CN1876050A - Pharmaceutical preparation for treating prostatitis, its preparation process and quality control method - Google Patents
Pharmaceutical preparation for treating prostatitis, its preparation process and quality control method Download PDFInfo
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Abstract
Disclosed is a medicinal preparation for treating prostatitis, process for preparation and quality control method thereof, wherein the preparation is made mainly from Chinese medicinal herbs including corktree bark, radix paeoniae rubrathe, root of red rooted saliva, peach kernels and lycopus, or their extracts of corresponding weight parts.
Description
Technical field: the present invention is prostatitic medicinal preparation of QIANLIE ANTONG of a kind of treatment and preparation method thereof and method of quality control, belongs to technical field of Chinese medicine.
Technical background: between twenty and fifty period, the incident disease of prostate is mainly acute and chronic prostatitis.Trace it to its cause, between twenty and fifty period is the male's sexual animated period just, and sexual activity is frequent, easily causes prostatic hyperemia repeatedly under the stimulation of sexual excitation, brings out inflammation.Secondly, be the most vigorous period of prostate secretion between twenty and fifty period, for the growth of antibacterial provides good condition.If do not note Personal hygiene, infect at low or other position of Abwehrkraft des Koepers, and pathogen just can enter prostate, forms acute and chronic inflammation.According to domestic statistics, prostatitis is the highest with between twenty and fifty people's prevalence, and the number of going to a doctor because of prostatitis in policlinic accounts for prescription on individual diagnosis patient's male 25%～30%.Nervous and busy city male more should guard against prostatitis, bring inconvenience with exempt from customs examination work, life, study.Long-term clinical practice proves that the prostatitic curative effect of Chinese medicine is definite.Wherein commercially available ANLIETONG PIAN has clearing away heat-damp and promoting diuresis, and blood circulation promoting and blood stasis dispelling is used for syndrome of stagnant dampness-heat, and disease is seen: frequent micturition, and urgent micturition, it is not smooth to urinate, lower abdominal distention pain etc.But this tablet is through extrusion modling, and disintegrate is slow, and drug effect speed is slower; So there is researcher that it should be capsule, as number of patent application is that " 200410023397.2 ", name are called " prostatitis-treating capsule and preparation method thereof ", and number of patent application is that " 200410000135.4 ", name are called the application of " a kind of pure oral preparation of Chinese traditional medicinal for the treatment of prostatosis and preparation method thereof "; But we find in the process of studying: the former has ignored this product is the very strong characteristics of the water extracted immersing paste, hygroscopicity, does not have rational technology and strict quality method, causes the easy moisture absorption bonding of product, the quality instability; Though the latter extracts the medicine that contains volatile oil, directly sprays into, cause volatile oil to be easy to loss, and big production can only obtain Aromatic water, and not only extraction ratio is low to that is to say our volatile oil, and loss is serious, increase cost, do not increased curative effect; In view of such circumstances, in order to improve stability of drug, need to seek a kind of therapeutic effect ideal, reliable in quality, dosage form reasonably effectively the medicine preparation overcome problem that prior art exists, enrich the dosage form kind, satisfy the needs in market.And, make said preparation reach satisfactory effect, and can standard production management, and it is done further research and more new development, at first said preparation will have the quality of stable and controllable; And the method for quality control of existing QIANLIE ANTONG preparation is comparatively rough, is difficult to reach modern medicines requirement stable and controllable for quality; Therefore, the new method that needs the control of the research QIANLIE ANTONG quality of the pharmaceutical preparations.
Summary of the invention: the objective of the invention is to: prostatitic medicinal preparation of QIANLIE ANTONG of a kind of treatment and preparation method thereof and method of quality control are provided; Comprise capsule, drop pill and their preparation method and method of quality control with characteristics such as covering bitterness, easy to carry, good mouthfeel, absorption are fast, steady quality.
The present invention constitutes like this: treat prostatitic pharmaceutical preparation, it is made into effervescent tablet, injection, powder pin, freeze-dried powder, gel, dispersible tablet, capsule, soft capsule, microcapsule, granule, pill, micropill, powder, drop pill, slow releasing preparation, controlled release preparation, gel, oral liquid, soft extract, extractum and membrane by Cortex Phellodendri 200g, Radix Paeoniae Rubra 200g, Radix Salviae Miltiorrhizae 100g, Semen Persicae 140g, Herba Lycopi 120g, Radix Linderae 120g, Semen Vaccariae 80g and Radix Angelicae Dahuricae 80g or with their extract of corresponding weight portion.
Concrete preparation is capsule or drop pill.
The preparation method for the treatment of prostatitic pharmaceutical preparation is: get Cortex Phellodendri, the fine powder that was ground into 80 mesh sieves is standby; When Radix Paeoniae Rubra, Radix Salviae Miltiorrhizae, Herba Lycopi, the Radix Linderae, Semen Vaccariae and the Radix Angelicae Dahuricae add 8 times of water and are heated to 80 ℃, add Semen Persicae again, continue heating, decoct three times, 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time, collecting decoction, filter, relative density was 1.05～1.10 thick paste when filtrate was condensed into 60 ℃, added the Cortex Phellodendri fine powder, made different preparations then respectively.
Capsule in the preparation prepares like this: get Cortex Phellodendri, the fine powder that was ground into 80 mesh sieves is standby; When Radix Paeoniae Rubra, Radix Salviae Miltiorrhizae, Herba Lycopi, the Radix Linderae, Semen Vaccariae and the Radix Angelicae Dahuricae add 8 times of water and be heated to 80 ℃, add Semen Persicae again, continue heating, decoct three times, 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time, collecting decoction filtered, relative density was 1.05～1.10 thick paste when filtrate was condensed into 60 ℃, and drying under reduced pressure is ground into fine powder, add Cortex Phellodendri fine powder and starch, Pulvis Talci, amount of talc is 5%, mixing, incapsulate, should control relative humidity during packing below 65.0%, promptly.
Drop pill in the preparation prepares like this: get Cortex Phellodendri, the fine powder that was ground into 80 mesh sieves is standby; Radix Paeoniae Rubra, Radix Salviae Miltiorrhizae, the Herba Lycopi, the Radix Linderae, when the Semen Vaccariae and the Radix Angelicae Dahuricae add 8 times of water and are heated to 80 ℃, add Semen Persicae again, continue heating, decoct three times, 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time, collecting decoction, filter, relative density was 1.05～1.10 thick paste when filtrate was condensed into 60 ℃, added the Cortex Phellodendri fine powder, was substrate with the Macrogol 4000, according to medicine: the part by weight of substrate=1: 2 adds Macrogol 4000, mixing, the employing internal diameter is 3.0mm, external diameter is the dropper of 4.0mm, drips 80 ℃ of system temperature, dripping speed is 20～30d/min, dripping distance is 5cm, splash in the long cooling column of 130cm, be liquid coolant again with the methyl-silicone oil, pill, promptly.
This treats the method for quality control of prostatitic pharmaceutical preparation: this method comprises following all or part of content:
(1) one or more differential test method in berberine hydrochloride, Cortex Phellodendri, Radix Paeoniae Rubra, peoniflorin, Radix Salviae Miltiorrhizae, danshensu or its sodium salt, protocatechualdehyde, salvianolic acid B or its magnesium salt, the Radix Angelicae Dahuricae, Semen Persicae, amygdalin, Herba Lycopi, the ursolic acid;
(2) one or more content test method in berberine hydrochloride, peoniflorin, salvianolic acid B or its magnesium salt, the protocatechualdehyde;
The discrimination method of preparation comprises following all or part of content:
A. one or both thin layer chromatography discrimination method in berberine hydrochloride, the Cortex Phellodendri in the preparation:
It is an amount of to get this preparation, adds diethyl ether or petroleum ether or ethyl acetate or chloroform extraction, discards extracting solution, and medicinal residues volatilize, and add 20～100% methanol or ethanol extraction again, the preparation need testing solution; Or it is an amount of to get this preparation, directly adds 20～100% methanol or ethanol extraction, the preparation need testing solution; Get the Cortex Phellodendri medical material, with reference to a kind of control medicinal material solution of making in the need testing solution preparation method; Other gets the berberine hydrochloride reference substance, adds 20～100% methanol or ethanol and makes reference substance solution; Test according to thin layer chromatography, draw one or both each 1～30 μ l in above-mentioned need testing solution, control medicinal material or the reference substance solution, put respectively on same silica gel G or silica gel H lamellae, with benzene or toluene or dimethylbenzene-ethyl acetate or Ethyl formate or sour acid butyl ester-isopropyl alcohol or n-butyl alcohol-methanol or ethanol-dense ammoniacal liquor=1～12: be developing solvent at 1～6: 0～3: 0～3: 0～1, take out, dry, put under the uviol lamp and inspect, in the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color;
B. one or both thin layer chromatography discrimination method in Radix Paeoniae Rubra, the peoniflorin in the preparation:
It is an amount of to get this preparation, adds 20～100% ethanol or methanol extraction, the preparation need testing solution; Get the Radix Paeoniae Rubra medical material, shine medical material solution in pairs with legal system; Other gets the peoniflorin reference substance, adds 20～100% ethanol or methanol and makes reference substance solution; According to the thin layer chromatography test, draw one or both each 1～30 μ l in above-mentioned need testing solution, control medicinal material or the reference substance solution, put respectively in same silica gel G or silica gel H or silica gel G F
254On the lamellae, with chloroform or dichloromethane-ethyl acetate or Ethyl formate or sour acid butyl ester-methanol or ethanol-formic acid or acetic acid=10～40: be developing solvent at 1～5: 2～12: 0～2, launches, take out, dry, spray is with vanillin sulphuric acid or ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color;
C. one or more thin layer chromatography discrimination method in Radix Salviae Miltiorrhizae, danshensu or its sodium salt, the protocatechualdehyde in the preparation:
It is an amount of to get this preparation, extracting in water, and extracting solution is regulated pH1～4 with acid solution, and with ethyl acetate or chloroform extraction, extracting solution evaporate to dryness, residue add methanol or ethanol makes dissolving, as need testing solution; Or it is an amount of to get this preparation, adds 20～100% ethanol or methanol extraction, the preparation need testing solution; Get the Radix Salviae Miltiorrhizae control medicinal material,, make control medicinal material solution with reference to one of need testing solution preparation method; Get danshensu or its sodium salt, protocatechualdehyde, add 20～100% methanol or ethanol and make reference substance solution; According to the thin layer chromatography test, draw one or more each 1～30 μ l in above-mentioned need testing solution, control medicinal material or the reference substance solution, put respectively in same silica gel G or silica gel H or silica gel G F
254On the lamellae, with chloroform or dichloromethane or benzene or ethyl acetate-acetone or butanone or ethyl acetate-formic acid or acetic acid=5～25: be developing solvent at 1～10: 0～4, launch, take out, dry, spray is inspected under the visible light with the mixed solution of liquor ferri trichloridi or the ferric chloride and the potassium ferricyanide, or with the ammonia steam smoked after, under uviol lamp, inspect; In the test sample chromatograph, with control medicinal material chromatograph, the corresponding position of reference substance chromatograph on, show the speckle of same color;
D. one or more thin layer chromatography discrimination method in Radix Salviae Miltiorrhizae, salvianolic acid B or its magnesium salt in the preparation:
It is an amount of to get this preparation, extracts the preparation need testing solution with 10～100% methanol or ethanol jolting; Other gets the Radix Salviae Miltiorrhizae control medicinal material, shines medical material solution in pairs with legal system; Salvianolic acid B or its magnesium salt are made reference substance solution; According to the thin layer chromatography test, draw one or both each 1～30 μ l in above-mentioned need testing solution, control medicinal material or the reference substance solution, put respectively in same silica gel G or silica gel H or silica gel G F
254On the lamellae, with toluene or benzene or dimethylbenzene-chloroform or dichloromethane-ethyl acetate or Ethyl formate or sour acid butyl ester-methanol or ethanol-formic acid or acetic acid=0.2～2: be developing solvent at 0.5～3: 0.5～4: 0～1: 0～2, launch, take out, dry, inspect under the uviol lamp, or spray is with ethanol solution of sulfuric acid, heating is inspected under the visible light; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color;
E. the thin layer chromatography discrimination method of the Radix Angelicae Dahuricae in the preparation:
It is an amount of to get this preparation, extracting in water, and extracting solution concentrates with chloroform or ethyl acetate extraction, extracting solution, as need testing solution; Or it is an amount of to get this preparation, extracts the preparation need testing solution with chloroform or ethyl acetate jolting; Other gets Radix Angelicae Dahuricae control medicinal material, with reference to one of need testing solution preparation method, makes control medicinal material solution; Test according to thin layer chromatography, draw each 1～30 μ l of above-mentioned two kinds of solution, put respectively on same silica gel G or silica gel H lamellae, with chloroform or dichloromethane or ethyl acetate-methanol or ethanol or acetone=1～9: 0.2～3 is developing solvent, put in the vapour-saturated expansion cylinder of ammonia, launch, take out, dry, put under the ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
F. one or both thin layer chromatography discrimination method in Semen Persicae, the amygdaloside in the preparation:
It is an amount of to get this preparation, adds 20～100% methanol or ethanol extraction, again by macroporous adsorptive resins, with 0～80% ethanol elution, collects the part eluent after extracting solution is handled, and evaporate to dryness, residue add 10～100% methanol or ethanol makes dissolving, as need testing solution; Get the Semen Persicae medical material, add diethyl ether or Petroleum ether extraction, discard extracting solution, add 20～100% methanol or ethanol extraction again, preparation control medicinal material solution; Other gets the amygdaloside reference substance, adds 20～100% methanol or ethanol and makes reference substance solution; Draw one or both each 1～30 μ l in above-mentioned need testing solution, control medicinal material or the reference substance solution, put respectively on same silica gel g thin-layer plate, with chloroform or dichloromethane-ethyl acetate or Ethyl formate or sour acid butyl ester-methanol or alcohol-water=0～15: 0～40: 1～22: 1～10 lower floor's solution 0～10 ℃ of placement is developing solvent, launch, take out, spray is with phosphomolybdic acid sulfuric acid solution or ethanol solution of sulfuric acid, and it is clear to be heated to colour developing; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color;
G. one or both thin layer chromatography discrimination method in Herba Lycopi, the ursolic acid in the preparation:
It is an amount of to get this preparation, adds diethyl ether or chloroform or ethyl acetate or ethanol or methanol or acetone extraction the preparation need testing solution; Other gets Herba Lycopi's control medicinal material, shines medical material solution in pairs with legal system; Get the ursolic acid reference substance again, add methanol or chloroform or ethyl acetate or ethanol and make dissolving, in contrast product solution; According to the thin layer chromatography test, draw one or both each 1～30 μ l in above-mentioned need testing solution, control medicinal material or the reference substance solution, put respectively in same silica gel G or silica gel H or silica gel G F
254On the lamellae, with cyclohexane extraction or normal hexane-chloroform or dichloromethane-ethyl acetate or butyl acetate or Ethyl formate-formic acid or acetic acid=0～20: be developing solvent at 1～5: 1～8: 0～1, launches, take out, dry, spray is with ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color;
H. the high performance liquid chromatography discrimination method of protocatechualdehyde in the preparation:
It is an amount of to get this preparation, extracting in water, and water liquid prepares need testing solution with ether or ethyl acetate or chloroform jolting extraction; Or it is an amount of to get this preparation, adds 10～100% methanol or ethanol extraction, the preparation need testing solution; It is an amount of to get the protocatechualdehyde reference substance, adds 20～100% methanol or ethanol and is made as reference substance solution; With octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels or dialkyl silane bonded silica gel is filler; Methanol or acetonitrile-water-acetic acid or formic acid or phosphoric acid=10～50: 30～95: 0.01～5 is mobile phase; The detection wavelength is one or several among 190～410nm; Number of theoretical plate calculates by protocatechualdehyde should be not less than 2000; Accurate respectively reference substance solution and each 1～30 μ l of need testing solution of drawing injects chromatograph of liquid, measures; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention;
I. the high performance liquid chromatography discrimination method of salvianolic acid B in the preparation:
It is an amount of to get this preparation, adds 10～100% methanol or ethanol extraction, the preparation need testing solution; It is an amount of to get the salvianolic acid B reference substance, adds 10～100% methanol or ethanol and makes reference substance solution; With octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels or dialkyl silane bonded silica gel is filler; Methanol or ethanol-acetonitrile-formic acid or acetic acid or phosphoric acid-water=10～30: 0～30: 0～5: 50～95 is mobile phase; The detection wavelength is one or several among 190～410nm; Number of theoretical plate calculates by salvianolic acid B should be not less than 2000; Accurate respectively reference substance solution and each 1～30 μ l of need testing solution of drawing injects chromatograph of liquid, measures; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention;
J. the high performance liquid chromatography discrimination method of peoniflorin in the preparation:
It is an amount of to get this preparation, adds 20～100% methanol or ethanol extraction, the preparation need testing solution; It is an amount of to get the peoniflorin reference substance, adds 20～100% methanol or ethanol and makes reference substance solution; With octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels or dialkyl silane bonded silica gel is filler; Methanol or acetonitrile-water-potassium dihydrogen phosphate or potassium dihydrogen phosphate or phosphoric acid or formic acid or acetic acid=5～50: 20～60: 0～5 is mobile phase; The detection wavelength is one or several among 190～410nm; Number of theoretical plate calculates by peoniflorin should be not less than 3000; Accurate respectively reference substance solution and each 1～30 μ l of need testing solution of drawing injects chromatograph of liquid, measures; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention;
K. the high performance liquid chromatography discrimination method of berberine hydrochloride in the preparation:
This preparation is an amount of before getting, and adds hydrochloric acid-methanol or ethanol=0～5: 100 solution extracts, the preparation need testing solution; Get the berberine hydrochloride reference substance, add above-mentioned solvent and make reference substance solution; With octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels or dialkyl silane bonded silica gel is filler; With water-potassium dihydrogen phosphate or potassium dihydrogen phosphate or phosphoric acid or formic acid or acetic acid-acetonitrile or methanol=0～60: be mobile phase at 0～5: 5～50; The detection wavelength is one or several among 190～410nm; Number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 2000; Accurate respectively reference substance solution and each 1～30 μ l of need testing solution of drawing injects chromatograph of liquid, measures; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention.
Specifically: the discrimination method of preparation comprises following all or part of content:
A. one or both thin layer chromatography discrimination method in berberine hydrochloride, the Cortex Phellodendri in the preparation:
It is an amount of to get this preparation, the 20ml that adds diethyl ether, and supersound process 20 minutes discards ether solution, and medicinal residues volatilize, and add methanol 20ml, and supersound process 20 minutes filters, and filtrate is concentrated into 2ml, as need testing solution; Get the Cortex Phellodendri medical material, shine medical material solution in pairs with legal system; Other gets the berberine hydrochloride reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw one or both each the 5 μ l in above-mentioned need testing solution, reference substance or the control medicinal material solution, put respectively on same silica gel g thin-layer plate, with benzene-ethyl acetate-methanol-isopropyl alcohol-strong ammonia solution=4: 3: 2: be developing solvent at 1.5: 0.5, launches, take out, dry, put under the uviol lamp 365nm and inspect, in the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color;
B. one or both thin layer chromatography discrimination method in Radix Paeoniae Rubra, the peoniflorin in the preparation:
It is an amount of to get this preparation, gets content, adds ethanol 25ml, and supersound process 20 minutes filters, and filtrate evaporate to dryness, residue add ethanol 2ml makes dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin layer chromatography, draw one or both each the 5 μ l in above-mentioned need testing solution, reference substance or the control medicinal material solution, respectively with same silica gel g thin-layer plate on, with chloroform-ethyl acetate-methanol-formic acid=40: 5: 12: 0.2 was developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, 105 ℃ dry by the fire to the speckle colour developing clear; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color;
C. one or more thin layer chromatography discrimination method in Radix Salviae Miltiorrhizae, danshensu or its sodium salt, the protocatechualdehyde in the preparation:
It is an amount of to get this preparation, adds water 20ml, and ultrasonic 30 minutes, centrifugal, supernatant was regulated pH value to 2 with dilute hydrochloric acid, extracted with ethyl acetate 20ml jolting, and extracting solution evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Salviae Miltiorrhizae control medicinal material 0.5g, and it is an amount of to add water, decocts 30 minutes, adds water to 20ml, shines medical material solution in pairs with legal system; Get danshensu or its sodium salt, protocatechualdehyde, add methanol and make reference substance solution; Test according to thin layer chromatography, draw one or more each the 5 μ l in above-mentioned need testing solution, reference substance or the control medicinal material solution, put respectively on same silica gel g thin-layer plate, with chloroform-acetone-formic acid=25: 10: 4 was developing solvent, launch, take out, dry, spray is placed about 30 minutes to clear spot with 2% ferric chloride alcoholic solution; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color;
D. one or more thin layer chromatography discrimination method in Radix Salviae Miltiorrhizae, salvianolic acid B or its magnesium salt in the preparation:
It is an amount of to get this preparation, and 75% methanol jolting is extracted, and extracting solution concentrates, as need testing solution; Other gets the Radix Salviae Miltiorrhizae control medicinal material, shines medical material solution in pairs with legal system; Salvianolic acid B or its magnesium salt add 75% methanol and make reference substance solution; According to the thin layer chromatography test, draw one or both each the 5 μ l in above-mentioned need testing solution, reference substance or the control medicinal material solution, put in same silica gel G F respectively
254On the lamellae, with toluene-chloroform-ethyl acetate-methanol-formic acid=2: 3: 4: be developing solvent at 0.5: 2, launches, and takes out, and dries, and 254nm inspects under the uviol lamp; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color;
E. the thin layer chromatography discrimination method of the Radix Angelicae Dahuricae in the preparation:
It is an amount of to get this preparation, and content adds water 20ml, and ultrasonic 30 minutes, centrifugal, supernatant was regulated pH value to 12 with sodium hydroxide test solution, extracted with chloroform 20ml jolting, and extracting solution is concentrated into 1ml, as need testing solution; Other gets Radix Angelicae Dahuricae control medicinal material 0.5g, adds chloroform 10ml, and ultrasonic 30 minutes, filter, filtrate is concentrated into 1ml, in contrast medical material solution; According to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with chloroform-methanol=9: 1, put in the vapour-saturated expansion cylinder of ammonia, launch, taking-up is dried, and puts that 254nm inspects under the ultra-violet lamp; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
F. one or both thin layer chromatography discrimination method in Semen Persicae, the amygdaloside in the preparation:
It is an amount of to get this preparation, adds methanol 20ml supersound process 20min, filters, filtrate evaporate to dryness, residue add water 5ml slight fever makes dissolving, puts cold, by the D101 type macroporous adsorptive resins of the internal diameter 1.5cm of water 20m prewashing, long 8cm,, discard water liquid, with ammonia solution 30ml eluting, discard ammoniacal liquor, reuse water 10ml eluting, discard water liquid, continue, collect eluent with 20% ethanol 30ml eluting, evaporate to dryness, residue add methanol 1ml makes dissolving as need testing solution; Get the Semen Persicae medical material, the 20ml that adds diethyl ether refluxes, and discards ether solution, adds methanol 20ml again and refluxes, and filters, and filtrate concentrates, in contrast medical material solution; Other gets the amygdaloside reference substance, adds methanol and makes the solution that every 1ml contains 2mg, in contrast product solution; Draw one or both each the 5 μ l in above-mentioned need testing solution, reference substance or the control medicinal material solution, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-water=15: 40: 22: 10 was developing solvent at 5～10 ℃ of lower floor's solution of placing 12h, launch, take out, spray immediately with the phosphomolybdic acid sulfuric acid solution, at 105 ℃ of about 10min of baking; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color;
G. one or both thin layer chromatography discrimination method in Herba Lycopi, the ursolic acid in the preparation:
It is an amount of to get this preparation, adds acetone 30ml, and supersound process 10 minutes is put coldly, filter, and the filtrate evaporate to dryness, residue soaks with petroleum ether 10ml, and the petroleum ether that inclines, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets Herba Lycopi's control medicinal material, shines medical material solution in pairs with legal system; Get the ursolic acid reference substance again, add dehydrated alcohol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw one or both each the 5 μ l in above-mentioned need testing solution, reference substance or the control medicinal material solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with cyclohexane extraction-chloroform-ethyl acetate-formic acid=20: 5: 8: 0.1 was developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the speckle of same color;
H. the high performance liquid chromatography discrimination method of protocatechualdehyde in the preparation:
It is an amount of to get this preparation, adds water 50ml, supersound process 30 minutes, take out, put, filter to room temperature, subsequent filtrate is regulated pH value to 2 with 10% hydrochloric acid, extracts 3 times with the ether jolting, each 10ml, merge ether extracted liquid, put evaporate to dryness in the water-bath, residue adds dissolve with methanol and standardize solution, filters with microporous filter membrane, get subsequent filtrate, as need testing solution; It is an amount of to get the protocatechualdehyde reference substance, puts in the brown measuring bottle, adds methanol and makes the solution that contains 12 μ g among every 1ml, in contrast product solution; With octadecylsilane chemically bonded silica is filler; Methanol-1% glacial acetic acid aqueous solution=13: 87 is a mobile phase; The detection wavelength is 281nm; Number of theoretical plate calculates by protocatechualdehyde should be not less than 2000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention;
I. the high performance liquid chromatography discrimination method of salvianolic acid B in the preparation:
It is an amount of to get this preparation, adds the methanol supersound process 30 minutes, takes out, and puts to room temperature, filters, as need testing solution; It is an amount of to get the salvianolic acid B reference substance, adds 75% methanol and makes reference substance solution; With octadecylsilane chemically bonded silica is filler; Methanol-acetonitrile-formic acid-water=30: 10: 1: 59 is mobile phase; The detection wavelength is 286nm; Number of theoretical plate calculates by salvianolic acid B should be not less than 2000; Draw each 10 μ l of reference substance solution and need testing solution respectively, inject chromatograph of liquid, measure; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention;
J. the high performance liquid chromatography discrimination method of peoniflorin in the preparation:
It is an amount of to get this preparation, adds the methanol supersound process 30 minutes, takes out, and puts to room temperature, filters, as need testing solution; It is an amount of to get the peoniflorin reference substance that is dried to constant weight, adds methanol and makes reference substance solution; With octadecylsilane chemically bonded silica is filler; Methanol-0.05mol/L potassium dihydrogen phosphate=40: 65 is mobile phase; The detection wavelength is 230nm; Number of theoretical plate calculates by peoniflorin should be not less than 3000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention;
K. the high performance liquid chromatography discrimination method of berberine hydrochloride in the preparation:
It is an amount of to get this preparation, adds the mixed solution supersound process 30 minutes of hydrochloric acid-methanol=1: 100, takes out, and puts to room temperature, supplies the solvent of loss, shakes up, and filters, and gets subsequent filtrate, is need testing solution; Get the berberine hydrochloride reference substance, add above-mentioned solvent and make reference substance solution; Regulating the 0.05mol/L sodium dihydrogen phosphate-acetonitrile of pH value to 3.0=75: 25 with phosphoric acid is mobile phase; The detection wavelength is 270nm; Number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 2000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention.
The content assaying method of this preparation comprises following all or part of content:
A. the high-efficient liquid phase chromatogram process measuring method of preparation Central Plains catechu aldehyde:
It is an amount of to get this preparation, and accurate the title decides, extracting in water, and water liquid prepares need testing solution with ether or ethyl acetate or chloroform jolting extraction; Or it is an amount of to get this preparation, adds 10～100% methanol or ethanol extraction, the preparation need testing solution; It is an amount of to get the protocatechualdehyde reference substance, adds 10～100% methanol or ethanol and is made as reference substance solution; With octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels or dialkyl silane bonded silica gel is filler; Methanol or acetonitrile-water-acetic acid or formic acid or phosphoric acid=10～50: 30～95: 0.01～5 is mobile phase; The detection wavelength is one or several among 190～410nm; Number of theoretical plate calculates by protocatechualdehyde should be not less than 2000; Accurate respectively reference substance solution and each 1～30 μ l of need testing solution of drawing injects chromatograph of liquid, measures, and calculates with one point external standard method or standard curve method; Content limit should be: must not be lower than 108 μ g with containing Radix Salviae Miltiorrhizae in this preparation in protocatechualdehyde on 1st;
B. the high-efficient liquid phase chromatogram process measuring method of content of danshinolic acid B in the preparation:
It is an amount of to get this preparation, and accurate the title decides, and adds 10～100% methanol or ethanol extraction, the preparation need testing solution; It is an amount of to get the salvianolic acid B reference substance, adds 10～100% methanol or ethanol and makes reference substance solution; With octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels or dialkyl silane bonded silica gel is filler; Methanol or ethanol-acetonitrile-formic acid or acetic acid or phosphoric acid-water=10～30: 0～30: 0～5: 50～95 is mobile phase; The detection wavelength is one or several among 190～410nm; Number of theoretical plate calculates by salvianolic acid B should be not less than 2000; Accurate respectively reference substance solution and each 1～30 μ l of need testing solution of drawing injects chromatograph of liquid, measures, and calculates with one point external standard method or standard curve method; Content limit should be: must not be lower than 10.8mg with containing Radix Salviae Miltiorrhizae in this preparation in salvianolic acid B on 1st;
C. the high-efficient liquid phase chromatogram process measuring method of paeoniflorin content in the preparation:
It is an amount of to get this preparation, and accurate the title decides, and adds 10～100% methanol or ethanol extraction, the preparation need testing solution; It is an amount of to get the peoniflorin reference substance, adds 10～100% methanol or ethanol and makes reference substance solution; With octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels or dialkyl silane bonded silica gel is filler; Methanol or acetonitrile-water-potassium dihydrogen phosphate or potassium dihydrogen phosphate or phosphoric acid or formic acid or acetic acid=5～50: 20～60: 0～5 is mobile phase; The detection wavelength is one or several among 190～410nm; Number of theoretical plate calculates by peoniflorin should be not less than 3000; Accurate respectively reference substance solution and each 1～30 μ l of need testing solution of drawing injects chromatograph of liquid, measures; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate with one point external standard method or standard curve method; Content limit should be: must not be lower than 13.2mg with containing Radix Paeoniae Rubra in this preparation in peoniflorin on 1st;
D. the high-efficient liquid phase chromatogram process measuring method of content of berberine hydrochloride in the preparation:
It is an amount of to get this preparation, and accurate the title decides, and adds hydrochloric acid-methanol=0～5: 100 solution extracts, the preparation need testing solution; Get the berberine hydrochloride reference substance, add above-mentioned solvent and make reference substance solution; With octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels or dialkyl silane bonded silica gel is filler; With water-potassium dihydrogen phosphate or potassium dihydrogen phosphate or phosphoric acid or formic acid or acetic acid-acetonitrile or methanol=20～60: be mobile phase at 0～5: 5～50; The detection wavelength is one or several among 190～410nm; Number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 2000; Accurate respectively reference substance solution and each 1～30 μ l of need testing solution of drawing injects chromatograph of liquid, measures, and calculates with one point external standard method or standard curve method; Content limit should be: must not be lower than 36mg with containing Cortex Phellodendri in this preparation in berberine hydrochloride on 1st.
Specifically, the content assaying method of this preparation comprises following all or part of content:
A. the high-efficient liquid phase chromatogram process measuring method of preparation Central Plains catechu aldehyde:
It is an amount of to get this preparation, and accurate the title decides, and puts in the tool plug conical flask, precision adds water 50ml, and weight, supersound process 30 minutes decided in accurate title, take out, put to room temperature, weight decided in accurate title, add water and supply the weight that subtracts mistake, shake up, filter, the accurate subsequent filtrate 10ml that draws, regulate pH value to 2 with 10% hydrochloric acid, extract 3 times, each 10ml with the ether jolting, merge ether extracted liquid, put evaporate to dryness in the water-bath, residue adds dissolve with methanol and quantitatively is transferred in the 10ml measuring bottle, adds methanol to scale, shake up, filter with microporous filter membrane, get subsequent filtrate, as need testing solution; It is an amount of to get the protocatechualdehyde reference substance, and accurate the title decides, and puts in the brown measuring bottle, adds methanol and makes the solution that contains 12 μ g among every 1ml, in contrast product solution; With octadecylsilane chemically bonded silica is filler; Methanol-1% glacial acetic acid aqueous solution=13: 87 is a mobile phase; The detection wavelength is 281nm; Number of theoretical plate calculates by protocatechualdehyde should be not less than 2000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate with one point external standard method, promptly; Content limit should be: must not be lower than 216 μ g with containing Radix Salviae Miltiorrhizae in this preparation in protocatechualdehyde on 1st;
B. the high-efficient liquid phase chromatogram process measuring method of content of danshinolic acid B in the preparation:
It is an amount of to get this preparation, and accurate the title decides, and adds the methanol supersound process 30 minutes, takes out, and puts to room temperature, and accurate the title decided weight, adds methanol and supplies the weight that subtracts mistake, shakes up, and filters, as need testing solution; It is an amount of to get the salvianolic acid B reference substance, and accurate the title decides, and adds 75% methanol and makes reference substance solution; With octadecylsilane chemically bonded silica is filler; Methanol-acetonitrile-formic acid-water=30: 10: 1: 59 is mobile phase; The detection wavelength is 286nm; Number of theoretical plate calculates by salvianolic acid B should be not less than 2000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate with one point external standard method, promptly; Content limit should be: must not be lower than 21.6mg with containing Radix Salviae Miltiorrhizae in this preparation in salvianolic acid B on 1st;
C. the high-efficient liquid phase chromatogram process measuring method of paeoniflorin content in the preparation:
It is an amount of to get this preparation, and accurate the title decides, and adds the methanol supersound process 30 minutes, takes out, and puts to room temperature, and accurate the title decided weight, adds methanol and supplies the weight that subtracts mistake, shakes up, and filters, as need testing solution; It is an amount of to get the peoniflorin reference substance that is dried to constant weight, and accurate the title decides, and adds methanol and makes reference substance solution; With octadecylsilane chemically bonded silica is filler; Methanol-0.05mol/L potassium dihydrogen phosphate=40: 65 is mobile phase; The detection wavelength is 230nm; Number of theoretical plate calculates by peoniflorin should be not less than 3000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate with one point external standard method, promptly; Content limit should be: must not be lower than 26.4mg with containing Radix Paeoniae Rubra in this preparation in peoniflorin on 1st;
D. the high-efficient liquid phase chromatogram process measuring method of content of berberine hydrochloride in the preparation:
It is an amount of to get this preparation, accurate claims surely, adds the mixed solution supersound process 30 minutes of hydrochloric acid-methanol=1: 100, takes out, and puts to room temperature, supplies the solvent of loss, shakes up, and filters, and gets subsequent filtrate, is need testing solution; Get the berberine hydrochloride reference substance, add above-mentioned solvent and make reference substance solution; Regulating the 0.05mol/L sodium dihydrogen phosphate-acetonitrile of pH value to 3.0=75: 25 with phosphoric acid is mobile phase; The detection wavelength is 270nm; Number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 2000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate with one point external standard method, promptly; Content limit should be: must not be lower than 72mg with containing Cortex Phellodendri in this preparation with berberine hydrochloride on 1st.
Compared with prior art, product provided by the invention has clearing away heat-damp and promoting diuresis, and the effect of blood circulation promoting and blood stasis dispelling is used for syndrome of stagnant dampness-heat, and disease is seen: frequent micturition, and urgent micturition, it is not smooth to urinate, and lower abdominal distention pains etc. have reasonable therapeutic effect for acute and chronic prostatitis; That the preparation of preparation has is easy to carry, cover bitterness, characteristics such as absorbing soon can be good, good anti-moisture ability, and preparation method is rationally feasible, and production cost is suitable, and economic benefit is more satisfactory; Method of quality control can guarantee the quality and the curative effect of product; Overcome the problem that prior art, product exist; Reached the purpose of invention.
The applicant under study for action with amount of water as factor, the varying level of high spot reviews factor is taken all factors into consideration in conjunction with aspects such as production cost, the energy decocting the influence of extraction effect.For the moulding process of capsule, the relative humidity that the applicant should control during to its adjuvant, packing is investigated.For drop pill, coating can increase moisture resistance, but also can influence disintegration rate, so the selection of coating material is just very crucial.The coating adjuvant of the most suitable this product and consumption, ratio, process conditions etc. have been found by experiment; Guarantee its science, reasonable, feasible; The preparation that obtains has superperformance and therapeutic effect.
Experimental example 1: Study on extraction
1.1 volatile oil extracts experiment
(1) androlin is caused the outgrowth influence of rat prostate
50 of Wistar rats, male, be divided into five groups at random by body weight: normal control group, model control group, estradiol matched group, drug extract group (not extracting volatile oil), drug extract group (extraction volatile oil).Rat excision bilateral testes begins the subcutaneous injection androlin after 1 week of recuperating, and begins administration simultaneously, continuous 1 month.The last administration was put to death animal after 24 hours, separate to take out prostate, weighed and carried out between each group relatively.The result shows: the model group prostate is heavy apparently higher than the normal control group, and estradiol matched group prostate is heavy significantly to be reduced with model control group.Drug extract group (not extracting volatile oil) does not have marked difference with drug extract group (extraction volatile oil) effect.
(2) xylol causes the influence of mice ear
Get body weight 18-22g mice, irritate stomach and give pharmaceutical composition of the present invention, every day 1 time, continuous 7 days, be coated with dimethylbenzene 0.1ml in the Mus auris dextra back of the body in 30 minutes after the last administration, mice is put to death in the cervical vertebra dislocation after 2 hours, lays round auricle with card punch in left and right sides ear same area, weighs, ratio with interaural difference and left ear is the swelling degree, compare each group difference, the result shows: drug extract group (not extracting volatile oil) does not have marked difference with drug extract group (extraction volatile oil) effect, sees the following form.
| Group | Number of animals | Contrast | Cause scorching ear weight (%) |
| Matched group | 10 | 100.0 | 189.6±39.7 |
| Aspirin | 10 | 100.0 | 132.9±28.5 |
| Drug extract group (extraction volatile oil) | 10 | 100.0 | 121.1±31.6 |
| Drug extract group (not extracting volatile oil) | 10 | 100.0 | 120.8±12.5 |
1.2 decocting process research
(1) factor is selected: the decocting for Chinese herbal medicine extraction effect is subjected to the influence of factors such as amount of water, extraction time, extraction time.Prior art is investigated extraction time, extraction time, so when Radix Paeoniae Rubra, Radix Salviae Miltiorrhizae, Herba Lycopi, the Radix Linderae, Semen Vaccariae, the Radix Angelicae Dahuricae and Semen Persicae medical material decoct investigation, choose amount of water as factor, the varying level of high spot reviews factor is to decocting the influence of extraction effect.Take all factors into consideration the selection factor level in conjunction with aspects such as production cost, the energy.
(2) index is determined: select extractum recovery rate and protocatechualdehyde content as evaluation index, its reason and assay method are as follows:
1. extractum recovery rate: extractum is the material base of solid preparation performance curative effect, and its yield height directly influence preparation process, is reasonable, effective control device so be chosen as the extraction index.
2. assay: extractum recovery rate height can not reflect fully that active ingredient extracts situation, so measure the contained protocatechualdehyde content of Radix Salviae Miltiorrhizae simultaneously as the decoction screening index.With reference to relevant document, adopt high-efficient liquid phase technique to measure the content of protocatechualdehyde.
Test method: take by weighing Radix Paeoniae Rubra 200g, Radix Salviae Miltiorrhizae 100g, Herba Lycopi 120g, Radix Linderae 120g, when the Semen Vaccariae 80g and the Radix Angelicae Dahuricae 80 add water and are heated to 80 ℃, add Semen Persicae 140 again, continue heating, decoct three times, 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time, collecting decoction filtered, filtrate concentrating adjusted and is settled to 1000ml, precision is measured 50ml, puts in the evaporating dish that is dried to constant weight, behind evaporate to dryness in the water-bath, in 105 ℃ of dryings 3 hours, move in the exsiccator, cooled off 30 minutes, weight decided in accurate rapidly title, calculate paste-forming rate, measure protocatechualdehyde content simultaneously.
(3) test: test arrangement and the results are shown in following table.
Amount of water is investigated table as a result
| Tested number | Amount of water (doubly) | Extractum recovery rate (%) | Protocatechualdehyde content (mg/g) | ||
| For the first time | For the second time | For the third time | |||
| 1 | 6 | 6 | 6 | 9.67 | 0.25 |
| 2 | 8 | 8 | 8 | 12.71 | 0.23 |
| 3 | 10 | 10 | 10 | 13.65 | 0.20 |
As seen from the above table, it is that 10,10,10 times extractum recovery rate difference is little with amount of water that amount of water is 8,8,8 times, but being 8,8,8 times from protocatechualdehyde content amount of water, to be better than amount of water be 10 times of amounts, therefore considered with becoming originally from energy savings, the optimised process of amount of water is for decocting with water three times, and amount of water is 8,8,8 times.And carry out confirmatory experiment according to this condition.
Table is as a result investigated in the amount of water checking
| Tested number | Amount of water (doubly) | Extractum recovery rate (%) | Protocatechualdehyde content (mg/g) | ||
| For the first time | For the second time | For the third time | |||
| 1 | 8 | 8 | 8 | 13.47 | 0.22 |
| 2 | 8 | 8 | 8 | 12.58 | 0.22 |
| 3 | 8 | 8 | 8 | 12.75 | 0.23 |
As seen from the above table, extractum recovery rate and protocatechualdehyde content difference of each group are little, and the condition that screening be described is stablized feasible, so the optimised process of definite amount of water adds 8 times of amounts for decocting with water three times at every turn.And carry out confirmatory experiment according to this condition.
In sum, the optimum extraction process of Radix Paeoniae Rubra, Radix Salviae Miltiorrhizae, Herba Lycopi, the Radix Linderae, Semen Vaccariae, the Radix Angelicae Dahuricae and Semen Persicae is that Radix Paeoniae Rubra, Radix Salviae Miltiorrhizae, Herba Lycopi, the Radix Linderae, Semen Vaccariae and the Radix Angelicae Dahuricae are when adding 8 times of water and being heated to 80 ℃, add Semen Persicae again, continue heating, decoct three times, 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time.
Experimental example 2 capsule Study on Forming
2.1 hygroscopicity is investigated
Cortex Phellodendri powder is broken into fine powder in the prior art, and we carry out hygroscopicity investigation test to the mixed material that extraction ointment, ointment add behind the Cortex Phellodendri medicated powder, the results are shown in following table.
The wettability test result
| Sample | Pure extract powder | Extract powder+crude drug powder | |
| The weighing bottle numbering | 1 | 2 | |
| Weight of material (g) | 0.99 | 1.01 | |
| Moisture absorption blanking time percentage (%) | 1h | 1.50 | 0.72 |
| 2h | 4.11 | 1.83 | |
| 3h | 5.78 | 3.56 | |
| 4h | 8.12 | 5.05 | |
| 6h | 9.71 | 6.26 | |
| 8h | 11.58 | 8.15 | |
| 10h | 13.05 | 10.02 | |
| 12h | 16.27 | 12.13 | |
| 24h | 18.45 | 14.32 | |
| 36h | 21.96 | 16.24 | |
| 48h | 26.18 | 18.96 | |
| 72h | 29.44 | 21.63 | |
| 84h | 31.60 | 22.24 | |
Investigate by wettability test, think that the extractum that adds the crude drug powder has anti-preferably hygroscopic effect.
2.2 diluent is selected
The material properties of considering extraction is basic identical, so we select for use starch to adjust prescription weight as diluent.
2.3 mobile the investigation
For guaranteeing that divided dose is accurate, require the good flowability of fill material tool, so to measure the flowability of method examination angle of repose mixed material.
Fixed funnel method: get 3 funnel series connection, lowermost end is apart from horizontal positioned graph paper 1.5cm place, carefully fill material is poured into along hopper walls in the funnel of going up most till the granule cone tip that bottom funnel forms touches the funnel end opening, measure the diameter of conical base by graph paper, (tg α=H/R/2), result of calculation sees the following form to calculate angle of repose.
α angle of repose of fill material
| Working sample | Angle of repose |
| 1 | 53.5° |
| 2 | 52.3° |
| 3 | 54.8° |
As seen from the above table, mixed material angle of repose＞40 ° show that promptly the mixed material property that flows is bad, can not satisfy the branch reload request.
2.4 fluidizer is investigated
From top angle of repose measurement result as can be seen, mixed material mobile relatively poor, divided dose is accurate when guaranteeing that capsule is loaded, and needs to increase the flowability of fill material, we screen fluidizer for this reason.Owing to used starch as diluent in the mixed material, still no longer consider to add again its consumption; Pulvis Talci can increase lubricity and flowability, and possess hydrophilic property, can not influence capsular disintegrate, thus we to adopt Pulvis Talci be fluidizer, and its consumption is investigated, result of the test sees the following form.
The amount of talc investigation table
| Sequence number | Amount of talc (%) | Angle of repose (°) |
| 1 | 2 | 43.6 |
| 2 | 5 | 32.7 |
| 3 | 8 | 31.8 |
From top result as can be seen, consumption was at 2% o'clock, improve to some extent the angle of repose to mixed material, but can't meet the demands, consumption is 5% and can reaches requirement at 8% o'clock, but amount of talc is 8% o'clock, and angle of repose, decline scope was not clearly, so we determine that amount of talc is 5%.
2.5 the fill material bulk density is measured and capsulae vacuus is selected
Generally according to the difference of crystal formation, fineness, density and the dosage of medicine, particularly bulk density is determined in the selection of capsulae vacuus specification.Adopt the graduated cylinder method to measure the mixed material bulk density, the mixture that is about to precision weighing is packed in the exsiccant 10ml graduated cylinder, about jolting gently, 20 times back and forth, recording capacity calculates, and the results are shown in following table.
The bulk density measurement result
| Batch | Weight (g) | Capacity (ml) | Bulk density (g/ml) | Meansigma methods |
| 1 | 2.03 | 3.5 | 0.58 | 0.59 |
| 2 | 2.83 | 4.8 | 0.59 | |
| 3 | 2.52 | 4.2 | 0.60 |
The result records the about 0.60 (g/cm of filler particles bulk density
3), according to the relation of capsulae vacuus number and approx. volume, select the packing of No. 0 hungry area softgel shell, promptly every capsules loading amount is about 0.45g (being equivalent to 1.04g crude drug/grain).
2.6 critical relative humidity (CRH) is measured
Material can be loaded smoothly in order to guarantee to produce, and the humidity that need control environment so that make material have good mobility, makes loading amount even, and we carry out equilibrium hygroscopicity test, i.e. moisture equilibrium at dry side curve determination to mixed material for this reason.Get totally six parts of the about 1g of mixed material, put in the weighing botle, the accurate title, decide, the weighing bottle cap is opened, put into relative humidity respectively and be 20%, 33%, 43%, 60%, 75%, 92% environment, in 25 ℃ of constant incubators, placed 84 hours, take out weighing botle, it is fixed to add a cover the accurate title in back, calculating the moisture absorption percentage rate, is abscissa with the relative humidity, and the moisture absorption percentage rate is a vertical coordinate, draw the moisture equilibrium at dry side curve and see accompanying drawing 1, result of the test sees the following form.
The moisture absorption percentage rate (%) of filler particles
| The saturated salt solution kind | Relative humidity (%) | Moisture absorption percentage rate (%) |
| CH 3COOK·1.5H 2O | 20 | 3.11 |
| MgCl 2·6H 2O | 33 | 4.62 |
| K 2CO 3·2H 2O | 43 | 7.24 |
| NaBr·2H 2O | 60 | 13.20 |
| NaCl | 75 | 22.22 |
| KNO 3 | 92 | 42.97 |
As can be known from the above table, capsule is under different relative humidity environment, and its water absorption does not wait, and is about 65.0% when following at relative humidity, and hygroscopicity is less, so should control relative humidity below 65.0% during packing.
Experimental example 3 drop pill Study on Forming
3.1 substrate screening
According to bibliographical information, drop pill substrate commonly used has Macrogol 4000 and polyethylene glycol 6000, thus our decision also to adopt Polyethylene Glycol be substrate, and the two is compared test.The Polyethylene Glycol of different model is put in the small beaker, be heated to 80-90 ℃, after treating whole fusions, add extract powder, investigate substrate and extract powder the fusion situation, select fusion situation dripping system (the system condition: expect warm 80 ℃ of writing out a prescription preferably, coolant is a dimethicone, drip apart from 6cm, drip 30～40 droplets/minute of speed), the results are shown in following table.
The fusion situation of substrate and principal agent relatively
| The prescription number | Prescription 1 | Prescription 2 | Prescription 3 | Prescription 5 | Prescription 6 | Prescription 7 |
| Extract powder (g) | 10 | 10 | 10 | 10 | 10 | 10 |
| Macrogol 4000 (g) | 10 | 15 | 20 | ------ | ------ | ------ |
| Polyethylene glycol 6000 (g) | ------ | ------ | ------ | 10 | 15 | 20 |
| Principal agent: substrate | 1∶1 | 1∶1.5 | 1∶2 | 1∶1 | 1∶1.5 | 1∶2 |
| The fusion situation of principal agent and substrate | Principal agent can merge with substrate, but system does not have flowability | Principal agent can merge with substrate, and the system flowability is fine | Principal agent can merge with substrate, and the system flowability is fine | Principal agent and substrate merge relatively poor | Principal agent can merge with substrate, but system does not have flowability | Principal agent can merge with substrate, and system flows better |
| The drop pill outward appearance | ------ | Smooth, roundness is good | Smooth, roundness is good | ------ | Roundness is poor, serious hangover | Roundness is poor, hangover |
| Drop pill hardness | ------ | Hardness is better | Hardness is better | ------ | Hardness is better | Hardness is better |
| The ball method of double differences is different | 4.3％ | 6.8％ | ------ | 11％ | ||
| Dissolve scattered time limit (min) | ------ | 6～8 | 7～9 | ------ | ------ | 12～18 |
The above results shows, the good fluidity of the 2 fusion medicinal liquids of writing out a prescription, and the drop pill good moldability, smooth, mellow and full, the ball method of double differences is different little, and molten loosing comparatively fast is so select No. 2 prescriptions to be optimal condition.
3.2 coolant is selected
The get it filled extract powder 10g of material, Macrogol 4000 15g, mix homogeneously is heated to 80-90 ℃, treat whole fusions after, get in right amount, splash into respectively in simethicone and the liquid paraffin coolant, be index with the molding situation of drop pill, the results are shown in following table.
Coolant is selected
| The cold agent kind of getting | Coolant temperature | Drip distance | Drip speed | The material temperature | Drop pill molding situation |
| Dimethicone | 10℃ | 5cm | 30～40d/min | 80℃ | Roundness is good, forming |
| Liquid paraffin | 10℃ | 5cm | 30～40d/min | 80℃ | The drop pill hangover, shape is relatively poor |
Last table shows, is that coolant drop pill roundness is good with the simethicone, forming.
3.3 coolant temperature is selected
Get the extract powder 10g of three kinds of medical materials, Macrogol 4000 15g, mix homogeneously is heated to 80-90 ℃, treat whole fusions after, get in right amount, splash into respectively in the simethicone coolant of different temperatures, observe drop pill molding situation, the results are shown in following table.
Coolant temperature is selected
| Coolant temperature | Drip distance | Drip speed | The material temperature | Drop pill molding situation |
| 10℃ | 6cm | 30～40d/min | 80℃ | Roundness is good, forming |
| 20℃ | 6cm | 30～40d/min | 80℃ | Roundness is good, forming |
| The gradient cooling | 6cm | 30～40d/min | 80℃ | Roundness is good, forming |
Annotate: the gradient cooling means is: top is 10～20 ℃, and the bottom is 5～10 ℃.
Last table shows that under above-mentioned three kinds of chilling temperatures, the mouldability of this product is all good, is easy operation, is 10～20 ℃ so select coolant temperature.
3.4 disintegration time is investigated
| Group | Disintegration time (min) | ||
| 1 | 2 | 3 | |
| Drop pill ANLIETONG PIAN of the present invention | 29.3 52.3 | 29.8 50.3 | 29.7 49.8 |
The result as can be known, technology gained preparation of the present invention has disintegrate effect preferably, is beneficial to the absorption of medicine.
Experimental example 4: to the research of prostatitis treating effect
50 of SD rats, anesthesia back routine disinfection cuts about skin 1.5cm.Isolate prostate, 40 rats are wherein caused non-bacterial chronic prostatitis animal model from 2% agar solution 0.1ml of left lobe of prostate, each injection sterilization of lobus dexter, all the other 10 rats are respectively injected sterile saline 0.1ml as the normal control group at left lobe of prostate, lobus dexter.Distinguish suture muscles, skin then, operation back 24h, with the rat random packet, 10 every group.Normal control group: distilled water 1ml/100g body weight; Model control group: distilled water 1ml/100g body weight; Commercially available ANLIETONG PIAN group, Capsules group of the present invention, Capsules group of the present invention: give the relative medicine suspension respectively, the administration volume is the 1ml/100g body weight, and drug dose is equivalent to be grown up clinical plan with 10 times of dosage.Each treated animal gastric infusion every day (or distilled water) 1 time is treated 45d continuously.24h after the last administration behind the title the weight of animals, puts to death the disconnected neck of rat, peels off prostate rapidly, after weighing, puts into the liquid-solid 48h of deciding of FAA, ethanol dehydration step by step, and dimethylbenzene is transparent, waxdip, paraffin embedding, conventional section 4 μ m, HE dyes.Quantity and morphological change situation with matter inflammatory cell and body of gland and lumen of gland between pattern analysis instrument connection computer analysis processing rat prostate.
1. to the influence of chronic prostatitis rat prostate weight coefficient due to the agar, concrete outcome sees the following form:
Influence to chronic prostatitis rat prostate weight coefficient due to the agar
| Group | n | Dosage (m/gkg -1) | Weight of prostate coefficient (m/mg100g -1) |
| Normal control group model matched group | 10 10 | - - | 138.5±26.7 228.9±36.4 |
| ANLIETONG PIAN group Capsules group of the present invention drop pill group of the present invention | 10 10 10 | 3.2 3.2 3.2 | 184.6±45.7 169.1±42.6 158.7±26.8 |
From last table as seen, use ANLIETONG PIAN, capsule of the present invention, drop pill of the present invention treatment 45d, its weight of prostate coefficient ratio model control group all reduces, and the effect of capsule of the present invention, drop pill is better than commercially available ANLIETONG PIAN.
2. to the influence of matter inflammatory cell quantity and form between prostate, concrete outcome sees the following form:
Influence to matter inflammatory cell quantity and form between prostate
| Group | Dosage (m/gkg -1) | Number of inflammatory cells (individual) | Inflammatory cell area summation (A/ μ m 2) | Area average (A/ μ m 2) |
| Normal control group model matched group ANLIETONG PIAN group Capsules group of the present invention drop pill group of the present invention | - - 3.2 3.2 3.2 | - 142.5±59.4 148.4±74.5 146.8±26.4 148.2±62.8 | - 104632.5±28214.1 55624.8±30483.4 48276.1±25631.5 45684.4±15324.6 | - 957.2±432.7 486.4±158.8 456.2±125.9 395.7±265.4 |
From last table as seen, behind application ANLIETONG PIAN, capsule of the present invention, the drop pill treatment 45d, inflammatory cell area summation, average area reduce.Inflammatory cell quantity and model control group are relatively, do not see minimizing, even slightly increase, this is owing to number of inflammatory cells in the matter between the model control group prostate is more, area is bigger, normal adhesion slabbing, and computer will connect to the reason that flaky a plurality of inflammatory cell identification is calculated as 1 inflammatory cell.
3. to the influence of prostate body of gland quantity and form
Influence to chronic prostatitis rat prostate body of gland quantity due to the agar and form
| Group | Area average (A/ μ m 2) | Girth average (A/ μ m 2) | Maximum gauge average (A/ μ m 2) | Minimum diameter average (A/ μ m 2) |
| Normal control group model matched group ANLIETONG PIAN group Capsules group of the present invention drop pill group of the present invention | 11265±4837 12572±2694 12893±3488 13254±1548 12687±2362 | 513.8±59.4 536.4±156.7 548.7±124.1 567.2±134.8 539.1±112.7 | 359.5±162.4 137.2±42.6 185.7±36.7 159.6±59.8 165.2±89.1 | 86.2±26.7 58.6±16.7 78.4±12.1 68.5±13.4 75.1±19.5 |
As seen from the above table, after using ANLIETONG PIAN, capsule of the present invention, drop pill treatment 45d, relatively each organizes the therapeutical effect that all has in various degree with model control group, body of gland area average, body of gland maximum gauge average etc. are obviously raise, and the effect of product of the present invention is better than commercially available ANLIETONG PIAN.
Experimental example 5: the research of method of quality control
5.1 the thin layer chromatography discrimination method of berberine hydrochloride, Cortex Phellodendri in the capsule
The purpose of this experiment is the feature for outstanding Cortex Phellodendri, and for getting rid of in the preparation interference with other composition like the contained constituent classes such as berberine hydrochloride of Cortex Phellodendri, the experimenter compares test respectively to sample extraction, development system, coloration method etc.; Through screening, determined the best approach and condition: it is an amount of to get the QIANLIE ANTONG preparation, the 20ml that adds diethyl ether, and supersound process 20 minutes discards ether solution, and medicinal residues volatilize, and add methanol 20ml, and supersound process 20 minutes filters, and filtrate is concentrated into 2ml, as need testing solution; Get the Cortex Phellodendri medical material, shine medical material solution in pairs with legal system; Other gets the berberine hydrochloride reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, with benzene-ethyl acetate-methanol-isopropyl alcohol-strong ammonia solution=4: 3: 2: be developing solvent at 1.5: 0.5, launches, take out, dry, put under the uviol lamp 365nm and inspect, in the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color.The expansion effect of several development systems relatively sees the following form in the experiment:
The thin layer chromatography discrimination method of berberine hydrochloride, Cortex Phellodendri in the capsule
| Developing solvent | Lamellae | Effect |
| Benzene-ethyl acetate-ethanol-formic acid (8: 6: 1: 1) | Silica gel G | Difference: sample separation is unintelligible |
| Benzene-butyl acetate-methanol (8: 4: 3) | Silica gel G | Difference: feminine gender has interference, the speckle hangover |
| Benzene-ethyl acetate-methanol-strong ammonia solution (4: 3: 3: 0.5) | Silica gel H | Preferable: it is clear that sample and reference substance all separate, negative noiseless |
| Benzene-ethyl acetate-methanol-isopropyl alcohol-strong ammonia solution (4: 3: 2: 1.5: 0.5) | Silica gel G | Best: it is clear, negative noiseless that sample and reference substance all separate |
5.2 the thin layer chromatography discrimination method of Radix Paeoniae Rubra, peoniflorin in the drop pill
The purpose of this experiment is the feature for outstanding Radix Paeoniae Rubra, and for getting rid of in the preparation interference with other composition like the contained constituent classes such as peoniflorin of Radix Paeoniae Rubra, the experimenter compares test respectively to sample extraction, development system, coloration method etc.; Through screening, determined the best approach and condition: it is an amount of to get the QIANLIE ANTONG preparation, gets content, adds ethanol 25ml, and supersound process 20 minutes filters, and filtrate evaporate to dryness, residue add ethanol 2ml makes dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 2mg, in contrast product solution; According to thin layer chromatography test, draw each 5 μ l of above-mentioned solution, respectively and on the same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-formic acid=40: 5: 12: 0.2 was developing solvent, launches, and takes out, dry, spray is with 5% vanillin sulfuric acid solution, 105 ℃ dry by the fire to speckle colour developing clear; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color;
The thin layer chromatography discrimination method of Radix Paeoniae Rubra, peoniflorin in the drop pill
| Developing solvent | Lamellae | Effect |
| Benzene-ethyl acetate-ethanol-formic acid (8: 4: 5: 1) | Silica gel G | Difference: sample separation is unintelligible |
| Ethyl acetate-methanol-formic acid (5: 12: 1) | Silica gel H | Difference: feminine gender has interference |
| Chloroform-Ethyl formate-ethanol-acetic acid (20: 5: 8: 1) | Silica gel G F 254 | Preferable: it is clear that sample and reference substance all separate, negative noiseless |
| Chloroform-ethyl acetate-methanol-formic acid (40: 5: 12: 0.2) | Silica gel G | Best: it is clear, negative noiseless that sample and reference substance all separate |
5.3 the thin layer chromatography discrimination method of Radix Salviae Miltiorrhizae, danshensu, protocatechualdehyde in the granule
The purpose of this experiment is the feature for outstanding Radix Salviae Miltiorrhizae, and for getting rid of in the preparation interference of other composition like the constituent classes such as the danshensu contained with Radix Salviae Miltiorrhizae, protocatechualdehyde, the experimenter compares test respectively to sample extraction, development system, coloration method etc.; Through screening, determined the best approach and condition: it is an amount of to get the QIANLIE ANTONG preparation, adds water 20ml, ultrasonic 30 minutes, centrifugal, supernatant is regulated pH value to 2 with dilute hydrochloric acid, extracts with ethyl acetate 20ml jolting, extracting solution evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Salviae Miltiorrhizae control medicinal material 0.5g, and it is an amount of to add water, decocts 30 minutes, adds water to 20ml, shines medical material solution in pairs with legal system; Get danshensu or its sodium salt, protocatechualdehyde, add methanol and make reference substance solution; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, with chloroform-acetone-formic acid=25: 10: 4 was developing solvent, launched, and took out, dry, spray ferric chloride alcoholic solution, place about 30 minutes to clear spot with 2%; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color;
The thin layer chromatography discrimination method of Radix Salviae Miltiorrhizae, danshensu, protocatechualdehyde in the granule
| Developing solvent | Lamellae | Effect |
| Benzene-ethyl acetate-ethanol (8: 4: 5) | Silica gel G | Difference: sample separation is unintelligible |
| Ethyl acetate-methanol-formic acid (5: 5: 1) | Silica gel G F 254 | Difference: feminine gender has interference |
| Dichloromethane-acetone-formic acid (5: 2: 4) | Silica gel H | Preferable: it is clear that sample and reference substance all separate, negative noiseless |
| Chloroform-acetone-formic acid (25: 10: 4) | Silica gel G | Best: it is clear, negative noiseless that sample and reference substance all separate |
5.4 the thin layer chromatography discrimination method of the Radix Angelicae Dahuricae in the capsule
The purpose of this experiment is the feature for the outstanding Radix Angelicae Dahuricae, and for getting rid of in the preparation interference with other composition like the contained constituent class of the Radix Angelicae Dahuricae, the experimenter compares test respectively to sample extraction, development system, coloration method etc.; Through screening, determined the best approach and condition: it is an amount of to get the QIANLIE ANTONG preparation, and content adds water 20ml, ultrasonic 30 minutes, centrifugal, supernatant was regulated pH value to 12 with sodium hydroxide test solution, extract with chloroform 20ml jolting, extracting solution is concentrated into 1ml, as need testing solution; Other gets Radix Angelicae Dahuricae control medicinal material 0.5g, adds chloroform 10ml, and ultrasonic 30 minutes, filter, filtrate is concentrated into 1ml, in contrast medical material solution; According to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with chloroform-methanol=9: 1, put in the vapour-saturated expansion cylinder of ammonia, launch, taking-up is dried, and puts that 254nm inspects under the ultra-violet lamp; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
The thin layer chromatography discrimination method of the Radix Angelicae Dahuricae in the capsule
| Developing solvent | Lamellae | Effect |
| Benzene-ethyl acetate-ethanol (8: 4: 1) | Silica gel G | Difference: sample separation is unintelligible |
| Ethyl acetate-ethanol-formic acid (5: 2: 1) | Silica gel H | Difference: feminine gender has interference |
| Chloroform-ethanol (4: 1) | Silica gel H | Preferable: it is clear that sample and reference substance all separate, negative noiseless |
| Chloroform-methanol (9: 1) | Silica gel G | Best: it is clear, negative noiseless that sample and reference substance all separate |
5.5 the high-efficient liquid phase chromatogram process measuring method of capsule Central Plains catechu aldehyde
Test is reference substance with the protocatechualdehyde, with Alltech P426 high performance liquid chromatograph, has established the best approach of the assay of protocatechualdehyde in the prostatitis-treating capsule:
It is an amount of to get the QIANLIE ANTONG preparation, and accurate the title decides, and puts in the tool plug conical flask, precision adds water 50ml, and weight, power 250W decided in accurate title, supersound process is 30 minutes under the frequency 33KHz, take out, put to room temperature, weight decided in accurate title, add water and supply the weight that subtracts mistake, shake up, filter, the accurate subsequent filtrate 10ml that draws, regulate pH value to 2 with 10% hydrochloric acid, extract 3 times, each 10ml with the ether jolting, merge ether extracted liquid, put evaporate to dryness in the water-bath, residue adds dissolve with methanol and quantitatively is transferred in the 10ml measuring bottle, adds methanol to scale, shake up, filter with microporous filter membrane, get subsequent filtrate, as need testing solution; It is an amount of to get the protocatechualdehyde reference substance, and accurate the title decides, and puts in the brown measuring bottle, adds methanol and makes the solution that contains 12 μ g among every 1ml, in contrast product solution; With octadecylsilane chemically bonded silica is filler; Methanol-1% glacial acetic acid aqueous solution=13: 87 is a mobile phase; The detection wavelength is 281nm; Number of theoretical plate calculates by protocatechualdehyde should be not less than 2000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate with one point external standard method, promptly; Content limit should be: every of this product contains protocatechualdehyde, must not be lower than 18.0 μ g.
This method has been passed through following 1～11 methodological study test respectively:
1 detects the selection of wavelength
It is an amount of that precision takes by weighing the protocatechualdehyde reference substance, adds methanol respectively and make the solution that every 1ml contains 13 μ g, respectively in the interscan of 200～400nm wave-length coverage.The result shows that protocatechualdehyde has absorption maximum at the 281nm place, therefore selects 281nm as the detection wavelength of measuring prostatitis-treating capsule Central Plains catechu aldehyde.
The selection of 2 extraction times
Get 40 of this product, get content, mixing, therefrom precision takes by weighing about 6g (totally 4 minutes), splits in the tool plug conical flask, and precision adds water 50ml, weight decided in accurate title, respectively supersound process (power 250W, frequency 33KHz) 10,20,30,40 minutes, take out, put to room temperature, weight decided in accurate title, add water and supply the weight that subtracts mistake, shake up, filter, the accurate subsequent filtrate 10ml that draws regulates pH value to 2 with 10% hydrochloric acid, extracts 3 times with the ether jolting, each 10ml merges ether extracted liquid, puts evaporate to dryness in the water-bath, residue adds dissolve with methanol and quantitatively is transferred in the 10ml measuring bottle, add methanol to scale, shake up, filter with microporous filter membrane (0.45 μ m), get subsequent filtrate, promptly.See the following form.
Extraction time
| Extraction time (min) | Protocatechualdehyde (μ g/ grain) |
| 10 | 21.47 |
| 20 | 22.46 |
| 30 | 23.69 |
| 40 | 23.72 |
The result shows that supersound process 30min can extract fully, so extraction time is decided to be 30 minutes.
3 chromatographic conditions
Chromatograph: Alltech P426;
Chromatographic column: Diamonsil (diamond) C
18(250 * 4.6mm, 5 μ m);
Mobile phase: methanol-1% glacial acetic acid aqueous solution (13: 87);
Detect wavelength: 281nm;
Column temperature: 30 ℃;
Flow velocity: 1ml/min;
Sample size: 10 μ l.
Obtain protocatechualdehyde, test sample chromatograph according to above-mentioned condition, its number of theoretical plate is pressed the protocatechualdehyde peak and is calculated greater than 2000.In the sample protocatechualdehyde chromatographic peak separate with close peak clear fully, separating degree is all greater than 1.5.
The test of 4 negative ELIMINATION OF ITS INTERFERENCE is for investigating the mensuration whether other medical material disturbs protocatechualdehyde, except that Cortex Phellodendri, takes by weighing other medical material and adjuvant is made negative control product solution and mensuration with method in the prescription ratio.The result shows that negative sample is noiseless to the assay of protocatechualdehyde.
5 reference substance purity tests provide protocatechualdehyde by Nat'l Pharmaceutical ﹠ Biological Products Control Institute, are respectively 99.1%, 99.2% through high effective liquid chromatography for measuring purity, meet assay reference substance requirement.
The investigation precision of 6 linear relationships is measured protocatechualdehyde reference substance solution 0.2ml, 0.6m, 1.0ml, 1.4ml, 1.8ml, splits in the 25ml measuring bottle, and it is fixed to scale to add methanol, shake up, the therefrom accurate respectively 10 μ l that draw inject chromatograph of liquid, according to high effective liquid chromatography for measuring.Amount with protocatechualdehyde is an abscissa, and peak area is that vertical coordinate is figure, the drawing standard curve.See the following form
The protocatechualdehyde linear relationship
| Numbering | Protocatechualdehyde amount (μ g) | Peak area |
| 1 | 0.034368 | 84202 |
| 2 | 0.103104 | 250682 |
| 3 | 0.171840 | 414574 |
| 4 | 0.240576 | 583623 |
| 5 | 0.309312 | 752806 |
Regression equation: Y=2429802.43X-359.85
Correlation coefficient: γ=0.9999
The result shows that protocatechualdehyde linear relationship within 0.034368 μ g～0.309312 μ g scope is good.
Through calculating, the protocatechualdehyde standard curve is one to cross the straight line of initial point, therefore selects one point external standard method to measure the content of protocatechualdehyde in the prostatitis-treating capsule.
The accurate protocatechualdehyde reference substance solution 10 μ l that draw of 7 precision test inject chromatograph of liquid, and replication 5 times is investigated reference substance solution precision, and measurement result sees the following form.
The precision test
| Test number (TN) | 1 | 2 | 3 | 4 | 5 | Meansigma methods | RSD(％) |
| Peak area | 305123 | 310712 | 308924 | 307201 | 302658 | 306924 | 1.03 |
The result shows that reference substance solution precision is good.
8 stability tests
8.1 the accurate protocatechualdehyde reference substance solution 10 μ l that draw of reference substance stability test inject chromatograph of liquid, measure at 0,2,6,10,24 hour sample introduction respectively, measurement result sees the following form.
Reference substance solution stability test result
| Time (h) | 0 | 2 | 6 | 10 | 24 | Meansigma methods | RSD(％) |
| Peak area | 305123 | 310712 | 308924 | 307201 | 302658 | 306924 | 1.03 |
The result shows that reference substance solution is good at 24 hours internal stabilities.
8.2 the accurate need testing solution 10 μ l that draw of need testing solution stability test inject chromatograph of liquid, measure at 0,2,6,10,24 hour sample introduction respectively, measurement result sees the following form.
Need testing solution stability test result
| Time (h) | 0 | 2 | 6 | 10 | 24 | Meansigma methods | RSD(％) |
| Content (μ g/ grain) | 24.12 | 23.85 | 23.76 | 23.91 | 23.85 | 23.90 | 0.57 |
The result shows that need testing solution is good at 24 hours internal stabilities.
9 replica tests are got this product content, and mixing is therefrom got about 6.0g, and parallel 5 parts, precision claims fixed, by operating under preparation of text need testing solution and the mensuration item.The results are shown in following table.
Replica test
| Time (h) | 0 | 2 | 6 | 10 | 24 | Meansigma methods | RSD(％) |
| Content (μ g/ grain) | 23.39 | 23.27 | 22.58 | 23.61 | 23.35 | 23.24 | 1.68 |
The result shows that repeatability is good.
The test of 10 average recoveries
Get this product content, mixing, therefrom precision takes by weighing about 3g, parallel 6 parts, splits in the tool plug conical flask; Precision takes by weighing protocatechualdehyde 15.84mg, puts in the 100ml measuring bottle, adds water and makes dissolving and fixed to scale in right amount, shake up, precision is measured 0.8ml, 1.0ml, 1.2ml each 2 parts, put altogether in the above-mentioned tool plug conical flask, precision adds water to 50ml, and weight, supersound process 30 minutes decided in accurate title, take out, put to room temperature, the accurate title, decided weight, adds water and supply the weight that subtracts mistake, shake up, filter, the accurate subsequent filtrate 10ml that draws regulates pH value to 2 with 10% hydrochloric acid, extract 3 times with the ether jolting, each 10ml merges ether extracted liquid, puts evaporate to dryness in the water-bath, residue adds dissolve with methanol and quantitatively is transferred in the 10ml measuring bottle, add methanol to scale, shake up, filter with microporous filter membrane, get subsequent filtrate, promptly.Measurement result sees the following form.
The test of protocatechualdehyde average recovery
| Numbering | Test sample weighing (g) | Pure product amount (μ g) in the test sample | Protocatechualdehyde addition (μ g) | The amount of recording (μ g) | The response rate (%) |
| 1 | 2.94873 | 156.21 | 126.72 | 277.64 | 95.83 |
| 2 | 3.12065 | 165.32 | 126.72 | 286.23 | 95.42 |
| 3 | 3.04721 | 161.43 | 158.40 | 319.24 | 99.63 |
| 4 | 3.07638 | 162.97 | 158.40 | 320.51 | 99.46 |
| 5 | 3.04296 | 161.20 | 190.08 | 347.61 | 98.06 |
| 6 | 3.12553 | 165.58 | 190.08 | 351.74 | 97.94 |
Protocatechualdehyde average recovery rate=97.72%, RSD=1.81%.
11 sample sizes are measured the preparation and the operation down of algoscopy item of pressing the text need testing solution, measure ten batch samples, the results are shown in following table.
Ten batch sample assay results
| Lot number | Protocatechualdehyde (μ g/ grain) |
| 1 | 23.12 |
| 2 | 20.97 |
| 3 | 24.56 |
| 4 | 43.87 |
| 5 | 20.64 |
| 6 | 23.12 |
| 7 | 22.48 |
| 8 | 21.79 |
| 9 | 22.03 |
| 10 | 20.58 |
Conclusion: tentative according to 10 batch sample assay results, every of this product contains protocatechualdehyde, must not be lower than 18.0 μ g.
Description of drawings: accompanying drawing 1 is a critical relative humidity curve chart of the present invention.
Concrete embodiment:
Embodiments of the invention 1: Cortex Phellodendri 200g, Radix Paeoniae Rubra 200g, Radix Salviae Miltiorrhizae 100g, Semen Persicae 140g, Herba Lycopi 120g, Radix Linderae 120g, Semen Vaccariae 80g, Radix Angelicae Dahuricae 80g
Get Cortex Phellodendri, the fine powder that was ground into 80 mesh sieves is standby; When Radix Paeoniae Rubra, Radix Salviae Miltiorrhizae, Herba Lycopi, the Radix Linderae, Semen Vaccariae and the Radix Angelicae Dahuricae add 8 times of water and are heated to 80 ℃, add Semen Persicae again, continue heating, decoct three times, 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time, collecting decoction filtered, relative density was 1.05～1.10 thick paste when filtrate was condensed into 60 ℃, drying under reduced pressure is ground into fine powder, adds Cortex Phellodendri fine powder and starch, Pulvis Talci, amount of talc is 5%, mixing incapsulates, and should control relative humidity during packing below 65.0%, promptly get capsule, this product oral, a time 4～6,3 times on the one.
Embodiments of the invention 2: Cortex Phellodendri 200g, Radix Paeoniae Rubra 200g, Radix Salviae Miltiorrhizae 100g, Semen Persicae 140g, Herba Lycopi 120g, Radix Linderae 120g, Semen Vaccariae 80g, Radix Angelicae Dahuricae 80g
Get Cortex Phellodendri, the fine powder that was ground into 80 mesh sieves is standby; Radix Paeoniae Rubra, Radix Salviae Miltiorrhizae, the Herba Lycopi, the Radix Linderae, when the Semen Vaccariae and the Radix Angelicae Dahuricae add 8 times of water and are heated to 80 ℃, add Semen Persicae again, continue heating, decoct three times, 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time, collecting decoction, filter, relative density was 1.05～1.10 thick paste when filtrate was condensed into 60 ℃, added the Cortex Phellodendri fine powder, was substrate with the Macrogol 4000, according to medicine: the part by weight of substrate=1: 2 adds Macrogol 4000, mixing, the employing internal diameter is 3.0mm, external diameter is the dropper of 4.0mm, drips 80 ℃ of system temperature, dripping speed is 20～30d/min, dripping distance is 5cm, splash in the long cooling column of 130cm, be liquid coolant again with the methyl-silicone oil, pill promptly gets drop pill.
Embodiments of the invention 3: Cortex Phellodendri 200g, Radix Paeoniae Rubra 200g, Radix Salviae Miltiorrhizae 100g, Semen Persicae 140g, Herba Lycopi 120g, Radix Linderae 120g, Semen Vaccariae 80g, Radix Angelicae Dahuricae 80g
It is standby that Cortex Phellodendri powder is broken into fine powder; When Radix Paeoniae Rubra, Radix Salviae Miltiorrhizae, Herba Lycopi, the Radix Linderae, Semen Vaccariae and the Radix Angelicae Dahuricae add water and are heated to 80 ℃, add Semen Persicae again, continue heating, decoct three times, 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time, collecting decoction, filter, filtrate is condensed into thick paste, adds distilled water, simple syrup, and mix homogeneously promptly gets oral liquid.
Embodiments of the invention 4: Cortex Phellodendri 200g, Radix Paeoniae Rubra 200g, Radix Salviae Miltiorrhizae 100g, Semen Persicae 140g, Herba Lycopi 120g, Radix Linderae 120g, Semen Vaccariae 80g, Radix Angelicae Dahuricae 80g
It is standby that Cortex Phellodendri powder is broken into fine powder; When Radix Paeoniae Rubra, Radix Salviae Miltiorrhizae, Herba Lycopi, the Radix Linderae, Semen Vaccariae and the Radix Angelicae Dahuricae add water and be heated to 80 ℃, add Semen Persicae again, continue heating, decoct three times, 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time, collecting decoction, filter, filtrate is condensed into thick paste, adds carbomer, makes gel.
Embodiments of the invention 5: Cortex Phellodendri 200g, Radix Paeoniae Rubra 200g, Radix Salviae Miltiorrhizae 100g, Semen Persicae 140g, Herba Lycopi 120g, Radix Linderae 120g, Semen Vaccariae 80g, Radix Angelicae Dahuricae 80g
It is standby that Cortex Phellodendri powder is broken into fine powder; When Radix Paeoniae Rubra, Radix Salviae Miltiorrhizae, Herba Lycopi, the Radix Linderae, Semen Vaccariae and the Radix Angelicae Dahuricae add water and be heated to 80 ℃, add Semen Persicae again, continue heating, decoct three times, 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time, collecting decoction filtered, filtrate is condensed into thick paste, and drying under reduced pressure is pulverized, add carboxymethyl starch sodium, crospolyvinylpyrrolidone, calcium hydrogen phosphate, mix homogeneously, tabletting is made dispersible tablet.
Embodiments of the invention 6: the thin layer chromatography discrimination method of Cortex Phellodendri in the tablet:
It is an amount of to get the QIANLIE ANTONG tablet, adds Petroleum ether extraction, discards extracting solution, and medicinal residues volatilize, and adds alcohol reflux again, filters, and filtrate concentrates, as need testing solution; Get the Cortex Phellodendri medical material, shine medical material solution in pairs with legal system; Test according to thin layer chromatography, draw each 30 μ l of above-mentioned solution, put respectively on same silica gel H lamellae, with benzene-ethyl acetate-methanol-isopropyl alcohol-strong ammonia solution=1: 1: 3: be developing solvent at 3: 1, takes out, and dries, put under the uviol lamp and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Embodiments of the invention 7: the thin layer chromatography discrimination method of berberine hydrochloride, Cortex Phellodendri in the granule
It is an amount of to get the QIANLIE ANTONG preparation, and the extraction that adds diethyl ether discards extracting solution, and medicinal residues volatilize, and add methanol extraction again, filters, and filtrate concentrates, as need testing solution; Get the Cortex Phellodendri medical material, shine medical material solution in pairs with legal system; Other gets the berberine hydrochloride reference substance, adds methanol or ethanol reference substance solution; Test according to thin layer chromatography, draw each 1 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, with dimethylbenzene-Ethyl formate-methanol-dense ammoniacal liquor=8: 5: 3: 0.1 was developing solvent, takes out, and dries, put under the uviol lamp and inspect, in the test sample chromatograph, with reference substance chromatograph, the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Embodiments of the invention 8: the thin layer chromatography discrimination method of Radix Paeoniae Rubra, peoniflorin in the capsule
It is an amount of to get the prostatitis-treating capsule content, adds methanol 25ml, and supersound process 20 minutes filters, and filtrate evaporate to dryness, residue add methanol makes dissolving, as need testing solution; Get the Radix Paeoniae Rubra control medicinal material, shine medical material solution in pairs with legal system; Other gets the peoniflorin reference substance, adds methanol and makes the solution that every 1ml contains 2mg, in contrast product solution; According to thin layer chromatography test, draw each 5 μ l of above-mentioned solution, respectively and on the same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-acetic acid=10: 1: 12: 2 was developing solvent, launches, and takes out, dry, spray is with 1% vanillin sulfuric acid solution, 105 ℃ dry by the fire to speckle colour developing clear; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color.
Embodiments of the invention 9: the thin layer chromatography discrimination method of peoniflorin in the drop pill
It is an amount of to get the QIANLIE ANTONG preparation, gets content, adds ethanol or methanol extraction, filters, and filtrate concentrates, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol or methanol is made reference substance solution; According to the thin layer chromatography test, draw each 1 μ l of above-mentioned two kinds of solution, put in same silica gel G F respectively
254On the lamellae, be developing solvent with chloroform-sour acid butyl ester-methanol=40: 1: 12, launch, take out, dry that spray is with 10% ethanol solution of sulfuric acid, it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Embodiments of the invention 10: the thin layer chromatography discrimination method of Radix Salviae Miltiorrhizae, danshensu sodium in the capsule
It is an amount of to get the prostatitis-treating capsule content, adds water temperature and soaks, and filters, and supernatant is regulated pH value to 1 with dilute hydrochloric acid, extracts with the chloroform jolting, and extracting solution evaporate to dryness, residue add methanol makes dissolving, as need testing solution; Other gets the Radix Salviae Miltiorrhizae control medicinal material, shines medical material solution in pairs with legal system; Get danshensu sodium, add methanol and make reference substance solution; According to thin layer chromatography test, draw each 1 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with chloroform-acetone-formic acid=5: 10: 4, launch, take out, dry, spray ferric chloride alcoholic solution with 2%; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color.
Embodiments of the invention 11: the thin layer chromatography discrimination method of danshensu, protocatechualdehyde in the granule
It is an amount of to get the QIANLIE ANTONG granule, adds the water supersound extraction, and extracting solution is regulated pH to 4 with acid solution, extracts with the ethyl acetate jolting, and extracting solution evaporate to dryness, residue add ethanol makes dissolving, as need testing solution; Get danshensu, protocatechualdehyde, add ethanol and make reference substance solution; According to the thin layer chromatography test, draw each 30 μ l of above-mentioned two kinds of solution, put in same silica gel G F respectively
254On the lamellae, be developing solvent, launch, take out that dry, spray is inspected under the visible light with the mixed solution of the ferric chloride and the potassium ferricyanide with benzene-ethyl acetate-formic acid=8: 6: 1; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Embodiments of the invention 12: the thin layer chromatography discrimination method of Radix Salviae Miltiorrhizae, salvianolic acid B in the tablet
It is an amount of to get the QIANLIE ANTONG tablet, adds methanol eddy and extracts, and extracting solution concentrates, as need testing solution; Other gets the Radix Salviae Miltiorrhizae control medicinal material, shines medical material solution in pairs with legal system; Get salvianolic acid B, add methanol and make reference substance solution; According to the thin layer chromatography test, draw each 1 μ l of above-mentioned three kinds of solution, put in same silica gel G F respectively
254On the lamellae, with toluene-chloroform-ethyl acetate-methanol-formic acid=2: 0.5: 0.5: be developing solvent at 0.5: 2, launches, and takes out, and dries, and 254nm inspects under the uviol lamp; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color.
Embodiments of the invention 13: the thin layer chromatography discrimination method of Radix Salviae Miltiorrhizae in the drop pill
It is an amount of to get the QIANLIE ANTONG drop pill, extracts with 50% ethanol jolting, and extracting solution concentrates, as need testing solution; Other gets the Radix Salviae Miltiorrhizae control medicinal material, shines medical material solution in pairs with legal system; According to thin layer chromatography test, draw each 30 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with benzene-chloroform-Ethyl formate-acetic acid=0.2: 0.5: 3: 1 developing solvent, launch, take out, dry, spray is with ethanol solution of sulfuric acid, and heating is inspected under the visible light; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Embodiments of the invention 14: the thin layer chromatography discrimination method of the Radix Angelicae Dahuricae in the capsule
It is an amount of to get the QIANLIE ANTONG preparation, and it is ultrasonic that content adds water, centrifugal, and supernatant is regulated pH value to 14 with sodium hydroxide test solution, extracts with chloroform 20ml jolting, and extracting solution concentrates, as need testing solution; Other gets Radix Angelicae Dahuricae control medicinal material and shines medical material solution in pairs with legal system; According to thin layer chromatography test, draw each 1 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, be developing solvent with chloroform-methanol=4: 1, launch, taking-up is dried, and puts that 254nm inspects under the ultra-violet lamp; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Embodiments of the invention 15: the thin layer chromatography discrimination method of the Radix Angelicae Dahuricae in the tablet
It is an amount of to get the QIANLIE ANTONG preparation, adds the water temperature lixiviate and gets, and extracting solution is regulated pH value to 9 with the potassium hydroxide test solution, extracts with the chloroform jolting, and extracting solution concentrates, as need testing solution; Other gets Radix Angelicae Dahuricae control medicinal material, adds ethyl acetate extraction, extracts to concentrate, in contrast medical material solution; According to thin layer chromatography test, draws each 30 μ l of above-mentioned kind of solution, put respectively on same silica gel H lamellae, be developing solvent with ethyl acetate-methanol=9: 1, expansion, taking-up is dried, and puts that 365nm inspects under the ultra-violet lamp; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Embodiments of the invention 16: the thin layer chromatography discrimination method of Semen Persicae, amygdalin in the granule
It is an amount of to get the QIANLIE ANTONG granule, adds methanol 20ml supersound process 20min, filters, filtrate evaporate to dryness, residue add water 5ml slight fever makes dissolving, puts cold, D101 type macroporous adsorptive resins by internal diameter 1.5cm, long 8cm adds water 20m prewashing once, last sample, discard water liquid,, discard ammoniacal liquor with ammonia solution 30ml eluting, reuse water 10ml eluting discards water liquid, continues with 20% ethanol 30ml eluting, collect eluent, evaporate to dryness, residue add methanol 1ml makes dissolving as need testing solution; Get the Semen Persicae medical material, the 20ml that adds diethyl ether refluxes, and discards ether solution, adds methanol 20ml again and refluxes, and filters, and filtrate concentrates, in contrast medical material solution; Other gets the amygdaloside reference substance, adds methanol and makes the solution that every 1ml contains 2mg, in contrast product solution; Draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate,, spray immediately, at 105 ℃ of about 10min of baking with 10% sulphuric acid ethanol so that chloroform-methanol-water=the lower floor's solution in placement below 10 ℃ was developing solvent in 13: 7: 2, launched, and took out; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color.
Embodiments of the invention 17: one or both thin layer chromatography discrimination method in Herba Lycopi, the ursolic acid in the drop pill
It is an amount of to get the QIANLIE ANTONG preparation, adds ethanol 30ml, and supersound process 10 minutes is put coldly, filter, and the filtrate evaporate to dryness, residue soaks with petroleum ether 10ml, and the petroleum ether that inclines, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets Herba Lycopi's control medicinal material, shines medical material solution in pairs with legal system; Get the ursolic acid reference substance again, add dehydrated alcohol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 1 μ l of above-mentioned solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with cyclohexane extraction-dichloromethane-ethyl acetate-acetic acid=10: 5: 1: 1 was developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color.
Embodiments of the invention 18: the high performance liquid chromatography discrimination method of protocatechualdehyde in the capsule
It is an amount of to get the prostatitis-treating capsule content, adds the water supersound process, filters, and subsequent filtrate is regulated pH value to 1 with 10% hydrochloric acid, extract with the ethyl acetate jolting, evaporate to dryness in the extracting solution water-bath, residue adds dissolve with methanol, filter with microporous filter membrane, get subsequent filtrate, as need testing solution; It is an amount of to get the protocatechualdehyde reference substance, puts in the brown measuring bottle, adds methanol and makes reference substance solution; With eight alkyl silane bonded silica gels is filler; Methanol-water-phosphoric acid=50: 50: 0.01 is a mobile phase; The detection wavelength is 361nm; Number of theoretical plate calculates by protocatechualdehyde should be not less than 2000; Accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing inject chromatograph of liquid, measure; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention.
Embodiments of the invention 19: the high performance liquid chromatography discrimination method of protocatechualdehyde in the tablet
It is an amount of to get the QIANLIE ANTONG tablet, adds water temperature and soaks processing, takes out, and puts to room temperature, filter, subsequent filtrate is regulated pH value to 3 with dilute hydrochloric acid, extracts the extracting solution evaporate to dryness with the chloroform jolting, residue adds dissolve with ethanol and standardize solution, filters with microporous filter membrane, gets subsequent filtrate, as need testing solution; It is an amount of to get the protocatechualdehyde reference substance, adds ethanol and makes reference substance solution; With octadecylsilane chemically bonded silica is filler; Acetonitrile-water-acetic acid=10: 95: 5 is mobile phase; The detection wavelength is 281nm; Number of theoretical plate calculates by protocatechualdehyde should be not less than 2000; Accurate respectively reference substance solution and each 30 μ l of need testing solution of drawing inject chromatograph of liquid, measure; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention.
Embodiments of the invention 20: the high performance liquid chromatography discrimination method of salvianolic acid B in the drop pill
It is an amount of to get the QIANLIE ANTONG drop pill, adds 80% methanol supersound process, filters, as need testing solution; It is an amount of to get the salvianolic acid B reference substance, adds 80% methanol and makes reference substance solution; With the dialkyl silane bonded silica gel is filler; Methanol-formic acid-water=30: 1: 59 is mobile phase; The detection wavelength is 286nm; Number of theoretical plate calculates by salvianolic acid B should be not less than 2000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention.
Embodiments of the invention 21: the high performance liquid chromatography discrimination method of salvianolic acid B in the capsule
It is an amount of to get the prostatitis-treating capsule content, adds 95% ethanol supersound process, takes out, and puts to room temperature, filters, as need testing solution; It is an amount of to get the salvianolic acid B reference substance, adds 95% ethanol and makes reference substance solution; With octadecylsilane chemically bonded silica is filler; Methanol-acetonitrile-phosphoric acid-water=10: 10: 0.4: 70 is mobile phase; The detection wavelength is 245nm; Number of theoretical plate calculates by salvianolic acid B should be not less than 2000; Accurate respectively reference substance solution and each 1 μ l of need testing solution of drawing injects chromatograph of liquid, measures; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention.
Embodiments of the invention 22: the high performance liquid chromatography discrimination method of peoniflorin in the granule
It is an amount of to get the QIANLIE ANTONG granule, adds the methanol supersound process, filters, as need testing solution; It is an amount of to get the peoniflorin reference substance, adds methanol and makes reference substance solution; With eight alkyl silane bonded silica gels is filler; Acetonitrile-water-potassium dihydrogen phosphate=5: 95: 5 is a mobile phase; The detection wavelength is 230nm; Number of theoretical plate calculates by peoniflorin should be not less than 3000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention.
Embodiments of the invention 23: the high performance liquid chromatography discrimination method of peoniflorin in the tablet
It is an amount of to get the QIANLIE ANTONG tablet, adds ethanol ultrasonic extraction, filters, as need testing solution; It is an amount of to get the peoniflorin reference substance, adds ethanol and makes reference substance solution; With eight alkyl silane bonded silica gels is filler; Methanol-water-phosphoric acid=50: 50: 0.5 is a mobile phase; The detection wavelength is 360nm; Number of theoretical plate calculates by peoniflorin should be not less than 3000; Accurate respectively reference substance solution and each 30 μ l of need testing solution of drawing inject chromatograph of liquid, measure; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention.
Embodiments of the invention 24: the high performance liquid chromatography discrimination method of berberine hydrochloride in the drop pill
It is an amount of to get the QIANLIE ANTONG drop pill, and the mixed solution supersound process that adds hydrochloric acid-methanol=5: 100 is taken out, and puts to room temperature, filters, and gets subsequent filtrate, is need testing solution; Get the berberine hydrochloride reference substance, add above-mentioned solvent and make reference substance solution; With octadecylsilane chemically bonded silica is filler; With water-acetic acid-acetonitrile=20: 5: 20 was mobile phase; The detection wavelength is 270nm; Number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 2000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention.
Embodiments of the invention 25: the high performance liquid chromatography discrimination method of berberine hydrochloride in the capsule
It is an amount of to get the prostatitis-treating capsule content, adds the ethanol supersound process, and extracting solution is a need testing solution; Get the berberine hydrochloride reference substance, add above-mentioned solvent and make reference substance solution; With the dialkyl silane bonded silica gel is filler; With water-acetic acid-acetonitrile=60: 1: 5 was mobile phase; The detection wavelength is 370nm; Number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 2000; Accurate respectively reference substance solution and each 1 μ l of need testing solution of drawing injects chromatograph of liquid, measures; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention.
Embodiments of the invention 26: the high-efficient liquid phase chromatogram process measuring method of drop pill Central Plains catechu aldehyde
It is an amount of to get the QIANLIE ANTONG drop pill, and accurate the title decides, and puts in the tool plug conical flask, precision adds water 50ml, and weight, supersound process 30 minutes decided in accurate title, take out, put to room temperature, weight decided in accurate title, add water and supply the weight that subtracts mistake, shake up, filter, the accurate subsequent filtrate 10ml that draws, regulate pH value to 2 with dilute hydrochloric acid, extract 3 times, each 10ml with the ethyl acetate jolting, the combined ethyl acetate extracting solution, put evaporate to dryness in the water-bath, residue adds dissolve with ethanol and quantitatively is transferred in the 10ml measuring bottle, adds ethanol to scale, shake up, filter with microporous filter membrane, get subsequent filtrate, as need testing solution; It is an amount of to get the protocatechualdehyde reference substance, and accurate the title decides, and puts in the brown measuring bottle, adds ethanol and makes the solution that contains 10 μ g among every 1ml, in contrast product solution; With eight alkyl silane bonded silica gels is filler; Acetonitrile-water-phosphoric acid=13: 87: 0.3 is mobile phase; The detection wavelength is 281nm; Number of theoretical plate calculates by protocatechualdehyde should be not less than 2000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate with one point external standard method, promptly; Content limit should be: must not be lower than 216 μ g with containing Radix Salviae Miltiorrhizae in protocatechualdehyde in the QIANLIE ANTONG drop pill on 1st.
Embodiments of the invention 27: the high-efficient liquid phase chromatogram process measuring method of granule Central Plains catechu aldehyde
It is an amount of to get the QIANLIE ANTONG preparation, and accurate the title decides, and adds the water supersound process, add water and supply the weight that subtracts mistake, shake up, filter, subsequent filtrate is regulated pH value to 3 with acid solution, extract with the chloroform jolting, merge extractive liquid, is put evaporate to dryness in the water-bath, residue adds dissolve with methanol and standardize solution, filter with microporous filter membrane, get subsequent filtrate, as need testing solution; It is an amount of to get the protocatechualdehyde reference substance, puts in the brown measuring bottle, adds methanol and is made as reference substance solution; With the dialkyl silane bonded silica gel is filler; Methanol-water-acetic acid=30: 95: 2 is mobile phase; The detection wavelength is 200nm; Number of theoretical plate calculates by protocatechualdehyde should be not less than 2000; Accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate with one point external standard method or standard curve method; Content limit should be: must not be lower than 216 μ g with containing Radix Salviae Miltiorrhizae in protocatechualdehyde in the QIANLIE ANTONG drop pill on 1st.
Embodiments of the invention 28: the high-efficient liquid phase chromatogram process measuring method of content of danshinolic acid B in the drop pill
It is an amount of to get the QIANLIE ANTONG drop pill, and accurate the title decides, and adds the methanol supersound process 30 minutes, takes out, and puts to room temperature, and accurate the title decided weight, adds methanol and supplies the weight that subtracts mistake, shakes up, and filters, as need testing solution; It is an amount of to get the salvianolic acid B reference substance, and accurate the title decides, and adds methanol and makes reference substance solution; With octadecylsilane chemically bonded silica is filler; Methanol-acetonitrile-acetic acid-water=10: 30: 1: 60 is mobile phase; The detection wavelength is 286nm; Number of theoretical plate calculates by salvianolic acid B should be not less than 2000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate with one point external standard method, promptly; Content limit should be: must not be lower than 21.6mg with containing Radix Salviae Miltiorrhizae in salvianolic acid B in the QIANLIE ANTONG preparation on 1st.
Embodiments of the invention 29: the high-efficient liquid phase chromatogram process measuring method of content of danshinolic acid B in the tablet
It is an amount of to get the QIANLIE ANTONG tablet, and accurate the title decides, and adds 50% ethanol supersound process 30 minutes, takes out, and puts to room temperature, and accurate the title decided weight, adds 50% ethanol and supplies the weight that subtracts mistake, shakes up, and filters, as need testing solution; It is an amount of to get the salvianolic acid B reference substance, and accurate the title decides, and adds 50% ethanol and makes reference substance solution; With the dialkyl silane bonded silica gel is filler; Acetonitrile-phosphoric acid-water=30: 0.3: 60 is mobile phase; The detection wavelength is 376nm; Number of theoretical plate calculates by salvianolic acid B should be not less than 2000; Accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate with one point external standard method, promptly; Content limit should be: must not be lower than 21.6mg with containing Radix Salviae Miltiorrhizae in salvianolic acid B in the QIANLIE ANTONG preparation on 1st.
Embodiments of the invention 30: the high-efficient liquid phase chromatogram process measuring method of paeoniflorin content in the tablet
It is an amount of to get the QIANLIE ANTONG tablet, and accurate the title decides, and adds the methanol supersound process 30 minutes, takes out, and puts to room temperature, and accurate the title decided weight, adds methanol and supplies the weight that subtracts mistake, shakes up, and filters, as need testing solution; It is an amount of to get the peoniflorin reference substance that is dried to constant weight, and accurate the title decides, and adds methanol and makes reference substance solution; With eight alkyl silane bonded silica gels is filler; Methanol-water-phosphoric acid=8: 60: 0.5 is a mobile phase; The detection wavelength is 230nm; Number of theoretical plate calculates by peoniflorin should be not less than 3000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate with one point external standard method, promptly; Content limit should be: must not be lower than 26.4mg with containing Radix Paeoniae Rubra in peoniflorin in the QIANLIE ANTONG preparation on 1st.
Embodiments of the invention 31: the high-efficient liquid phase chromatogram process measuring method of content of berberine hydrochloride in the granule
It is an amount of to get the QIANLIE ANTONG granule, and accurate the title decides, and adds the methanol supersound process 30 minutes, takes out, and puts to room temperature, supplies the solvent of loss, shakes up, and filters, and gets subsequent filtrate, is need testing solution; Get the berberine hydrochloride reference substance, add above-mentioned solvent and make reference substance solution; Water-potassium dihydrogen phosphate-acetonitrile=60: 5: 5 is a mobile phase; The detection wavelength is 350nm; Number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 2000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate with one point external standard method, promptly; Content limit should be: must not be lower than 72mg with containing Cortex Phellodendri in the QIANLIE ANTONG preparation with berberine hydrochloride on 1st.
Embodiments of the invention 32: the thin layer chromatography discrimination method of berberine hydrochloride, Cortex Phellodendri in the capsule
It is an amount of to get the QIANLIE ANTONG preparation, the 20ml that adds diethyl ether, and supersound process 20 minutes discards ether solution, and medicinal residues volatilize, and add methanol 20ml, and supersound process 20 minutes filters, and filtrate is concentrated into 2ml, as need testing solution; Get the Cortex Phellodendri medical material, shine medical material solution in pairs with legal system; Other gets the berberine hydrochloride reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, with benzene-ethyl acetate-methanol-isopropyl alcohol-strong ammonia solution=4: 3: 2: be developing solvent at 1.5: 0.5, launches, take out, dry, put under the uviol lamp 365nm and inspect, in the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color.
Embodiments of the invention 33: the thin layer chromatography discrimination method of Radix Paeoniae Rubra, peoniflorin in the drop pill
It is an amount of to get the QIANLIE ANTONG preparation, gets content, adds ethanol 25ml, and supersound process 20 minutes filters, and filtrate evaporate to dryness, residue add ethanol 2ml makes dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 2mg, in contrast product solution; According to thin layer chromatography test, draw each 5 μ l of above-mentioned solution, respectively and on the same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-formic acid=40: 5: 12: 0.2 was developing solvent, launches, and takes out, dry, spray is with 5% vanillin sulfuric acid solution, 105 ℃ dry by the fire to speckle colour developing clear; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color.
Embodiments of the invention 34: the thin layer chromatography discrimination method of Radix Salviae Miltiorrhizae, danshensu, protocatechualdehyde in the preparation
It is an amount of to get the QIANLIE ANTONG preparation, adds water 20ml, and ultrasonic 30 minutes, centrifugal, supernatant was regulated pH value to 2 with dilute hydrochloric acid, extracted with ethyl acetate 20ml jolting, and extracting solution evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Salviae Miltiorrhizae control medicinal material 0.5g, and it is an amount of to add water, decocts 30 minutes, adds water to 20ml, shines medical material solution in pairs with legal system; Get danshensu, protocatechualdehyde, add methanol and make reference substance solution; According to the thin layer chromatography test, draw above-mentioned solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-acetone-formic acid=25: 10: 4 was developing solvent, launched, and took out, dry, spray ferric chloride alcoholic solution, place about 30 minutes to clear spot with 2%; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color.
Embodiments of the invention 35: the thin layer chromatography discrimination method of Radix Salviae Miltiorrhizae, salvianolic acid B in the tablet
It is an amount of to get the QIANLIE ANTONG preparation, and 75% methanol jolting is extracted, and extracting solution concentrates, as need testing solution; Other gets the Radix Salviae Miltiorrhizae control medicinal material, shines medical material solution in pairs with legal system; Salvianolic acid B or its magnesium salt add 75% methanol and make reference substance solution; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned solution, put in same silica gel G F respectively
254On the lamellae, with toluene-chloroform-ethyl acetate-methanol-formic acid=2: 3: 4: be developing solvent at 0.5: 2, launches, and takes out, and dries, and 254nm inspects under the uviol lamp; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color.
Embodiments of the invention 36: the thin layer chromatography discrimination method of the Radix Angelicae Dahuricae in the granule
It is an amount of to get the QIANLIE ANTONG preparation, and content adds water 20ml, and ultrasonic 30 minutes, centrifugal, supernatant was regulated pH value to 12 with sodium hydroxide test solution, extracted with chloroform 20ml jolting, and extracting solution is concentrated into 1ml, as need testing solution; Other gets Radix Angelicae Dahuricae control medicinal material 0.5g, adds chloroform 10ml, and ultrasonic 30 minutes, filter, filtrate is concentrated into 1ml, in contrast medical material solution; According to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with chloroform-methanol=9: 1, put in the vapour-saturated expansion cylinder of ammonia, launch, taking-up is dried, and puts that 254nm inspects under the ultra-violet lamp; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Embodiments of the invention 37: the thin layer chromatography discrimination method of Semen Persicae, amygdalin in the capsule
It is an amount of to get the QIANLIE ANTONG preparation, adds methanol 20ml supersound process 20min, filters, filtrate evaporate to dryness, residue add water 5ml slight fever makes dissolving, puts cold, D101 type macroporous adsorptive resins by internal diameter 1.5cm, long 8cm adds water 20m prewashing once, last sample, discard water liquid,, discard ammoniacal liquor with ammonia solution 30ml eluting, reuse water 10ml eluting discards water liquid, continues with 20% ethanol 30ml eluting, collect eluent, evaporate to dryness, residue add methanol 1ml makes dissolving as need testing solution; Get the Semen Persicae medical material, the 20ml that adds diethyl ether refluxes, and discards ether solution, adds methanol 20ml again and refluxes, and filters, and filtrate concentrates, in contrast medical material solution; Other gets the amygdaloside reference substance, adds methanol and makes the solution that every 1ml contains 2mg, in contrast product solution; Draw each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-water=15: 40: 22: 10 was developing solvent at 5～10 ℃ of lower floor's solution of placing 12h, launch, take out, spray immediately, at 105 ℃ of about 10min of baking with the phosphomolybdic acid sulfuric acid solution; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color.
Embodiments of the invention 38: the thin layer chromatography discrimination method of Herba Lycopi, ursolic acid in the tablet
It is an amount of to get the QIANLIE ANTONG preparation, adds acetone 30ml, and supersound process 10 minutes is put coldly, filter, and the filtrate evaporate to dryness, residue soaks with petroleum ether 10ml, and the petroleum ether that inclines, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets Herba Lycopi's control medicinal material, shines medical material solution in pairs with legal system; Get the ursolic acid reference substance again, add dehydrated alcohol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 5 μ l of above-mentioned solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with cyclohexane extraction-chloroform-ethyl acetate-formic acid=20: 5: 8: 0.1 was developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the speckle of same color.
Embodiments of the invention 39: the high performance liquid chromatography discrimination method of protocatechualdehyde in the granule
It is an amount of to get the QIANLIE ANTONG preparation, adds water 50ml, supersound process 30 minutes, take out, put, filter to room temperature, subsequent filtrate is regulated pH value to 2 with 10% hydrochloric acid, extracts 3 times with the ether jolting, each 10ml, merge ether extracted liquid, put evaporate to dryness in the water-bath, residue adds dissolve with methanol and standardize solution, filters with microporous filter membrane, get subsequent filtrate, as need testing solution; It is an amount of to get the protocatechualdehyde reference substance, puts in the brown measuring bottle, adds methanol and makes the solution that contains 12 μ g among every 1ml, in contrast product solution; With octadecylsilane chemically bonded silica is filler; Methanol-1% glacial acetic acid aqueous solution=13: 87 is a mobile phase; The detection wavelength is 281nm; Number of theoretical plate calculates by protocatechualdehyde should be not less than 2000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention.
Embodiments of the invention 40: the high performance liquid chromatography discrimination method of salvianolic acid B in the drop pill
It is an amount of to get the QIANLIE ANTONG preparation, adds the methanol supersound process 30 minutes, takes out, and puts to room temperature, filters, as need testing solution; It is an amount of to get the salvianolic acid B reference substance, adds 75% methanol and makes reference substance solution; With octadecylsilane chemically bonded silica is filler; Methanol-acetonitrile-formic acid-water=30: 10: 1: 59 is mobile phase; The detection wavelength is 286nm; Number of theoretical plate calculates by salvianolic acid B should be not less than 2000; Draw each 10 μ l of reference substance solution and need testing solution respectively, inject chromatograph of liquid, measure; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention.
Embodiments of the invention 41: the high performance liquid chromatography discrimination method of peoniflorin in the tablet
It is an amount of to get the QIANLIE ANTONG preparation, adds the methanol supersound process 30 minutes, takes out, and puts to room temperature, filters, as need testing solution; It is an amount of to get the peoniflorin reference substance that is dried to constant weight, adds methanol and makes reference substance solution; With octadecylsilane chemically bonded silica is filler; Methanol-0.05mol/L potassium dihydrogen phosphate=40: 65 is mobile phase; The detection wavelength is 230nm; Number of theoretical plate calculates by peoniflorin should be not less than 3000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention.
Embodiments of the invention 42: the high performance liquid chromatography discrimination method of berberine hydrochloride in the capsule
It is an amount of to get the QIANLIE ANTONG preparation, adds the mixed solution supersound process 30 minutes of hydrochloric acid-methanol=1: 100, takes out, and puts to room temperature, supplies the solvent of loss, shakes up, and filters, and gets subsequent filtrate, is need testing solution; Get the berberine hydrochloride reference substance, add above-mentioned solvent and make reference substance solution; Regulating the 0.05mol/L sodium dihydrogen phosphate-acetonitrile of pH value to 3.0=75: 25 with phosphoric acid is mobile phase; The detection wavelength is 270nm; Number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 2000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention.
Embodiments of the invention 43: the high-efficient liquid phase chromatogram process measuring method of capsule Central Plains catechu aldehyde
It is an amount of to get the QIANLIE ANTONG preparation, and accurate the title decides, and puts in the tool plug conical flask, precision adds water 50ml, and weight, supersound process 30 minutes decided in accurate title, take out, put to room temperature, weight decided in accurate title, add water and supply the weight that subtracts mistake, shake up, filter, the accurate subsequent filtrate 10ml that draws, regulate pH value to 2 with 10% hydrochloric acid, extract 3 times, each 10ml with the ether jolting, merge ether extracted liquid, put evaporate to dryness in the water-bath, residue adds dissolve with methanol and quantitatively is transferred in the 10ml measuring bottle, adds methanol to scale, shake up, filter with microporous filter membrane, get subsequent filtrate, as need testing solution; It is an amount of to get the protocatechualdehyde reference substance, and accurate the title decides, and puts in the brown measuring bottle, adds methanol and makes the solution that contains 12 μ g among every 1ml, in contrast product solution; With octadecylsilane chemically bonded silica is filler; Methanol-1% glacial acetic acid aqueous solution=13: 87 is a mobile phase; The detection wavelength is 281nm; Number of theoretical plate calculates by protocatechualdehyde should be not less than 2000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate with one point external standard method, promptly; Content limit is: be not less than 216 μ g with containing Radix Salviae Miltiorrhizae in protocatechualdehyde in the QIANLIE ANTONG preparation on 1st.
Embodiments of the invention 44: the high-efficient liquid phase chromatogram process measuring method of content of danshinolic acid B in the drop pill
It is an amount of to get the QIANLIE ANTONG preparation, and accurate the title decides, and adds the methanol supersound process 30 minutes, takes out, and puts to room temperature, and accurate the title decided weight, adds methanol and supplies the weight that subtracts mistake, shakes up, and filters, as need testing solution; It is an amount of to get the salvianolic acid B reference substance, and accurate the title decides, and adds 75% methanol and makes reference substance solution; With octadecylsilane chemically bonded silica is filler; Methanol-acetonitrile-formic acid-water=30: 10: 1: 59 is mobile phase; The detection wavelength is 286nm; Number of theoretical plate calculates by salvianolic acid B should be not less than 2000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate with one point external standard method, promptly; Content limit is: be not less than 21.6mg with containing Radix Salviae Miltiorrhizae in salvianolic acid B in the QIANLIE ANTONG preparation on 1st.
Embodiments of the invention 45: the high-efficient liquid phase chromatogram process measuring method of paeoniflorin content in the granule
It is an amount of to get the QIANLIE ANTONG preparation, and accurate the title decides, and adds the methanol supersound process 30 minutes, takes out, and puts to room temperature, and accurate the title decided weight, adds methanol and supplies the weight that subtracts mistake, shakes up, and filters, as need testing solution; It is an amount of to get the peoniflorin reference substance that is dried to constant weight, and accurate the title decides,, add methanol and make reference substance solution; With octadecylsilane chemically bonded silica is filler; Methanol-0.05mol/L potassium dihydrogen phosphate=40: 65 is mobile phase; The detection wavelength is 230nm; Number of theoretical plate calculates by peoniflorin should be not less than 3000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate with one point external standard method, promptly; Content limit is: be not less than 26.4mg with containing Radix Paeoniae Rubra in peoniflorin in the QIANLIE ANTONG preparation on 1st.
Embodiments of the invention 46: the high-efficient liquid phase chromatogram process measuring method of content of berberine hydrochloride in the tablet
It is an amount of to get the QIANLIE ANTONG preparation, accurate claims surely, adds the mixed solution supersound process 30 minutes of hydrochloric acid-methanol=1: 100, takes out, and puts to room temperature, supplies the solvent of loss, shakes up, and filters, and gets subsequent filtrate, is need testing solution; Get the berberine hydrochloride reference substance, add above-mentioned solvent and make reference substance solution; Regulating the 0.05mol/L sodium dihydrogen phosphate-acetonitrile of pH value to 3.0=75: 25 with phosphoric acid is mobile phase; The detection wavelength is 270nm; Number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 2000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate with one point external standard method, promptly; Content limit is: be not less than 72mg with containing Cortex Phellodendri in the QIANLIE ANTONG preparation with berberine hydrochloride on 1st.
Claims (10)
1. prostatitic pharmaceutical preparation of treatment, it is characterized in that: it is made into effervescent tablet, injection, powder pin, freeze-dried powder, gel, dispersible tablet, capsule, soft capsule, microcapsule, granule, pill, micropill, powder, drop pill, slow releasing preparation, controlled release preparation, gel, oral liquid, soft extract, extractum and membrane by Cortex Phellodendri 200g, Radix Paeoniae Rubra 200g, Radix Salviae Miltiorrhizae 100g, Semen Persicae 140g, Herba Lycopi 120g, Radix Linderae 120g, Semen Vaccariae 80g and Radix Angelicae Dahuricae 80g or with their extract of corresponding weight portion.
2. according to the prostatitic pharmaceutical preparation of the described treatment of claim 1, it is characterized in that: described preparation is capsule or drop pill.
3. the preparation method of the prostatitic pharmaceutical preparation of treatment as claimed in claim 1 or 2 is characterized in that: get Cortex Phellodendri, the fine powder that was ground into 80 mesh sieves is standby; When Radix Paeoniae Rubra, Radix Salviae Miltiorrhizae, Herba Lycopi, the Radix Linderae, Semen Vaccariae and the Radix Angelicae Dahuricae add 8 times of water and are heated to 80 ℃, add Semen Persicae again, continue heating, decoct three times, 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time, collecting decoction, filter, relative density was 1.05～1.10 thick paste when filtrate was condensed into 60 ℃, added the Cortex Phellodendri fine powder, made different preparations then respectively.
4. according to the preparation method of the prostatitic pharmaceutical preparation of the described treatment of claim 3, it is characterized in that: the capsule in the described preparation prepares like this: get Cortex Phellodendri, the fine powder that was ground into 80 mesh sieves is standby; When Radix Paeoniae Rubra, Radix Salviae Miltiorrhizae, Herba Lycopi, the Radix Linderae, Semen Vaccariae and the Radix Angelicae Dahuricae add 8 times of water and be heated to 80 ℃, add Semen Persicae again, continue heating, decoct three times, 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time, collecting decoction filtered, relative density was 1.05～1.10 thick paste when filtrate was condensed into 60 ℃, and drying under reduced pressure is ground into fine powder, add Cortex Phellodendri fine powder and starch, Pulvis Talci, amount of talc is 5%, mixing, incapsulate, should control relative humidity during packing below 65.0%, promptly.
5. according to the preparation method of the prostatitic pharmaceutical preparation of the described treatment of claim 3, it is characterized in that: the drop pill in the described preparation prepares like this: get Cortex Phellodendri, the fine powder that was ground into 80 mesh sieves is standby; Radix Paeoniae Rubra, Radix Salviae Miltiorrhizae, the Herba Lycopi, the Radix Linderae, when the Semen Vaccariae and the Radix Angelicae Dahuricae add 8 times of water and are heated to 80 ℃, add Semen Persicae again, continue heating, decoct three times, 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time, collecting decoction, filter, relative density was 1.05～1.10 thick paste when filtrate was condensed into 60 ℃, added the Cortex Phellodendri fine powder, was substrate with the Macrogol 4000, according to medicine: the part by weight of substrate=1: 2 adds Macrogol 4000, mixing, the employing internal diameter is 3.0mm, external diameter is the dropper of 4.0mm, drips 80 ℃ of system temperature, dripping speed is 20～30d/min, dripping distance is 5cm, splash in the long cooling column of 130cm, be liquid coolant again with the methyl-silicone oil, pill, promptly.
6. the method for quality control of the prostatitic pharmaceutical preparation of treatment as claimed in claim 1 or 2 is characterized in that: this method comprises following all or part of content:
(1) one or more differential test method in berberine hydrochloride, Cortex Phellodendri, Radix Paeoniae Rubra, peoniflorin, Radix Salviae Miltiorrhizae, danshensu or its sodium salt, protocatechualdehyde, salvianolic acid B or its magnesium salt, the Radix Angelicae Dahuricae, Semen Persicae, amygdalin, Herba Lycopi, the ursolic acid;
(2) one or more content test method in berberine hydrochloride, peoniflorin, salvianolic acid B or its magnesium salt, the protocatechualdehyde.
7. according to the method for quality control of the prostatitic pharmaceutical preparation of the described treatment of claim 6, it is characterized in that: the discrimination method of described preparation comprises following all or part of content:
A. one or both thin layer chromatography discrimination method in berberine hydrochloride, the Cortex Phellodendri in the preparation:
It is an amount of to get this preparation, adds diethyl ether or petroleum ether or ethyl acetate or chloroform extraction, discards extracting solution, and medicinal residues volatilize, and add 20～100% methanol or ethanol extraction again, the preparation need testing solution; Or it is an amount of to get this preparation, directly adds 20～100% methanol or ethanol extraction, the preparation need testing solution; Get the Cortex Phellodendri medical material, with reference to a kind of control medicinal material solution of making in the need testing solution preparation method; Other gets the berberine hydrochloride reference substance, adds 20～100% methanol or ethanol and makes reference substance solution; Test according to thin layer chromatography, draw one or both each 1～30 μ l in above-mentioned need testing solution, control medicinal material or the reference substance solution, put respectively on same silica gel G or silica gel H lamellae, with benzene or toluene or dimethylbenzene-ethyl acetate or Ethyl formate or sour acid butyl ester-isopropyl alcohol or n-butyl alcohol-methanol or ethanol-dense ammoniacal liquor=1～12: be developing solvent at 1～6: 0～3: 0～3: 0～1, take out, dry, put under the uviol lamp and inspect, in the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color;
B. one or both thin layer chromatography discrimination method in Radix Paeoniae Rubra, the peoniflorin in the preparation:
It is an amount of to get this preparation, adds 20～100% ethanol or methanol extraction, the preparation need testing solution; Get the Radix Paeoniae Rubra medical material, shine medical material solution in pairs with legal system; Other gets the peoniflorin reference substance, adds 20～100% ethanol or methanol and makes reference substance solution; Test according to thin layer chromatography, draw one or both each 1～30 μ l in above-mentioned need testing solution, control medicinal material or the reference substance solution, put respectively on same silica gel G or silica gel H or silica GF254 lamellae, with chloroform or dichloromethane-ethyl acetate or Ethyl formate or sour acid butyl ester-methanol or ethanol-formic acid or acetic acid=10～40: be developing solvent at 1～5: 2～12: 0～2, launch, take out, dry, spray is with vanillin sulphuric acid or ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color;
C. one or more thin layer chromatography discrimination method in Radix Salviae Miltiorrhizae, danshensu or its sodium salt, the protocatechualdehyde in the preparation:
It is an amount of to get this preparation, extracting in water, and extracting solution is regulated pH1～4 with acid solution, and with ethyl acetate or chloroform extraction, extracting solution evaporate to dryness, residue add methanol or ethanol makes dissolving, as need testing solution; Or it is an amount of to get this preparation, adds 20～100% ethanol or methanol extraction, the preparation need testing solution; Get the Radix Salviae Miltiorrhizae control medicinal material,, make control medicinal material solution with reference to one of need testing solution preparation method; Get danshensu or its sodium salt, protocatechualdehyde, add 20～100% methanol or ethanol and make reference substance solution; Test according to thin layer chromatography, draw one or more each 1～30 μ l in above-mentioned need testing solution, control medicinal material or the reference substance solution, put respectively on same silica gel G or silica gel H or silica GF254 lamellae, with chloroform or dichloromethane or benzene or ethyl acetate-acetone or butanone or ethyl acetate-formic acid or acetic acid=5～25: be developing solvent at 1～10: 0～4, launch, take out, dry, spray is with the mixed solution of liquor ferri trichloridi or the ferric chloride and the potassium ferricyanide, inspect under the visible light, or with the ammonia steam smoked after, under uviol lamp, inspect; In the test sample chromatograph, with control medicinal material chromatograph, the corresponding position of reference substance chromatograph on, show the speckle of same color;
D. one or more thin layer chromatography discrimination method in Radix Salviae Miltiorrhizae, salvianolic acid B or its magnesium salt in the preparation:
It is an amount of to get this preparation, extracts the preparation need testing solution with 10～100% methanol or ethanol jolting; Other gets the Radix Salviae Miltiorrhizae control medicinal material, shines medical material solution in pairs with legal system; Salvianolic acid B or its magnesium salt are made reference substance solution; Test according to thin layer chromatography, draw one or both each 1～30 μ l in above-mentioned need testing solution, control medicinal material or the reference substance solution, put respectively on same silica gel G or silica gel H or silica GF254 lamellae, with toluene or benzene or dimethylbenzene-chloroform or dichloromethane-ethyl acetate or Ethyl formate or sour acid butyl ester-methanol or ethanol-formic acid or acetic acid=0.2～2: be developing solvent at 0.5～3: 0.5～4: 0～1: 0～2, launch, take out, dry, inspect under the uviol lamp, or spray is with ethanol solution of sulfuric acid, heating is inspected under the visible light; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color;
E. the thin layer chromatography discrimination method of the Radix Angelicae Dahuricae in the preparation:
It is an amount of to get this preparation, extracting in water, and extracting solution concentrates with chloroform or ethyl acetate extraction, extracting solution, as need testing solution; Or it is an amount of to get this preparation, extracts the preparation need testing solution with chloroform or ethyl acetate jolting; Other gets Radix Angelicae Dahuricae control medicinal material, with reference to one of need testing solution preparation method, makes control medicinal material solution; Test according to thin layer chromatography, draw each 1～30 μ l of above-mentioned two kinds of solution, put respectively on same silica gel G or silica gel H lamellae, with chloroform or dichloromethane or ethyl acetate-methanol or ethanol or acetone=1～9: 0.2～3 is developing solvent, put in the vapour-saturated expansion cylinder of ammonia, launch, take out, dry, put under the ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
F. one or both thin layer chromatography discrimination method in Semen Persicae, the amygdaloside in the preparation:
It is an amount of to get this preparation, adds 20～100% methanol or ethanol extraction, passes through macroporous adsorptive resins after extracting solution is handled again,, with 0～80% ethanol elution, collect the part eluent, evaporate to dryness, residue add 10～100% methanol or ethanol makes dissolving, as need testing solution; Get the Semen Persicae medical material, add diethyl ether or Petroleum ether extraction, discard extracting solution, add 20～100% methanol or ethanol extraction again, preparation control medicinal material solution; Other gets the amygdaloside reference substance, adds 20～100% methanol or ethanol and makes reference substance solution; Draw one or both each 1～30 μ l in above-mentioned need testing solution, control medicinal material or the reference substance solution, put respectively on same silica gel g thin-layer plate, with chloroform or dichloromethane-ethyl acetate or Ethyl formate or sour acid butyl ester-methanol or alcohol-water=0～15: 0～40: 1～22: 1～10 lower floor's solution 0～10 ℃ of placement is developing solvent, launch, take out, spray is with phosphomolybdic acid sulfuric acid solution or ethanol solution of sulfuric acid, and it is clear to be heated to colour developing; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color;
G. one or both thin layer chromatography discrimination method in Herba Lycopi, the ursolic acid in the preparation:
It is an amount of to get this preparation, adds diethyl ether or chloroform or ethyl acetate or ethanol or methanol or acetone extraction the preparation need testing solution; Other gets Herba Lycopi's control medicinal material, shines medical material solution in pairs with legal system; Get the ursolic acid reference substance again, add methanol or chloroform or ethyl acetate or ethanol and make dissolving, in contrast product solution; Test according to thin layer chromatography, draw one or both each 1～30 μ l in above-mentioned need testing solution, control medicinal material or the reference substance solution, put respectively on same silica gel G or silica gel H or silica GF254 lamellae, with cyclohexane extraction or normal hexane-chloroform or dichloromethane-ethyl acetate or butyl acetate or Ethyl formate-formic acid or acetic acid=0～20: be developing solvent at 1～5: 1～8: 0～1, launch, take out, dry, spray is with ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color;
H. the high performance liquid chromatography discrimination method of protocatechualdehyde in the preparation:
It is an amount of to get this preparation, extracting in water, and water liquid prepares need testing solution with ether or ethyl acetate or chloroform jolting extraction; Or it is an amount of to get this preparation, adds 10～100% methanol or ethanol extraction, the preparation need testing solution; It is an amount of to get the protocatechualdehyde reference substance, adds 20～100% methanol or ethanol and is made as reference substance solution; With octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels or dialkyl silane bonded silica gel is filler; Methanol or acetonitrile-water-acetic acid or formic acid or phosphoric acid=10～50: 30～95: 0.01～5 is mobile phase; The detection wavelength is one or several among 190～410nm; Number of theoretical plate calculates by protocatechualdehyde should be not less than 2000; Accurate respectively reference substance solution and each 1～30 μ l of need testing solution of drawing injects chromatograph of liquid, measures; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention;
I. the high performance liquid chromatography discrimination method of salvianolic acid B in the preparation:
It is an amount of to get this preparation, adds 10～100% methanol or ethanol extraction, the preparation need testing solution; It is an amount of to get the salvianolic acid B reference substance, adds 10～100% methanol or ethanol and makes reference substance solution; With octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels or dialkyl silane bonded silica gel is filler; Methanol or ethanol-acetonitrile-formic acid or acetic acid or phosphoric acid-water=10～30: 0～30: 0～5: 50～95 is mobile phase; The detection wavelength is one or several among 190～410nm; Number of theoretical plate calculates by salvianolic acid B should be not less than 2000; Accurate respectively reference substance solution and each 1～30 μ l of need testing solution of drawing injects chromatograph of liquid, measures; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention;
J. the high performance liquid chromatography discrimination method of peoniflorin in the preparation:
It is an amount of to get this preparation, adds 20～100% methanol or ethanol extraction, the preparation need testing solution; It is an amount of to get the peoniflorin reference substance, adds 20～100% methanol or ethanol and makes reference substance solution; With octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels or dialkyl silane bonded silica gel is filler; Methanol or acetonitrile-water-potassium dihydrogen phosphate or potassium dihydrogen phosphate or phosphoric acid or formic acid or acetic acid=5～50: 20～60: 0～5 is mobile phase; The detection wavelength is one or several among 190～410nm; Number of theoretical plate calculates by peoniflorin should be not less than 3000; Accurate respectively reference substance solution and each 1～30 μ l of need testing solution of drawing injects chromatograph of liquid, measures; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention;
K. the high performance liquid chromatography discrimination method of berberine hydrochloride in the preparation:
This preparation is an amount of before getting, and adds hydrochloric acid-methanol or ethanol=0～5: 100 solution extracts, the preparation need testing solution; Get the berberine hydrochloride reference substance, add above-mentioned solvent and make reference substance solution; With octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels or dialkyl silane bonded silica gel is filler; With water-potassium dihydrogen phosphate or potassium dihydrogen phosphate or phosphoric acid or formic acid or acetic acid-acetonitrile or methanol=0～60: be mobile phase at 0～5: 5～50; The detection wavelength is one or several among 190～410nm; Number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 2000; Accurate respectively reference substance solution and each 1～30 μ l of need testing solution of drawing injects chromatograph of liquid, measures; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention.
8. according to the method for quality control of the prostatitic pharmaceutical preparation of the described treatment of claim 7, it is characterized in that: the discrimination method of described preparation comprises following all or part of content:
A. one or both thin layer chromatography discrimination method in berberine hydrochloride, the Cortex Phellodendri in the preparation:
It is an amount of to get this preparation, the 20ml that adds diethyl ether, and supersound process 20 minutes discards ether solution, and medicinal residues volatilize, and add methanol 20ml, and supersound process 20 minutes filters, and filtrate is concentrated into 2ml, as need testing solution; Get the Cortex Phellodendri medical material, shine medical material solution in pairs with legal system; Other gets the berberine hydrochloride reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw one or both each the 5 μ l in above-mentioned need testing solution, reference substance or the control medicinal material solution, put respectively on same silica gel g thin-layer plate, with benzene-ethyl acetate-methanol-isopropyl alcohol-strong ammonia solution=4: 3: 2: be developing solvent at 1.5: 0.5, launches, take out, dry, put under the uviol lamp 365nm and inspect, in the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color;
B. one or both thin layer chromatography discrimination method in Radix Paeoniae Rubra, the peoniflorin in the preparation:
It is an amount of to get this preparation, gets content, adds ethanol 25ml, and supersound process 20 minutes filters, and filtrate evaporate to dryness, residue add ethanol 2ml makes dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin layer chromatography, draw one or both each the 5 μ l in above-mentioned need testing solution, reference substance or the control medicinal material solution, respectively with same silica gel g thin-layer plate on, with chloroform-ethyl acetate-methanol-formic acid=40: 5: 12: 0.2 was developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, 105 ℃ dry by the fire to the speckle colour developing clear; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color;
C. one or more thin layer chromatography discrimination method in Radix Salviae Miltiorrhizae, danshensu or its sodium salt, the protocatechualdehyde in the preparation:
It is an amount of to get this preparation, adds water 20ml, and ultrasonic 30 minutes, centrifugal, supernatant was regulated pH value to 2 with dilute hydrochloric acid, extracted with ethyl acetate 20ml jolting, and extracting solution evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Salviae Miltiorrhizae control medicinal material 0.5g, and it is an amount of to add water, decocts 30 minutes, adds water to 20ml, shines medical material solution in pairs with legal system; Get danshensu or its sodium salt, protocatechualdehyde, add methanol and make reference substance solution; Test according to thin layer chromatography, draw one or more each the 5 μ l in above-mentioned need testing solution, reference substance or the control medicinal material solution, put respectively on same silica gel g thin-layer plate, with chloroform-acetone-formic acid=25: 10: 4 was developing solvent, launch, take out, dry, spray is placed about 30 minutes to clear spot with 2% ferric chloride alcoholic solution; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color;
D. one or more thin layer chromatography discrimination method in Radix Salviae Miltiorrhizae, salvianolic acid B or its magnesium salt in the preparation:
It is an amount of to get this preparation, and 75% methanol jolting is extracted, and extracting solution concentrates, as need testing solution; Other gets the Radix Salviae Miltiorrhizae control medicinal material, shines medical material solution in pairs with legal system; Salvianolic acid B or its magnesium salt add 75% methanol and make reference substance solution; Test according to thin layer chromatography, draw one or both each the 5 μ l in above-mentioned need testing solution, reference substance or the control medicinal material solution, put respectively on same silica GF254 lamellae, with toluene-chloroform-ethyl acetate-methanol-formic acid=2: 3: 4: be developing solvent at 0.5: 2, launch, take out, dry, 254nm inspects under the uviol lamp; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color;
E. the thin layer chromatography discrimination method of the Radix Angelicae Dahuricae in the preparation:
It is an amount of to get this preparation, and content adds water 20ml, and ultrasonic 30 minutes, centrifugal, supernatant was regulated pH value to 12 with sodium hydroxide test solution, extracted with chloroform 20ml jolting, and extracting solution is concentrated into 1ml, as need testing solution; Other gets Radix Angelicae Dahuricae control medicinal material 0.5g, adds chloroform 10ml, and ultrasonic 30 minutes, filter, filtrate is concentrated into 1ml, in contrast medical material solution; According to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with chloroform-methanol=9: 1, put in the vapour-saturated expansion cylinder of ammonia, launch, taking-up is dried, and puts that 254nm inspects under the ultra-violet lamp; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
F. one or both thin layer chromatography discrimination method in Semen Persicae, the amygdaloside in the preparation:
It is an amount of to get this preparation, adds methanol 20ml supersound process 20min, filters, filtrate evaporate to dryness, residue add water 5ml slight fever makes dissolving, puts cold, D101 type macroporous adsorptive resins by the internal diameter 1.5cm of water 20m prewashing, long 8cm discards water liquid, with ammonia solution 30ml eluting, discard ammoniacal liquor, reuse water 10ml eluting discards water liquid, continue with 20% ethanol 30ml eluting, collect eluent, evaporate to dryness, residue add methanol 1ml makes dissolving as need testing solution; Get the Semen Persicae medical material, the 20ml that adds diethyl ether refluxes, and discards ether solution, adds methanol 20ml again and refluxes, and filters, and filtrate concentrates, in contrast medical material solution; Other gets the amygdaloside reference substance, adds methanol and makes the solution that every 1ml contains 2mg, in contrast product solution; Draw one or both each the 5 μ l in above-mentioned need testing solution, reference substance or the control medicinal material solution, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-water=15: 40: 22: 10 was developing solvent at 5～10 ℃ of lower floor's solution of placing 12h, launch, take out, spray immediately with the phosphomolybdic acid sulfuric acid solution, at 105 ℃ of about 10min of baking; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color;
G. one or both thin layer chromatography discrimination method in Herba Lycopi, the ursolic acid in the preparation:
It is an amount of to get this preparation, adds acetone 30ml, and supersound process 10 minutes is put coldly, filter, and the filtrate evaporate to dryness, residue soaks with petroleum ether 10ml, and the petroleum ether that inclines, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets Herba Lycopi's control medicinal material, shines medical material solution in pairs with legal system; Get the ursolic acid reference substance again, add dehydrated alcohol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw one or both each the 5 μ l in above-mentioned need testing solution, reference substance or the control medicinal material solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with cyclohexane extraction-chloroform-ethyl acetate-formic acid=20: 5: 8: 0.1 was developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the speckle of same color;
H. the high performance liquid chromatography discrimination method of protocatechualdehyde in the preparation:
It is an amount of to get this preparation, adds water 50ml, supersound process 30 minutes, take out, put, filter to room temperature, subsequent filtrate is regulated pH value to 2 with 10% hydrochloric acid, extracts 3 times with the ether jolting, each 10ml, merge ether extracted liquid, put evaporate to dryness in the water-bath, residue adds dissolve with methanol and standardize solution, filters with microporous filter membrane, get subsequent filtrate, as need testing solution; It is an amount of to get the protocatechualdehyde reference substance, puts in the brown measuring bottle, adds methanol and makes the solution that contains 12 μ g among every 1ml, in contrast product solution; With octadecylsilane chemically bonded silica is filler; Methanol-1% glacial acetic acid aqueous solution=13: 87 is a mobile phase; The detection wavelength is 281nm; Number of theoretical plate calculates by protocatechualdehyde should be not less than 2000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention;
I. the high performance liquid chromatography discrimination method of salvianolic acid B in the preparation:
It is an amount of to get this preparation, adds the methanol supersound process 30 minutes, takes out, and puts to room temperature, filters, as need testing solution; It is an amount of to get the salvianolic acid B reference substance, adds 75% methanol and makes reference substance solution; With octadecylsilane chemically bonded silica is filler; Methanol-acetonitrile-formic acid-water=30: 10: 1: 59 is mobile phase; The detection wavelength is 286nm; Number of theoretical plate calculates by salvianolic acid B should be not less than 2000; Draw each 10 μ l of reference substance solution and need testing solution respectively, inject chromatograph of liquid, measure; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention;
J. the high performance liquid chromatography discrimination method of peoniflorin in the preparation:
It is an amount of to get this preparation, adds the methanol supersound process 30 minutes, takes out, and puts to room temperature, filters, as need testing solution; It is an amount of to get the peoniflorin reference substance that is dried to constant weight, adds methanol and makes reference substance solution; With octadecylsilane chemically bonded silica is filler; Methanol-0.05mol/L potassium dihydrogen phosphate=40: 65 is mobile phase; The detection wavelength is 230nm; Number of theoretical plate calculates by peoniflorin should be not less than 3000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention;
K. the high performance liquid chromatography discrimination method of berberine hydrochloride in the preparation:
It is an amount of to get this preparation, adds the mixed solution supersound process 30 minutes of hydrochloric acid-methanol=1: 100, takes out, and puts to room temperature, supplies the solvent of loss, shakes up, and filters, and gets subsequent filtrate, is need testing solution; Get the berberine hydrochloride reference substance, add above-mentioned solvent and make reference substance solution; Regulating the 0.05mol/L sodium dihydrogen phosphate-acetonitrile of pH value to 3.0=75: 25 with phosphoric acid is mobile phase; The detection wavelength is 270nm; Number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 2000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure; In the test sample chromatograph, have the chromatographic peak consistent with the reference substance chromatographic retention.
9. according to the method for quality control of the prostatitic pharmaceutical preparation of the described treatment of claim 6, it is characterized in that: the content assaying method of described preparation comprises following all or part of content:
A. the high-efficient liquid phase chromatogram process measuring method of preparation Central Plains catechu aldehyde:
It is an amount of to get this preparation, and accurate the title decides, extracting in water, and water liquid prepares need testing solution with ether or ethyl acetate or chloroform jolting extraction; Or it is an amount of to get this preparation, adds 10～100% methanol or ethanol extraction, the preparation need testing solution; It is an amount of to get the protocatechualdehyde reference substance, adds 10～100% methanol or ethanol and is made as reference substance solution; With octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels or dialkyl silane bonded silica gel is filler; Methanol or acetonitrile-water-acetic acid or formic acid or phosphoric acid=10～50: 30～95: 0.01～5 is mobile phase; The detection wavelength is one or several among 190～410nm; Number of theoretical plate calculates by protocatechualdehyde should be not less than 2000; Accurate respectively reference substance solution and each 1～30 μ l of need testing solution of drawing injects chromatograph of liquid, measures, and calculates with one point external standard method or standard curve method; Content limit should be: must not be lower than 108 μ g with containing Radix Salviae Miltiorrhizae in this preparation in protocatechualdehyde on 1st;
B. the high-efficient liquid phase chromatogram process measuring method of content of danshinolic acid B in the preparation:
It is an amount of to get this preparation, and accurate the title decides, and adds 10～100% methanol or ethanol extraction, the preparation need testing solution; It is an amount of to get the salvianolic acid B reference substance, adds 10～100% methanol or ethanol and makes reference substance solution; With octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels or dialkyl silane bonded silica gel is filler; Methanol or ethanol-acetonitrile-formic acid or acetic acid or phosphoric acid-water=10～30: 0～30: 0～5: 50～95 is mobile phase; The detection wavelength is one or several among 190～410nm; Number of theoretical plate calculates by salvianolic acid B should be not less than 2000; Accurate respectively reference substance solution and each 1～30 μ l of need testing solution of drawing injects chromatograph of liquid, measures, and calculates with one point external standard method or standard curve method; Content limit should be: must not be lower than 10.8mg with containing Radix Salviae Miltiorrhizae in this preparation in salvianolic acid B on 1st;
C. the high-efficient liquid phase chromatogram process measuring method of paeoniflorin content in the preparation:
It is an amount of to get this preparation, and accurate the title decides, and adds 10～100% methanol or ethanol extraction, the preparation need testing solution; It is an amount of to get the peoniflorin reference substance, adds 10～100% methanol or ethanol and makes reference substance solution; With octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels or dialkyl silane bonded silica gel is filler; Methanol or acetonitrile-water-potassium dihydrogen phosphate or potassium dihydrogen phosphate or phosphoric acid or formic acid or acetic acid=5～50: 20～60: 0～5 is mobile phase; The detection wavelength is one or several among 190～410nm; Number of theoretical plate calculates by peoniflorin should be not less than 3000; Accurate respectively reference substance solution and each 1～30 μ l of need testing solution of drawing injects chromatograph of liquid, measures; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate with one point external standard method or standard curve method; Content limit should be: must not be lower than 13.2mg with containing Radix Paeoniae Rubra in this preparation in peoniflorin on 1st;
D. the high-efficient liquid phase chromatogram process measuring method of content of berberine hydrochloride in the preparation:
It is an amount of to get this preparation, and accurate the title decides, and adds hydrochloric acid-methanol=0～5: 100 solution extracts, the preparation need testing solution; Get the berberine hydrochloride reference substance, add above-mentioned solvent and make reference substance solution; With octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels or dialkyl silane bonded silica gel is filler; With water-potassium dihydrogen phosphate or potassium dihydrogen phosphate or phosphoric acid or formic acid or acetic acid-acetonitrile or methanol=20～60: be mobile phase at 0～5: 5～50; The detection wavelength is one or several among 190～410nm; Number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 2000; Accurate respectively reference substance solution and each 1～30 μ l of need testing solution of drawing injects chromatograph of liquid, measures, and calculates with one point external standard method or standard curve method; Content limit should be: must not be lower than 36mg with containing Cortex Phellodendri in this preparation in berberine hydrochloride on 1st.
10. according to the method for quality control of the prostatitic pharmaceutical preparation of the described treatment of claim 9, it is characterized in that: the content assaying method of described preparation comprises following all or part of content:
A. the high-efficient liquid phase chromatogram process measuring method of preparation Central Plains catechu aldehyde:
It is an amount of to get this preparation, and accurate the title decides, and puts in the tool plug conical flask, precision adds water 50ml, and weight, supersound process 30 minutes decided in accurate title, take out, put to room temperature, weight decided in accurate title, add water and supply the weight that subtracts mistake, shake up, filter, the accurate subsequent filtrate 10ml that draws, regulate pH value to 2 with 10% hydrochloric acid, extract 3 times, each 10ml with the ether jolting, merge ether extracted liquid, put evaporate to dryness in the water-bath, residue adds dissolve with methanol and quantitatively is transferred in the 10ml measuring bottle, adds methanol to scale, shake up, filter with microporous filter membrane, get subsequent filtrate, as need testing solution; It is an amount of to get the protocatechualdehyde reference substance, and accurate the title decides, and puts in the brown measuring bottle, adds methanol and makes the solution that contains 12 μ g among every 1ml, in contrast product solution; With octadecylsilane chemically bonded silica is filler; Methanol-1% glacial acetic acid aqueous solution=13: 87 is a mobile phase; The detection wavelength is 281nm; Number of theoretical plate calculates by protocatechualdehyde should be not less than 2000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate with one point external standard method, promptly; Content limit should be: must not be lower than 216 μ g with containing Radix Salviae Miltiorrhizae in this preparation in protocatechualdehyde on 1st;
B. the high-efficient liquid phase chromatogram process measuring method of content of danshinolic acid B in the preparation:
It is an amount of to get this preparation, and accurate the title decides, and adds the methanol supersound process 30 minutes, takes out, and puts to room temperature, and accurate the title decided weight, adds methanol and supplies the weight that subtracts mistake, shakes up, and filters, as need testing solution; It is an amount of to get the salvianolic acid B reference substance, and accurate the title decides, and adds 75% methanol and makes reference substance solution; With octadecylsilane chemically bonded silica is filler; Methanol-acetonitrile-formic acid-water=30: 10: 1: 59 is mobile phase; The detection wavelength is 286nm; Number of theoretical plate calculates by salvianolic acid B should be not less than 2000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate with one point external standard method, promptly; Content limit should be: must not be lower than 21.6mg with containing Radix Salviae Miltiorrhizae in this preparation in salvianolic acid B on 1st;
C. the high-efficient liquid phase chromatogram process measuring method of paeoniflorin content in the preparation:
It is an amount of to get this preparation, and accurate the title decides, and adds the methanol supersound process 30 minutes, takes out, and puts to room temperature, and accurate the title decided weight, adds methanol and supplies the weight that subtracts mistake, shakes up, and filters, as need testing solution; It is an amount of to get the peoniflorin reference substance that is dried to constant weight, and accurate the title decides, and adds methanol and makes reference substance solution; With octadecylsilane chemically bonded silica is filler; Methanol-0.05mol/L potassium dihydrogen phosphate=40: 65 is mobile phase; The detection wavelength is 230nm; Number of theoretical plate calculates by peoniflorin should be not less than 3000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate with one point external standard method, promptly; Content limit should be: must not be lower than 26.4mg with containing Radix Paeoniae Rubra in this preparation in peoniflorin on 1st;
D. the high-efficient liquid phase chromatogram process measuring method of content of berberine hydrochloride in the preparation:
It is an amount of to get this preparation, accurate claims surely, adds the mixed solution supersound process 30 minutes of hydrochloric acid-methanol=1: 100, takes out, and puts to room temperature, supplies the solvent of loss, shakes up, and filters, and gets subsequent filtrate, is need testing solution; Get the berberine hydrochloride reference substance, add above-mentioned solvent and make reference substance solution; Regulating the 0.05mol/L sodium dihydrogen phosphate-acetonitrile of pH value to 3.0=75: 25 with phosphoric acid is mobile phase; The detection wavelength is 270nm; Number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 2000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate with one point external standard method, promptly; Content limit should be: must not be lower than 72mg with containing Cortex Phellodendri in this preparation with berberine hydrochloride on 1st.
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| CN102526305A (en) * | 2012-02-14 | 2012-07-04 | 史志辉 | Chinese medicinal capsules for treating prostatitis and prostatic hyperplasia and preparation method for Chinese medicinal capsules |
| CN102818875A (en) * | 2011-06-10 | 2012-12-12 | 天津同仁堂集团股份有限公司 | Quality control method of vessel rehabilitation tablets |
| WO2013053187A1 (en) * | 2011-10-14 | 2013-04-18 | 西安千禾药业有限责任公司 | Detection method for traditional chinese medicine composition for treating acute and chronic prostatitis |
| CN103134896A (en) * | 2011-11-25 | 2013-06-05 | 张金荣 | Detection method for Chinese materia medica preparation for treating chronic prostatitis |
| CN105012994A (en) * | 2015-08-25 | 2015-11-04 | 东莞市达庆医疗器械有限公司 | Medical, functional and biological hydrogel dressing for urinary system and preparation method of hydrogel dressing |
| CN106511631A (en) * | 2016-10-25 | 2017-03-22 | 西安千禾药业股份有限公司 | Qianlieping preparation used for treating prostatitis and preparation method thereof |
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| CN102818875A (en) * | 2011-06-10 | 2012-12-12 | 天津同仁堂集团股份有限公司 | Quality control method of vessel rehabilitation tablets |
| WO2013053187A1 (en) * | 2011-10-14 | 2013-04-18 | 西安千禾药业有限责任公司 | Detection method for traditional chinese medicine composition for treating acute and chronic prostatitis |
| CN103134896A (en) * | 2011-11-25 | 2013-06-05 | 张金荣 | Detection method for Chinese materia medica preparation for treating chronic prostatitis |
| CN102526305A (en) * | 2012-02-14 | 2012-07-04 | 史志辉 | Chinese medicinal capsules for treating prostatitis and prostatic hyperplasia and preparation method for Chinese medicinal capsules |
| CN105012994A (en) * | 2015-08-25 | 2015-11-04 | 东莞市达庆医疗器械有限公司 | Medical, functional and biological hydrogel dressing for urinary system and preparation method of hydrogel dressing |
| CN107782816A (en) * | 2016-08-31 | 2018-03-09 | 天津中新药业研究中心 | A kind of detection method of clearing heat and detoxicating cool blood stranguria-treating drug |
| CN106511631A (en) * | 2016-10-25 | 2017-03-22 | 西安千禾药业股份有限公司 | Qianlieping preparation used for treating prostatitis and preparation method thereof |
| CN107884508A (en) * | 2017-04-16 | 2018-04-06 | 湖南安邦制药有限公司 | The quality determining method of Yinhuang lung clearing capsule |
| CN107884508B (en) * | 2017-04-16 | 2021-01-12 | 湖南安邦制药有限公司 | Quality detection method of Yinhuang lung-clearing capsule |
| CN109406707A (en) * | 2018-11-29 | 2019-03-01 | 四川新绿色药业科技发展有限公司 | A kind of TLC Identification of stir-baked SEMEN PERSICAE and its preparation |
| CN113834895A (en) * | 2021-08-28 | 2021-12-24 | 海南葫芦娃药业集团股份有限公司 | Quality control method of amygdalin in infantile lung heat cough and asthma granules |
| CN113834895B (en) * | 2021-08-28 | 2023-02-24 | 海南葫芦娃药业集团股份有限公司 | Quality control method of amygdalin in infantile lung heat cough and asthma granules |
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| CN100582774C (en) | 2010-01-20 |
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