rapid thin-layer identification method for six medicinal materials in Jinling Changan capsule
CN110702833B (en) * 2019-09-27 2021-08-10 石家庄平安医院有限公司 Rapid thin-layer identification method for six medicinal materials in Jinling Changan capsule

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