CN105030722A - Preparation method of Antike capsules - Google Patents
Preparation method of Antike capsules Download PDFInfo
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- CN105030722A CN105030722A CN201510385236.6A CN201510385236A CN105030722A CN 105030722 A CN105030722 A CN 105030722A CN 201510385236 A CN201510385236 A CN 201510385236A CN 105030722 A CN105030722 A CN 105030722A
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Abstract
The invention provides a preparation method of Antike capsules. The method comprises the following steps: 1, carrying out refluxing extraction on a Chinese angelica raw material by using an ethanol-water solution, filtering, taking the obtained clear liquid, and concentrating to obtain Chinese angelica extract, wherein the Chinese angelica raw material preferably adopts coarse Chinese angelica powder; 2, decocting a toad skin raw material in water, and filtering to obtain dry toad skin extract, wherein the toad skin raw material preferably adopts coarse toad skin powder; 3, mixing the Chinese angelica extract obtained in step 1 with the dry toad skin extract obtained in step 2 according to a mass ratio of 0.8-2.3, adding a wetting agent, and uniformly mixing; and 4, granulating, finishing, drying, and filling capsules to obtain the Antike capsules. Effective components of raw medicinal materials are extracted through the method, so few contents in the capsules under a same content requirement are met, thereby the capsules are shrunk, patient deglutition is facilitated, and especially esophageal cancer patients are benefited.
Description
Technical field
The present invention relates to a kind of preparation method of compound Chinese medicinal preparation, particularly a kind of preparation method of Antike capsule.
Background technology
Antike capsule is the compound Chinese medicinal preparation be made up of Radix Angelicae Sinensis, Cutis Bufonis, has hard masses softening and resolving, removing toxic substances analgesic therapy, the effect of nourshing blood and promoting blood circulation.For esophageal carcinoma ecchymosis disease, share the curative effect that can strengthen the esophageal carcinoma, gastric cancer and hepatocarcinoma with radiotherapy, the clinical symptoms of patient, life quality can be improved.
Cutis Bufonis is the dry skin of Bufonidae animal Bufo siccus (BufobufogargarizansCantor) or Bufo melanostictus (BufomelanostictusSchneider), it has heat-clearing and toxic substances removing, effect of diuretic relieving distension, the content of its effective ingredient is most important for the curative effect of Antike capsule.In Cutis Bufonis, the active component of contained Venenum Bufonis about has more than ten to plant, and mainly (be called Venenum Bufonis poison (bufotoxins), its main chemical compositions is cinobufagin, resibufogenin etc. for bufalin (bufogenins) and its lipid.
Principle active component in Radix Angelicae Sinensis is ferulic acid, has antiplatelet aggregation, suppresses platelet 5-HT release, suppresses the generation of platelet thrombus element a2 (txa2), strengthen prostaglandin activity, analgesia, the effects such as alleviating vascular spasm.
Existing Antike capsule preparation technology, for Radix Angelicae Sinensis medical material and Cutis Bufonis medical material to be pulverized respectively, granulates, filled capsules, packaging.Such preparation technology due to Radix Angelicae Sinensis medical material and the process of Cutis Bufonis medical material simple, cause effective ingredient cinobufagin, resibufogenin and the ferulaic acid content fluctuation or unstable in Antike capsule, and these effective ingredient can not be absorbed fully by patient, the medication dose of patient and medicining times are increased, limits the extensive clinical practice of Antike capsule.
Therefore, be necessary to be optimized the preparation method of existing Antike capsule and to improve.
Summary of the invention
For the needs in above-mentioned industry and market, the object of the present invention is to provide a kind of preparation method of Antike capsule, this preparation method achieves the accurate control of the content to effective ingredient cinobufagin, resibufogenin and the ferulic acid in Antike capsule, effective ingredient in Antike capsule can be made full use of by patient, improve the compliance that this product uses.
The invention provides a kind of preparation method of Antike capsule, described method comprises:
1) by Radix Angelicae Sinensis raw material with ethanol water reflux, extract, filter, get clear liquid, concentrated to obtain eumenol; Preferably, described Radix Angelicae Sinensis raw material is Radix Angelicae Sinensis coarse powder;
2) by Cutis Bufonis raw material with soak by water, filter, concentrated obtain Cutis Bufonis dry extract; Preferably, described Cutis Bufonis raw material is Cutis Bufonis coarse powder;
3) by step 1) gained eumenol and step 2) gained Cutis Bufonis dry extract is that the ratio of 0.8-2.3:1 mixes with mass ratio, then, adds wetting agent, mixing;
4) after granulation, granulate, dry also filled capsules, obtains Antike capsule.
According in one embodiment of the invention, step 1) volumetric concentration of described ethanol water is 50 ~ 95%; Preferably, the volumetric concentration of described ethanol water is 60 ~ 80%, and more preferably, the volumetric concentration of described ethanol water is 65%.
According in one embodiment of the invention, step 1) in be 3 ~ 7 times of the quality of described Radix Angelicae Sinensis raw material in the volume of ethanol water in the described reflux, extract, of ml:g, the time of reflux, extract, is 0.5 ~ 3 hour; Preferably, in reflux, extract, the volume of ethanol water is 4 times of the quality of described Radix Angelicae Sinensis raw material, and the time of reflux, extract, is 1.0 hours; More preferably, reflux, extract, 1 ~ 2 time is repeated.
According in one embodiment of the invention, step 1) described eumenol is by by step 1) described clear liquid is evaporated to paste at 45 ~ 55 DEG C, reclaim ethanol to tasteless, drying obtains.
According in one embodiment of the invention, step 2) described Cutis Bufonis dry extract be by by Cutis Bufonis raw material with water soaking 0.5 ~ 3 hour, then be the soak by water of 8 ~ 16 times 20 ~ 70 minutes of the quality of described Cutis Bufonis raw material in order to quality, filter, be cooled to less than 40 DEG C, concentrate and obtain Cutis Bufonis dry extract; Preferably, the medicinal residues obtained to described filtration are that the water of 5 ~ 10 times of described medicinal residues quality decocts 10 ~ 50 minutes again in order to quality, after decoction liquor being merged, filter, concentrated, obtain Cutis Bufonis dry extract.
According in one embodiment of the invention, step 3) described wetting agent to be volumetric concentration be 30 ~ 60% alcoholic solution; Being preferably volumetric concentration is the alcoholic solution of 55.5%.
According in one embodiment of the invention, step 4) described drying is carried out in exsiccator, and the inlet temperature setting described exsiccator is 60-100 DEG C, leaving air temp is 45-85 DEG C, 1 ~ 3 hour drying time; Preferably, described capsule is No. 4 hard capsules; More preferably, described capsule loading amount is 0.09-0.13g/ grain.
According in one embodiment of the invention, described preparation method is further comprising the steps of:
5) with high performance liquid chromatography to step 4) total amount of cinobufagin in the Antike capsule of gained and resibufogenin detects; Preferably, described high performance liquid chromatography is filler with octadecylsilane chemically bonded silica, take acetonitrile as mobile phase A, will using g:ml concentration be 0.5% potassium dihydrogen phosphate aqueous solution as Mobile phase B, described potassium dihydrogen phosphate aqueous solution with formic acid adjust ph for 2.5; Described high performance liquid chromatography is 296nm at determined wavelength, and flow velocity is 1.0ml/min, carries out under the testing conditions that column temperature is 40 DEG C;
6) with high performance liquid chromatography to step 4) ferulaic acid content in the Antike capsule of gained detects; Preferably, described high performance liquid chromatography take octadecylsilane chemically bonded silica as filler, and methanol-1% glacial acetic acid solution is mobile phase, and wherein, methanol and volumetric concentration are the volume ratio of the glacial acetic acid solution of 1% is 30:70; Described high performance liquid chromatography is carried out under determined wavelength is the testing conditions of 320nm.
Further, present invention also offers a kind of Antike capsule prepared according to above-mentioned method.Described Antike capsule loading amount is 0.09-0.13g/ grain; Preferably, described capsule is No. 4 hard capsules.
On the other hand, the present invention has following beneficial effect:
The preparation method of Antike capsule provided by the invention and the Antike capsule of preparation thereof have following beneficial effect relative to existing corresponding preparation technology and product:
1, the control of Cutis Bufonis effective ingredient.Principle active component in Cutis Bufonis is cinobufagin and resibufogenin, accurately can control cinobufagin and resibufogenin total amount by extracting.
2, the control of Radix Angelicae Sinensis effective ingredient.Principle active component in Radix Angelicae Sinensis is ferulic acid, by extracting the content that accurately can control ferulic acid.
3, capsule number reduces.By extracting raw medicinal herbs effective ingredient, the capsule 's content meeting equal volume requirement being tailed off, therefore can reduce capsule, be conducive to patient swallow, particularly to patient with esophageal carcinoma advantageously.
4, take quantity to reduce.By extracting raw medicinal herbs effective ingredient, extracts many again can be filled in capsule even less in the capsule of former use, the content of every capsules being improved, dose can be made thus to be kept to 1 by 2 and just can reach taking dose requirement.
Accompanying drawing explanation
The chromatogram that Fig. 1 is cinobufagin shown in table 2 and resibufogenin standard substance;
Fig. 2 is the detection chromatogram of sample 1 cinobufagin and resibufogenin content;
Fig. 3 is the detection chromatogram of sample 2 cinobufagin and resibufogenin content;
Fig. 4 is the detection chromatogram of sample 3 cinobufagin and resibufogenin content;
Fig. 5 is the chromatogram of the standard substance of ferulic acid shown in table 3;
Fig. 6 is the detection chromatogram of ferulaic acid content in sample 1;
Fig. 7 is the detection chromatogram of ferulaic acid content in sample 2;
Fig. 8 is the detection chromatogram of ferulaic acid content in sample 3.
Detailed description of the invention
Further illustrate the present invention below in conjunction with embodiment, should be appreciated that embodiment only for further illustrating and explaining the present invention, not for limiting the present invention.
embodiment 1chinese medicine extraction
1. Radix Angelicae Sinensis extracts
Get Radix Angelicae Sinensis coarse powder and add 50% ~ 95% ethanol water reflux, extract, the volume of the ethanol water added in ml:g is 3 ~ 7 times amount of the quality of Radix Angelicae Sinensis coarse powder, reflux 0.5 ~ 3.0 hour, filter, get clear liquid, at 45-55 DEG C, be evaporated to paste, reclaim ethanol to tasteless, drying, obtains extractum for subsequent use.
2. Cutis Bufonis extracts
Get Cutis Bufonis coarse powder, add the water that quality is 8 ~ 16 times amount of the quality of Cutis Bufonis coarse powder, decoct 20 ~ 70 minutes, filter, be cooled to less than 40 DEG C, be condensed into dry extract, for subsequent use.
embodiment 2chinese medicine extraction
1. Radix Angelicae Sinensis extracts
Get Radix Angelicae Sinensis coarse powder and add 60 ~ 80% ethanol water reflux, extract, twice, the volume of the ethanol water at every turn added is 4 ~ 6 times amount of the quality of Radix Angelicae Sinensis coarse powder, reflux 1.0 ~ 2.0 hours, filter, get clear liquid, at 45-55 DEG C, be evaporated to paste, reclaim ethanol to tasteless, drying, obtains extractum for subsequent use.
2. Cutis Bufonis extracts
Get Cutis Bufonis coarse powder, soak 0.5 ~ 3 hour, add the water that quality is 10 ~ 15 times amount of the quality of Cutis Bufonis coarse powder, decoct 30 ~ 60 minutes, filter, medicinal residues add the water of 5 ~ 10 times amount again, then decoct 10 ~ 50 minutes, merge secondary decoction liquor, filter, be cooled to less than 40 DEG C, be condensed into dry extract, for subsequent use.
embodiment 3chinese medicine extraction
1. Radix Angelicae Sinensis extracts
Get Radix Angelicae Sinensis coarse powder and add 65% ethanol water reflux, extract, twice, the volume of the ethanol water at every turn added is 4 times amount of Radix Angelicae Sinensis coarse powder, refluxes 1.0 hours, filter, get clear liquid, at 45-55 DEG C, be evaporated to paste, reclaim ethanol to tasteless, dry, obtain eumenol for subsequent use.
2. Cutis Bufonis extracts
Get Cutis Bufonis coarse powder, soak 1.5 hours, add the water that volume is 14 times amount of the quality of Cutis Bufonis coarse powder, decoct 30 minutes, filter, medicinal residues add the water of 6 times amount again, then decoct 15 minutes, merge secondary decoction liquor, filter, be cooled to less than 40 DEG C, be condensed into Cutis Bufonis dry extract, for subsequent use.
embodiment 4preparation
The present embodiment use prepares Antike capsule according to the eumenol of embodiment 3 preparation and Cutis Bufonis dry extract.
1 takes raw material
Take appropriate eumenol and Cutis Bufonis dry extract with the ratio that the mass ratio of eumenol and Cutis Bufonis dry extract is 0.8 ~ 2.3:1, take 95% appropriate ethanol simultaneously, make the total amount of eumenol and Cutis Bufonis extractum and the mass ratio of 95% ethanol be 6.7:1.The mass ratio of eumenol and Cutis Bufonis dry extract is preferably 1.6:1, to obtain preferably effect.
2 granulate
2.1 join wetting agent: the ethanol of concentration 95% and appropriate purified water are hybridly prepared into the ethanol water that volumetric concentration is 30 ~ 60%, and being preferably embodied as using volumetric concentration is that the ethanol water of 55.5% is as wetting agent.
The wet grain of 2.2 system: put in the blender of wet granulator by the eumenol of a doses, Cutis Bufonis extractum, make it seal, opens after stirring arm is dry mixed 20 minutes with low or first gear and shuts down.Add the wetting agent preparing a doses, open stirring arm with low or first gear wet mixing after 1 minute, then open granulation oar low speed and granulate 2 ~ 4 minutes; Open dispensing valve, be discharged in clean container.
2.3 dry
Wet granular is laid in the exsiccator of boiling drier, hermetically drying device, setting inlet temperature and leaving air temp, careful unlatching steam valve, starts blower fan, starts dry, inlet temperature slowly should be raised up to design temperature, and avoiding heats up suddenly causes particle drying uneven; In order to ensure material thermally equivalent, shut down after dry 45 minutes, turning over materials once.Unlatching stirring paddle continues to be dried to leaving air temp and reaches setting value, dry end.Every pot of dry run about 2.0 ~ 3.2 hours, discharging is in clean container.
2.4 granulate
By dry granule through crushing and pelletizing, material is transferred to mixing chamber.
2.5 always mix
Dry granule is placed in mixer, closes charging aperture, start mixing, after mixing terminates, open discharging opening, be discharged in the clean container of inner lining plastic bag.
3 capsule-fillings
Check medicinal hard capsule and should be No. 4 capsules.
Medicinal hard capsule is joined in capsule hopper, open vacuum, granule is added in filling machine hopper, regulate feed time, setting stick car test is looked into, and adjustment loading, appoints and get 10, calculate average particle weight after weighing, deduction capsulae vacuus weight, adjustment loading amount is theoretical loading amount 0.09-0.13g/ grain.
Every 20 minutes, randomly draw 10 and check that average loading amount should meet the requirements.As fluctuation appears in average loading amount, should adjust in time.
4 is aluminum-plastic packaged
Adjustment Aluminium-coating Packer extremely following state, upper hot plate 110-140 DEG C, lower hot plate 110-140 DEG C.Heat-seal temperature 170-210 DEG C, print temperature 100-150 DEG C.Die-cut speed: 60 ~ 80 cut/min, start rolling inspection hollow plate molding situation, after qualified, loaded by intermediate products in the drug bucket of Aluminium-coating Packer, start is carried out aluminum-plastic packaged.
embodiment 5: the content detection of Antike capsule
One, the content of the effective ingredient of prepared according to the methods of the invention Antike capsule is detected
1, total quantity measuring method of cinobufagin and resibufogenin
Chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filler; Acetonitrile is mobile phase A, is Mobile phase B, carries out gradient elution by table 1 in 0.5% potassium dihydrogen phosphate (be the potassium dihydrogen phosphate aqueous solution of 0.5% with g:ml compound concentration, then with formic acid adjust ph for 2.50);
Table 1 chromatograph detects the gradient elution of cinobufagin and resibufogenin
| Time (minute) | Mobile phase A (%) | Mobile phase B (%) |
| 0～70 | 34.7 | 65.3 |
| 70～90 | 34.7→90 | 65.3→10 |
| 90～110 | 90→34.7 | 10→65.3 |
| 120 | 34.7 | 65.3 |
Determined wavelength is 296nm; Flow velocity is 1.0ml/min; Column temperature is 40 DEG C.Number of theoretical plate presses cinobufagin peak and resibufogenin peak calculates, and is not less than 4000 respectively.
Cinobufagin is got in the preparation of reference substance solution, resibufogenin reference substance is appropriate, accurately weighed, adds methanol and makes every lml respectively containing the solution of cinobufagin and resibufogenin 7.5 μ g/ml and 2.5 μ g/ml, to obtain final product.
The content under content uniformity item is got in the preparation of need testing solution, mixing, take about 2g, accurately weighed, add 100ml methanol, to put in water-bath reflux 1 hour, use buchner funnel sucking filtration, residue proper amount of methanol washs three times, merging filtrate, filtrate puts evaporate to dryness in water-bath, residue adds a small amount of dissolve with methanol, and evaporate to dryness methanol after stirring with 1g silica gel (200-300 order), upper silicagel column, with thiacyclohexane: chloroform: acetone (4:3:3) eluting, collect eluent 50ml, evaporate to dryness, residue dissolve with methanol, move into completely in 10ml measuring bottle, and be diluted to scale by methanol constant volume, obtain.
Algoscopy is accurate respectively draws reference substance solution 10 μ l, need testing solution 10 μ l, injection liquid chromatography, and record chromatogram, measures, to obtain final product.
According to said method, the Antike capsule sampling prepared according to embodiment 4 is detected.Fig. 1 is the chromatogram that table 2 is depicted as cinobufagin and resibufogenin reference substance, Fig. 2 is the detection chromatogram of sample 1 cinobufagin and resibufogenin content, Fig. 3 is the detection chromatogram of sample 2 cinobufagin and resibufogenin content, and Fig. 4 is the detection chromatogram of sample 3 cinobufagin and resibufogenin content.Be about 44.5 ~ 45.2min at the appearance time of above-mentioned each figure cinobufagin, and the appearance time of resibufogenin is about 49.5 ~ 50.3min.The content of sample cinobufagin and resibufogenin is calculated according to the main peak area of reference substance collection of illustrative plates and test sample collection of illustrative plates.Sample the testing result obtained for three times as shown in table 2:
The total amount sampling Detection of table 2 Antike capsule cinobufagin and resibufogenin
2, ferulaic acid content detection method
Chromatographic condition and system suitability experiment octadecylsilane chemically bonded silica are filler, and methanol-1% glacial acetic acid solution (30:70) is mobile phase, determined wavelength 320nm, and number of theoretical plate should be not less than 3500 by ferulic acid peak.
The preparation precision of reference substance solution takes ferulic acid reference substance 10mg, puts in 100ml measuring bottle, adds dissolve with methanol and be diluted to scale, shake up, precision measures 1ml, puts in 10ml measuring bottle, add methanol dilution to scale, shake up, obtain (every 1ml is containing ferulic acid 0.01mg)
The content that the preparation of need testing solution takes under content uniformity item is appropriate, mixing, accurately weighed, take about 0.6g, accurately weighed, precision adds methyl alcohol-formic acid (95:5) solution 25ml, close plug, supersound extraction 30 minutes, filters, discard just filtrate, get subsequent filtrate as need testing solution.
Algoscopy is accurate respectively draws reference substance solution and each 10 μ l of need testing solution, and injection liquid chromatography, records peak area, calculates, to obtain final product.
According to said method, the Antike capsule sampling prepared according to embodiment 4 is detected.Fig. 5 is the chromatogram that table 3 is depicted as ferulic acid reference substance, and Fig. 6 is the detection chromatogram of ferulaic acid content in sample 1, and Fig. 7 is the detection chromatogram of ferulaic acid content in sample 2, and Fig. 8 is the detection chromatogram of ferulaic acid content in sample 3.Calculating the content of ferulic acid in sample according to the main peak area of reference substance collection of illustrative plates and test sample collection of illustrative plates, to sample the testing result obtained for three times as shown in table 3:
Ferulaic acid content sampling Detection in table 3 Antike capsule
Two, the content of the effective ingredient of the Antike capsule prepared according to former process is detected
Adopt the content of detection method to the effective ingredient of the Antike capsule prepared according to former technique same as described above to detect, result is as shown in table 4, table 5
Ferulaic acid content sampling Detection in Antike capsule prepared by the former technique of table 4
The total amount sampling Detection of Antike capsule cinobufagin prepared by the former technique of table 5 and resibufogenin
From above-mentioned result of sampling inspection, although the volume-diminished of Antike capsule capsule prepared by process according to the present invention, but the content of the effective ingredient in capsule significantly improves, dose can be made thus to be kept to one of the present invention by original 2 and can to reach taking dose requirement.And, the fluctuation of the active constituent content in Antike capsule is also significantly improved according to process of the present invention, accurately can control the total amount of capsule cinobufagin and resibufogenin and the content of ferulic acid, further ensure stability and the safety of medicine.
Although present invention has been description to a certain degree, significantly, under the condition not departing from the spirit and scope of the present invention, can carry out the suitable change of each condition.Be appreciated that and the invention is not restricted to described embodiment, and be attributed to the scope of claim, it comprises the equivalent replacement of described each factor.
Claims (10)
1. a preparation method for Antike capsule, is characterized in that, described method comprises:
1) by Radix Angelicae Sinensis raw material with ethanol water reflux, extract, filter, get clear liquid, concentrated to obtain eumenol; Preferably, described Radix Angelicae Sinensis raw material is Radix Angelicae Sinensis coarse powder;
2) by Cutis Bufonis raw material with soak by water, filter, obtain Cutis Bufonis dry extract; Preferably, described Cutis Bufonis raw material is Cutis Bufonis coarse powder;
3) by step 1) gained eumenol and step 2) gained Cutis Bufonis dry extract is 0.8 ~ 2.3:1 with mass ratio ratio mixes, and then, adds wetting agent, mixing;
4) after granulation, granulate, dry also filled capsules, obtains Antike capsule.
2. the method for claim 1, is characterized in that, step 1) described in the volumetric concentration of ethanol water be 50 ~ 95%; Preferably, the volumetric concentration of described ethanol water is 60 ~ 80%, and more preferably, the volumetric concentration of described ethanol water is 65%.
3. method as claimed in claim 1 or 2, is characterized in that, step 1) in be 3 ~ 7 times of the quality of described Radix Angelicae Sinensis raw material in the volume of ethanol water in the described reflux, extract, of ml:g, the time of reflux, extract, is 0.5 ~ 3 hour; Preferably, in reflux, extract, the volume of ethanol water is 4 times of the quality of described Radix Angelicae Sinensis raw material, and the time of reflux, extract, is 1.0 hours; More preferably, reflux, extract, 1 ~ 2 time is repeated.
4. the method as described in any one in claims 1 to 3, is characterized in that, step 1) described eumenol is by by step 1) described clear liquid is evaporated to paste at 45 ~ 55 DEG C, reclaim ethanol to tasteless, drying obtains.
5. the method according to any one of Claims 1 to 4, it is characterized in that, step 2) described Cutis Bufonis dry extract be by by Cutis Bufonis raw material with water soaking 0.5 ~ 3 hour, then be the soak by water of 8 ~ 16 times 20 ~ 70 minutes of the quality of described Cutis Bufonis raw material with quality, filter, be cooled to less than 40 DEG C, concentrate and obtain Cutis Bufonis dry extract; Preferably, the medicinal residues described filtration obtained are that the water of 5 ~ 10 times of described medicinal residues quality decocts 10 ~ 50 minutes again with quality, after decoction liquor being merged, filter, concentrate, obtain Cutis Bufonis dry extract.
6. the method as described in any one of Claims 1 to 5, is characterized in that, step 3) described wetting agent to be volumetric concentration be 30 ~ 60% alcoholic solution; Being preferably volumetric concentration is the alcoholic solution of 55.5%.
7. the method as described in any one of claim 1 ~ 6, is characterized in that, step 4) described drying is carried out in exsiccator, and the inlet temperature setting described exsiccator is 60-100 DEG C, leaving air temp is 45-85 DEG C, 1 ~ 3 hour drying time; Preferably, described capsule is No. 4 hard capsules; More preferably, described capsule loading amount is 0.09-0.13g/ grain.
8. the method as described in any one of claim 1 ~ 7, is characterized in that, described method also comprises:
5) with high performance liquid chromatography to step 4) total amount of cinobufagin in the Antike capsule of gained and resibufogenin detects; Preferably, described high performance liquid chromatography is filler with octadecylsilane chemically bonded silica, take acetonitrile as mobile phase A, will in g:ml concentration be 0.5% potassium dihydrogen phosphate for Mobile phase B, described potassium dihydrogen phosphate with formic acid adjust ph for 2.5; Described high performance liquid chromatography is 296nm at determined wavelength, and flow velocity is 1.0ml/min, carries out under the testing conditions that column temperature is 40 DEG C;
6) with high performance liquid chromatography to step 4) ferulaic acid content in the Antike capsule of gained detects; Preferably, described high performance liquid chromatography take octadecylsilane chemically bonded silica as filler, and methanol-1% glacial acetic acid solution is mobile phase, and wherein, methanol and volumetric concentration are the volume ratio of the glacial acetic acid solution of 1% is 30:70; Described high performance liquid chromatography is carried out under determined wavelength is the testing conditions of 320nm.
9. the Antike capsule prepared of the method for a basis as described in any one of claim 1 ~ 8.
10. Antike capsule as claimed in claim 9, it is characterized in that, described Antike capsule loading amount is 0.09-0.13g/ grain; Preferably, described capsule is No. 4 hard capsules.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106511414A (en) * | 2016-12-13 | 2017-03-22 | 长春雷允上药业有限公司 | Pharmaceutical composition for treating tumor and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101632696A (en) * | 2008-07-22 | 2010-01-27 | 长春国奥药业有限公司 | Medicinal composition for treating malignant tumor and preparation method thereof |
-
2015
- 2015-06-30 CN CN201510385236.6A patent/CN105030722A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101632696A (en) * | 2008-07-22 | 2010-01-27 | 长春国奥药业有限公司 | Medicinal composition for treating malignant tumor and preparation method thereof |
Non-Patent Citations (7)
| Title |
|---|
| 孙凌飞，等: "蟾皮当归合剂对肾癌细胞的放射敏感性的影响及作用机制探讨", 《中国肿瘤临床与康复》 * |
| 李瑛，等: "安替可胶囊物效基础研究进展", 《亚太传统医药》 * |
| 杨明，等: "《中药药剂学》", 31 August 2008, 上海科学技术出版社 * |
| 殷佩浩，等: "《中药蟾酥的研究与应用》", 31 December 2014, 第二军医大学出版社 * |
| 王晓东，等: "蟾皮提取分离方法及有效成分的研究进展", 《武警医学院学报》 * |
| 申文江，等: "安替可对肾癌细胞的放射敏感性影响", 《第八届全国中西医结合肿瘤学术会议论文集》 * |
| 詹益兴，等: "《绿色精细化工 天然产品制造法 第4集》", 28 February 2009, 科学技术文献出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106511414A (en) * | 2016-12-13 | 2017-03-22 | 长春雷允上药业有限公司 | Pharmaceutical composition for treating tumor and preparation method and application thereof |
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Application publication date: 20151111 |