CN1309373C - Granular preparation for treating cancer and its quality control method - Google Patents
Granular preparation for treating cancer and its quality control method Download PDFInfo
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- CN1309373C CN1309373C CNB2004100780993A CN200410078099A CN1309373C CN 1309373 C CN1309373 C CN 1309373C CN B2004100780993 A CNB2004100780993 A CN B2004100780993A CN 200410078099 A CN200410078099 A CN 200410078099A CN 1309373 C CN1309373 C CN 1309373C
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- 206010028980 Neoplasm Diseases 0.000 title claims abstract description 32
- 201000011510 cancer Diseases 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 238000003908 quality control method Methods 0.000 title claims abstract description 18
- 239000008187 granular material Substances 0.000 claims abstract description 33
- CWVRJTMFETXNAD-FWCWNIRPSA-N 3-O-Caffeoylquinic acid Natural products O[C@H]1[C@@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-FWCWNIRPSA-N 0.000 claims abstract description 25
- PZIRUHCJZBGLDY-UHFFFAOYSA-N Caffeoylquinic acid Natural products CC(CCC(=O)C(C)C1C(=O)CC2C3CC(O)C4CC(O)CCC4(C)C3CCC12C)C(=O)O PZIRUHCJZBGLDY-UHFFFAOYSA-N 0.000 claims abstract description 25
- CWVRJTMFETXNAD-KLZCAUPSSA-N Neochlorogenin-saeure Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O CWVRJTMFETXNAD-KLZCAUPSSA-N 0.000 claims abstract description 25
- CWVRJTMFETXNAD-JUHZACGLSA-N chlorogenic acid Chemical compound O[C@@H]1[C@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-JUHZACGLSA-N 0.000 claims abstract description 25
- 229940074393 chlorogenic acid Drugs 0.000 claims abstract description 25
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- 235000001368 chlorogenic acid Nutrition 0.000 claims abstract description 25
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- 239000003814 drug Substances 0.000 claims abstract description 20
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- 238000000034 method Methods 0.000 claims abstract description 19
- 150000007965 phenolic acids Chemical class 0.000 claims abstract description 16
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
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- 230000004580 weight loss Effects 0.000 claims description 3
- XXMFJKNOJSDQBM-UHFFFAOYSA-N 2,2,2-trifluoroacetic acid;hydrate Chemical compound [OH3+].[O-]C(=O)C(F)(F)F XXMFJKNOJSDQBM-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
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- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims description 2
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- 238000012850 discrimination method Methods 0.000 claims 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 claims 1
- 206010058467 Lung neoplasm malignant Diseases 0.000 abstract description 4
- 208000005718 Stomach Neoplasms Diseases 0.000 abstract description 4
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Abstract
The present invention relates to a preparation method and a quality control method of a Chinese patent medicine granule which has the functions of resisting cancer, relieving inflammation and relieving asthma and is mainly used for treating diseases of esophagus cancer, gastric cancer, lung cancer, liver cancer, etc. The granule of the present invention comprises glaucescent fissistigma root which is used as a raw medicinal material, 100 parts by weight of beta-cyclodextrin which is used as an auxiliary solvent, 3 parts by weight of aspartame which is used as a corrective and 390 parts by weight of dextrine which is used as a molding agent. The preparation technology comprises advanced methods of dissolution assistance with beta-cyclodextrin, spray drying and dry granulation, effective components are completely preserved, and continuous mass production under a GMP condition can be realized conveniently. The quality control method comprises thin layer identification of glaucescent fissistigma root, content measurement of chlorogenic acid, content measurement of total phenolic acid and content measurement of total alkaloid.
Description
(technical field)
The present invention relates to a kind of Chinese patent medicine preparation that is used for diseases such as esophageal carcinoma, gastric cancer, pulmonary carcinoma, hepatocarcinoma the disappear flat particulate preparation method of cancer, method of quality control, belong to the field of Chinese medicines.
(background technology)
Tumor is a commonly encountered diseases, multiple and high lethal disease, and wherein esophageal carcinoma, gastric cancer, pulmonary carcinoma, hepatocarcinoma then are the highest kinds of mortality rate in this systemic disease.The sickness rate of tumor has tangible age characteristics, and it increases with advancing age, and the age is big more, and sickness rate is high more, and the research pay attention to day by day of such medicine is used also increasingly extensive.If the modern chemistry drug main suppresses the cytotoxic drug of tumor growth, it is very big mostly to be symptomatic treatment and side effect, and major part has a strong impact on immunity and digestive system.Wherein also do not have to suppress tumor growth again to human consumption, immune system have no side effect safe, efficient, can be for the medicine of taking for a long time, and develop the Chinese medicine traditional advantage, exploitation preparation stabilization, drug safety, dosage is accurate, quality controllable, the reliable Chinese medicine preparation of curative effect is significant.
The Chinese medicine XIAOAIPING TANGJIANG is a kind of Chinese medicine patent medicine preparation that is used for diseases such as esophageal carcinoma, gastric cancer, pulmonary carcinoma, hepatocarcinoma, made by main material medicine Radix Fissistigmatis Glaucescentis, Radix Fissistigmatis Glaucescentis is the dry rattan of Asclepiadaceae milk Lepidium plant Caulis Marsdeniae Tenacissimae, and Radix Fissistigmatis Glaucescentis has anticancer, antiinflammatory, antiasthmatic effect.The extraction process of at present commercially available XIAOAIPING TANGJIANG is all boiled through decocting and is removed by filter precipitation then and insoluble matter is made, and this can cause a part of water solublity relatively poor as loss of active ingredients such as phenolic acids and alkaloidss, thereby influences the curative effect of medicine; In addition, syrup is solution state, and some effective ingredient such as chlorogenic acid etc. are unstable in aqueous solution, also can cause the reduction of active constituent content.The said preparation method of quality control is more backward simultaneously, has only simple qualitative identification, can't control its quality better, guarantees curative effect.Above-mentioned reason makes XIAOAIPING TANGJIANG be difficult to reach curative effect height, good stability, the high requirement of quality control degree of accuracy of modern medicines.So content of the present invention just provides a kind of preparation method and method of quality control thereof of Radix Astragali essenc granule novel form.
(summary of the invention)
One of purpose of the present invention provides a kind of Chinese medicine flat particulate preparation method of cancer that disappears, and two of purpose provides the flat particulate method of quality control of a kind of cancer that disappears.
Inventing the flat granule of cancer that disappears is that crude drug is made by Radix Fissistigmatis Glaucescentis 3750 weight portions, and medicament also contains cosolvent beta-schardinger dextrin-100 weight portions, contains forming agent oligomeric lactose 390 weight portions.
The present invention's flat granule of cancer that will disappear adopts advanced preparation technology, is prepared from as beta-schardinger dextrin-hydrotropy, spray drying, dry granulation etc., and it is more that effective ingredient such as chlorogenic acid, total phenolic acid and total alkaloids are kept, and improved our curative effect.
The disappear method of quality control of the flat granule of cancer of the present invention: 1, Radix Fissistigmatis Glaucescentis has been carried out the thin layer discriminating; 2, with high effective liquid chromatography for measuring chlorogenic acid contents; 3, with determined by ultraviolet spectrophotometry the content of total phenolic acid; 4, with gravimetric detemination total alkaloid contents wherein, this has improved the quality control standard of preparation greatly, guarantees the curative effect of preparation effectively.
The preparation method of the flat granule of cancer that disappears of the present invention is as follows:
Get Radix Fissistigmatis Glaucescentis 3750 weight portions, decoct with water three times, collecting decoction leaves standstill, filter, it is 1.06～1.12 (50 ℃) that filtrate is concentrated into relative density, gets clear paste, adds inclusion agents beta-schardinger dextrin-100 weight portions, fully stir, under atomize, feed hot-air, carry out spray drying, 170-180 ℃ of hot-air inlet temperature, leaving air temp 70-90 ℃, get spray powder, add-on type agent oligomeric lactose 390 weight portions add correctives aspartame 3 weight portions again, dry granulation under 18-60 ℃ of temperature, granulate, packing, every bag of 4g, promptly.
The method of quality control of the flat granule of cancer that disappears of the present invention is as follows:
(1) thin layer of Radix Fissistigmatis Glaucescentis is differentiated
Get the about 10g of this product, porphyrize adds hot water 100ml dissolving, is concentrated into 20ml, puts in the separatory funnel, adds strong ammonia solution 1ml, with dichloromethane 40ml, 30ml difference extracting twice.Combining extraction liquid volatilizes, and residue adds methanol 2ml makes dissolving, as need testing solution.Other gets control medicinal material 10g, adds 50% ethanol 100ml reflux, extract, 30 minutes, is concentrated into 20ml, put in the separatory funnel, add strong ammonia solution 0.5ml dichloromethane 40ml, 30ml extracting twice respectively, merge extractive liquid,, volatilize, residue adds methanol 2ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (appendix VI B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, exhibition cylinder built-in one little hartshorn bottle, be developing solvent with dichloromethane-methanol-strong ammonia solution (20: 2: 0.25) after saturated 1 hour, launch, take out, dry, put under the uviol lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(2) chlorogenic acid contents is measured
The preparation of reference substance solution: it is an amount of that precision takes by weighing the chlorogenic acid reference substance, adds methanol and make the solution that contains 0.025mg among every 1ml, in contrast product solution.
The preparation of need testing solution: get powder 0.8g, the accurate title, decide, and puts in the tool plug conical flask, the accurate 50% methanol 50ml that adds, and close plug claims to decide weight, supersound process 30min.Put coldly, weigh, supply weightlessness, shake up with 50% methanol,, (10000rpm) centrifugal 10 minutes at a high speed gets supernatant, promptly.
With octadecylsilane chemically bonded silica is filler;
Flow velocity: 1.0ml/min;
Mobile phase is:
Methanol 23 volumes
0.1% trifluoroacetic acid water, 77 volumes
Mobile phase can also for
Methanol 23 volumes
0.1% phosphate aqueous solution, 77 volumes
The detection wavelength is 326nm;
Number of theoretical plate calculates by the chlorogenic acid peak should be not less than 3000.
(3) assay of total phenolic acid
UV spectrophotometer measuring
The detection wavelength is 326nm;
With the methanol solution is blank, with ultraviolet spectrophotometry (appendix V of Chinese Pharmacopoeia version in 2000
A) content of the total phenolic acid of detection.
(4) total alkaloid contents is measured
With the chloroform is extractant extraction alkaloid
Gravimetric method is calculated total alkaloid content.
(specific embodiment)
The disappear preparation of the flat granule of cancer of embodiment one
Take by weighing Radix Fissistigmatis Glaucescentis 375g, alcohol extraction twice decocted 2 hours for the first time, decocted 2 hours for the second time, merge pure liquid, filter, reclaim ethanol, be condensed into relative density 1.10 (70 ℃) and get extractum, 60 ℃ of insulations add beta-schardinger dextrin-10g, stir, spray drying gets spray powder, add aspartame 0.5g, lactose 39g, mixing, material is dry granulation under 50 ℃ of temperature, and granulate gets brown particle 100g.Be distributed into bag by each dose 4.0g.
Embodiment two beta-schardinger dextrin-s disperse the selection of hydrotropy condition
Because the water-soluble of the more contained phenolic acids effective ingredient of we is relatively poor, regular meeting has precipitation to produce in the extracting solution, so adopt beta-schardinger dextrin-to make its better dispersion, increases its dissolubility.In order to select the dispersive optimum condition of beta-schardinger dextrin-, four comparative tests have been carried out.
Take by weighing Radix Fissistigmatis Glaucescentis 18.75kg, decoct with water three times, collecting decoction leaves standstill, filter, it is 1.10 (50 ℃) that filtrate is concentrated into relative density, clear paste, with 5 parts of clear paste div in par aeq, add not commensurability beta-schardinger dextrin-respectively, after stirring evenly, mesh screen filters, and spray drying gets spray powder.As investigating index, investigate its influence with total phenolic acid, the results are shown in Table 1 total phenolic acid retention rate.
Table 1 beta-schardinger dextrin-consumption is to the influence of total phenolic acid retention rate
The result shows, solubilization-aid effect was still undesirable when the beta-schardinger dextrin-consumption was 25g, when increasing to 50g, the retention rate of total phenolic acid is higher, when increasing to 100g and 200g again as the beta-schardinger dextrin-consumption, the retention rate difference of index components is little during with 50g, considers production cost and solubilization-aid effect, and the consumption of best beta-schardinger dextrin-is 100g.
Mainly contain effective component content in flat granule of embodiment three types of diabetes cancer and the XIAOAIPING TANGJIANG relatively
" the flat granule of the cancer that disappears " carried out the assay comparative test with " XIAOAIPING TANGJIANG ", is index, experimental result such as following table with chlorogenic acid wherein, total phenolic acid and total alkaloid contents.
Table 3 " the flat granule of the cancer that disappears " has carried out the assay comparative test with " XIAOAIPING TANGJIANG "
| Group | Index components | ||
| Chlorogenic acid | Total phenolic acid | Total alkaloids | |
| XIAOAIPING TANGJIANG (mg/15ml) the raising rate (%) of the flat granule of cancer (mg/ bag) granule that disappear than former syrup | 3.4 5.2 52.94 | 87.5 142.4 62.74 | 4.8 8.7 81.25 |
The result who is recorded by last table shows that chlorogenic acid, total phenolic acid, total alkaloid contents are compared with XIAOAIPING TANGJIANG (contained crude drug amount is suitable with every bag of contained crude drug amount of the flat granule of the cancer that disappears in every 15ml XIAOAIPING TANGJIANG) and be significantly improved in the flat granule of the cancer that disappears.This preparation has adopted the inclusion of beta-schardinger dextrin-, makes liposoluble ingredient and alkaloids composition that some water solublity are relatively poor obtain good reservation, and makes the suspension type granule, and the composition that extracts medicinal liquid is fully kept, and active constituent content obviously increases.And in the former syrup, above-mentioned effective ingredient can concentrate at medicinal liquid, can lose when filtering, and poor stability and easily decompose and destroy in aqueous solution such as liposoluble ingredient such as chlorogenic acid, also can influence content of effective.
Embodiment four outlet and inlet temperature are to the influence of spray drying powder
The spray drying condition is very important to the reservation and the grain forming of composition.For the benefit of the reservation of effective ingredient and grain forming compare as table 4 inlet temperature, leaving air temp.
Table 4 outlet and inlet temperature is to the influence of spray drying powder
| Inlet temperature (℃) | Leaving air temp (℃) | Chlorogenic acid retention rate (%) | Water content (%) | To the influence of granulating |
| 190 180 180 170 170 | 90 80 70 80 70 | 75.1 84.1 90.5 94.5 96.7 | 2.9 3.3 4.3 4.5 5.0 | Poor slightly better fine better |
The granulation result of the test shows, the water content of this preparation semi-finished product fine silt is at 4.0～6.0% o'clock, and directly dry type makes granularity, granule that hardness is suitable; Water content is higher than at 8.0% o'clock, and mobility of particle is relatively poor, and the back moisture of granulating is difficult to be controlled in 5%; Water content was less than 4.0% o'clock, and particulate fine powder is many slightly, and productive rate can descend.Therefore should control spray-dired inlet temperature is 170-180 ℃, leaving air temp 70-90 ℃.
Embodiment five disappears the flat granule of cancer by following method quality control ()
Radix Fissistigmatis Glaucescentis is differentiated and is got the about 10g of this product, and porphyrize adds hot water 100ml dissolving, is concentrated into 20ml, puts in the separatory funnel, adds strong ammonia solution 1ml, with dichloromethane 40ml, 30ml difference extracting twice.Combining extraction liquid volatilizes, and residue adds methanol 2ml makes dissolving, as need testing solution.Other gets control medicinal material 10g, adds 50% ethanol 100ml reflux, extract, 30 minutes, is concentrated into 20ml, put in the separatory funnel, add strong ammonia solution 0.5ml dichloromethane 40ml, 30ml extracting twice respectively, merge extractive liquid,, volatilize, residue adds methanol 2ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (appendix VI B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, exhibition cylinder built-in one little hartshorn bottle, be developing solvent with dichloromethane-methanol-strong ammonia solution (20: 2: 0.25) after saturated 1 hour, launch, take out, dry, put under the uviol lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
Embodiment six disappears the flat granule of cancer by following method quality control (two)
Chlorogenic acid contents is measured:
[assay] measured according to high performance liquid chromatography (61 pages of 2000 editions appendix of Chinese Pharmacopoeia).
Wherein flow phase system test shows: (v/v) (v/v) obtain similar analysis collection of illustrative plates when being mobile phase to methanol-0.1% trifluoroacetic acid aqueous solution (23: 77) with methanol-0.1% phosphate aqueous solution (23: 77), but trifluoroacetic acid is an organic acid, it is all little than phosphoric acid to the influence of chromatographic apparatus and chromatographic column, and it is preferably to make mobile phase pH reagent with trifluoroacetic acid.
System suitability test Waters510 pump, ultraviolet 486 detectors, the anti-phase C18 post of Huaiyin Han Bang Kromasil of company (4.6*250mm, 5 μ m), methanol-0.1% trifluoroacetic acid aqueous solution (23: 77) is a mobile phase (v/v), flow velocity is 1ml/min; The detection wavelength is 327nm.
Number of theoretical plate calculates by the chlorogenic acid peak should be not less than 3000.
The chlorogenic acid reference substance that the preparation precision of reference substance solution takes by weighing in 60 ℃ of drying under reduced pressure to constant weight is an amount of, and accurate the title decides, and methanol is mixed with and contains chlorogenic acid 0.025mg among every 1ml.
Content under this product content uniformity item is got in the preparation of need testing solution, and porphyrize is got powder 0.8g, and accurate the title decides, put in the tool plug conical flask accurate 50% methanol 50ml, the close plug of adding, claim to decide weight, supersound process 30min (ultrasonic power is 250w, and frequency is 50KHz).Put coldly, claim to decide weight again, supply with 50% methanol and subtract weight loss, shake up, (10000rpm) centrifugal 10 minutes at a high speed gets supernatant, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject hplc determination, calculate, promptly.
This product contains chlorogenic acid (C for every bag
15H
18O
9) must not be less than 4.0mg.
Embodiment seven disappears the flat granule of cancer by following method quality control (three)
The assay of total acid:
[assay] measured according to ultraviolet spectrophotometry (appendix VA of Chinese Pharmacopoeia version in 2000).
Instrument: Tianjin, island UV-2487 ultraviolet spectrophotometer.
With 50% methanol is blank, and the detection wavelength is 326nm.
The chlorogenic acid reference substance that the preparation precision of reference substance solution takes by weighing in 60 ℃ of drying under reduced pressure to constant weight is an amount of, and accurate the title decides, and makes the solution that every 1ml contains 0.01mg approximately with mobile phase, promptly.
Content under this product content uniformity item is got in the preparation of need testing solution, and porphyrize is got powder 0.05g, and accurate the title decides, put in the tool plug conical flask accurate 50% methanol 50ml, the close plug of adding, claim to decide weight, supersound process 30min (ultrasonic power is 250w, and frequency is 50KHz).Put coldly, claim to decide weight again, supply with 50% methanol and subtract weight loss, shake up, (10000rpm) centrifugal 10 minutes at a high speed gets supernatant, promptly.
Algoscopy gets reference substance solution respectively and need testing solution is put in the cuvette in right amount, measures, promptly.
This product contains total phenolic acid with chlorogenic acid (C for every bag
15H
18O
9) meter, must not be less than 120mg.
Embodiment eight disappears the flat granule of cancer by following method quality control (four)
Total alkaloid contents is measured:
[assay] gravimetric detemination total alkaloid contents
Assay method is got content under this product content uniformity item, and porphyrize is got powder 10.0g, and accurate the title decides, put in the tool plug conical flask, and 0.5% aqueous hydrochloric acid solution supersound extraction 3 times, each 30ml filters merging filtrate; Filtrate is washed 5 times with chloroform, and each 20ml discards chloroform solution, acid liquid is regulated pH value to 10 with ammonia, it is saturated to add sodium chloride, extracts 5 times with the chloroform jolting, each 20ml, the chloroform solution that merges 5 extractions, fling to solvent and promptly get total alkaloids, with come together total alkaloids be dried to constant weight for 105 ℃, move in the exsiccator, weigh rapidly after the cooling, calculate total alkaloid contents mensuration in the test sample.
This product contains total alkaloids for every bag, must not be less than 7.0mg.
Description of drawings:
Fig. 1 chlorogenic acid reference substance HPLC figure
Fig. 2 lacks Radix Fissistigmatis Glaucescentis negative sample HPLC figure
Fig. 3 compound recipe Radix Fissistigmatis Glaucescentis particulate samples HPLC figure
Claims (7)
1. a granule for the treatment of cancer is that crude drug is made by 3750 weight portion Radix Fissistigmatis Glaucescentiss, it is characterized in that: contain cosolvent beta-schardinger dextrin-100 weight portions, contain correctives aspartame 3 weight portions, contain forming agent oligomeric lactose 390 weight portions.
2. a kind of preparation method for the treatment of the granule of cancer according to claim 1 is as follows by concrete steps:
It is standby to take by weighing Radix Fissistigmatis Glaucescentis;
Decoct with water three times, collecting decoction leaves standstill, and filters, and it is to stop in 1.10 o'clock that filtrate is concentrated into relative density; Get clear paste, add inclusion agents beta-schardinger dextrin-100 weight portions, fully stir, under atomize, feed hot-air, carry out spray drying, 170-180 ℃ of hot-air inlet temperature, leaving air temp 70-90 ℃, get spray powder, add-on type agent oligomeric lactose 390 weight portions add correctives aspartame 3 weight portions again, dry granulation under 18-60 ℃ of temperature, granulate, packing, every bag of 4g, promptly.
3. a kind of Radix Fissistigmatis Glaucescentis discrimination method for the treatment of the granule of cancer according to claim 1 is characterized in that:
Get the about 10g of this product, porphyrize adds hot water 100ml dissolving, is concentrated into 20ml, puts in the separatory funnel, adds strong ammonia solution 1ml, with dichloromethane 40ml, 30ml difference extracting twice.Combining extraction liquid volatilizes, and residue adds methanol 2ml makes dissolving, as need testing solution, other gets control medicinal material 10g, adds 50% ethanol 100ml reflux, extract, 30 minutes, is concentrated into 20ml, put in the separatory funnel, add strong ammonia solution 0.5ml dichloromethane 40ml, 30ml extracting twice respectively, merge extractive liquid, volatilizes, residue adds methanol 2ml makes dissolving, in contrast medical material solution.Draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, exhibition cylinder built-in one little hartshorn bottle is that methylene chloride-methanol-strong ammonia solution of 20: 2: 0.25 is developing solvent with volume ratio after saturated 1 hour, launches, take out, dry, put under the 365nm uviol lamp and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
4. a kind of chlorogenic acid contents assay method for the treatment of the granule of cancer according to claim 1 is characterized in that:
The preparation of reference substance solution: the chlorogenic acid reference substance that precision takes by weighing in 60 ℃ of drying under reduced pressure to constant weight is an amount of, and accurate the title decides, and methanol is mixed with and contains chlorogenic acid 0.025mg among every 1ml;
The preparation of need testing solution: get content under this product content uniformity item, porphyrize is got powder 0.8g, the accurate title, decide, and puts in the tool plug conical flask, the accurate 50% methanol 50ml that adds, close plug claims to decide weight, supersound process 30min, put coldly, claim to decide weight again, with 50% methanol supply subtract lose weight, shake up, 10000rpm high speed centrifugation 10 minutes is got supernatant, promptly;
Chromatographic condition: with octadecylsilane chemically bonded silica is filler;
Mobile phase is: volume ratio is 23: 77 methanol-0.1% a trifluoroacetic acid water;
The detection wavelength is 326nm, flow velocity: 1ml/min;
Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid.
5. a kind of chlorogenic acid contents assay method for the treatment of the granule of cancer according to claim 4 is characterized in that:
Mobile phase is: volume ratio is 23: 77 methanol-0.1% phosphoric acid water.
6. a kind of method of quality control for the treatment of the granule of cancer according to claim 1 is characterized in that:
With 50% methanol is blank, and the detection wavelength is 326nm,
The preparation of reference substance solution: the chlorogenic acid reference substance that precision takes by weighing in 60 ℃ of drying under reduced pressure to constant weight is an amount of, and accurate the title decides, and makes the solution that every 1ml contains 0.01mg approximately with mobile phase, promptly;
The preparation of need testing solution: get content under this product content uniformity item, porphyrize is got powder 0.05g, the accurate title, decide, and puts in the tool plug conical flask, the accurate 50% methanol 50ml that adds, close plug claims to decide weight, supersound process 30min, put coldly, claim again to decide weight, supply with 50% methanol and subtract weight loss, shake up, 10000rpm high speed centrifugation 10 minutes is got supernatant, promptly;
Get reference substance solution and need testing solution respectively and put in right amount in the cuvette, measure the content of total phenolic acid.
7. a kind of method of quality control for the treatment of the granule of cancer according to claim 1 is characterized in that:
Get this product content, porphyrize is got powder 10.0g, and accurate the title decides, put in the tool plug conical flask, and 0.5% aqueous hydrochloric acid solution supersound extraction 3 times, each 30ml filters merging filtrate; Filtrate is washed 5 times with chloroform, and each 20ml discards chloroform solution, acid liquid is regulated pH value to 10 with ammonia, it is saturated to add sodium chloride, extracts 5 times with the chloroform jolting, each 20ml, the chloroform solution that merges 5 extractions, fling to solvent and promptly get total alkaloids, with come together total alkaloids be dried to constant weight for 105 ℃, move in the exsiccator, weigh rapidly after the cooling, measure total alkaloid contents.
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| CN100387234C (en) * | 2005-07-08 | 2008-05-14 | 张晴龙 | Medicine containing forrest silk vine root orherb aglycone, and its preparing method and use |
| CN101612183B (en) * | 2008-06-26 | 2011-12-21 | 江苏正大天晴药业股份有限公司 | Glaucescent fissistigma root saponin extract, pharmaceutical composition and preparation method and application thereof |
| CN104391065B (en) * | 2011-03-04 | 2016-03-30 | 南京圣和药业股份有限公司 | The method for building up of CAULIS MARSDENIAE TENACISSIMAE medicinal material and preparation finger and application |
| CN102526142B (en) * | 2012-03-17 | 2014-07-16 | 北京电子科技职业学院 | Glaucescent fissistigma root granules and preparation method thereof |
| CN107843665A (en) * | 2017-11-01 | 2018-03-27 | 汤臣倍健股份有限公司 | A kind of assay method of adenosine content and its application |
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| 中华人民共和国药品标准中药成方制剂第20册 277，中华人民共和国卫生部药典委员会 1998 * |
| 中华人民共和国药品标准中药成方制剂第20册 277，中华人民共和国卫生部药典委员会 1998;中华人民共和国药品标准中药成方制剂第20册 278，中华人民共和国卫生部药典委员会 1998 * |
| 中华人民共和国药品标准中药成方制剂第20册 278，中华人民共和国卫生部药典委员会 1998 * |
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