CN1698758A - Pharmaceutical preparation of bastardtoad flax and its preparation method and quality control method - Google Patents
Pharmaceutical preparation of bastardtoad flax and its preparation method and quality control method Download PDFInfo
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Abstract
The invention relates to a pharmaceutical preparation of bastardtoad flax and its preparation method and quality control method, wherein the preparation is prepared from Thesium chinense Turcz. The preparation can be made into various dosage forms including drop pills, it has the effects of reducing fever, anti-inflammation, cough-relieving and phlegm resolving.
Description
Technical field: the present invention is a kind of hundred stamen pharmaceutical preparatioies and preparation method thereof and its method of quality control, belongs to technical field of Chinese medicine.
Background technology: Herba Thesii has heat clearing and inflammation relieving, effects such as relieving cough and resolving phlegm; Be used for acute and chronic pharyngolaryngitis, tracheitis, rhinitis, cold, fever, pneumonia etc.The product that has gone on the market has capsule and tablet, but the dosage form of these two kinds of products is relatively backward, absorbing of medicine is relatively poor, so have researcher such as number of patent application to be called " hydrochloric acid Herba Thesii intravenous drip liquid, injection and processing technology " for " 03110877.6 ", name, number of patent application is that " 03110953.5 ", name are called " hydrochloric acid BAIRUI JUJUEBIAN and processing technology ", and number of patent application be that " 200410023041.9 ", name are called in the patent of " BAIRUI FENSANPIAN and manufacture method " and ask; Though injection bioavailability height is to use inconvenience, untoward reaction is many, and danger coefficient is big, the cost height; The chewable tablet mouthfeel is relatively poor; Dispersible tablet is owing to need a large amount of disintegrating agents, cost height; In view of such circumstances, in order to improve stability of drug, need a kind of therapeutic effect ideal of searching, reliable in quality, the reasonably effective medicine preparation of dosage form to enrich the dosage form kind, satisfy market demand.
Summary of the invention: the objective of the invention is to:, provide hundred stamen pharmaceutical preparatioies and preparation method thereof and its method of quality control at prior art; The method of quality control that needs in drop pill with characteristics such as covering bitterness, easy to carry, good mouthfeel, absorption are fast, steady quality and the production process particularly is provided.
The present invention constitutes like this: it is mainly by Herba Thesii 400-800g or the 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 or the membrane that are made with the extract of corresponding weight portion.Say accurately: described preparation is a drop pill.
The preparation method of hundred stamen pharmaceutical preparatioies of the present invention: get Herba Thesii, add the decocting that 5-12 doubly measures and boil 1-3 time, each 1-3 hour, collecting decoction filters, and filtrate concentrates, add ethanol precipitation 1-3 time, make to contain alcohol amount and reach 60-95%, stir evenly, leave standstill, filter, filtrate recycling ethanol concentrates, and makes different preparations then respectively.
Drop pill of the present invention is preparation like this: get Herba Thesii, the decocting that adds 10 times of amounts boils secondary, each 2 hours, collecting decoction, filter, filtrate concentrates, and adds ethanol and makes and contain the alcohol amount and reach 70%, stir evenly, left standstill 24 hours, and filtered filtrate recycling ethanol, with the Macrogol 4000 is substrate, according to medicine: the part by weight of substrate=1: 4 adds Macrogol 4000, mixing, and the employing internal diameter is 4.0mm, external diameter is the dropper of 6.0mm, drip 70 ℃ of system temperature, dripping speed is 25～30d/min, dripping distance is 5cm, splashing in the long cooling column of 120cm, is liquid coolant again with the methyl-silicone oil, and adopt the gradient cooling: the Temperature Distribution of gradient liquid coolant is 40 ℃～50 ℃, 10 ℃～30 ℃, 0 ℃～4 ℃, pill, promptly.
Specifically, drop pill of the present invention is like this preparation: get Herba Thesii, decoct with water secondary, and 2 hours for the first time, 1.5 hours for the second time, filter, merging filtrate, concentrating under reduced pressure is put coldly, adds doubling dose 75% ethanol, stirs evenly; Add equivalent ethanol again, stir evenly.After leaving standstill 12 hours, the leaching supernatant, reclaim ethanol, concentrating under reduced pressure, with the Macrogol 4000 is substrate, according to medicine: the part by weight of substrate=1: 4 adds Macrogol 4000, mixing, the employing internal diameter is that 4.0mm, external diameter are the dropper of 6.0mm, and dripping system temperature 70 ℃, droplet speed is that 25～30d/min, a distance are 5cm, splashes in the long cooling column of 120cm, be liquid coolant again with the methyl-silicone oil, the cooling of employing gradient: the Temperature Distribution of gradient liquid coolant is 40 ℃～50 ℃, 10 ℃～30 ℃, 0 ℃～4 ℃, pill, promptly.
More specifically: drop pill of the present invention is preparation like this: get Herba Thesii, decoct with water 1.5 hours, filter, filtrate concentrates, put coldly, successively add 70% by concentrated solution weight, each one times of amount of 95% ethanol stirs evenly, leave standstill, get supernatant, filter filtrate decompression, with the Macrogol 4000 is substrate, according to medicine: the part by weight of substrate=1: 4 adds Macrogol 4000, mixing, and the employing internal diameter is 4.0mm, external diameter is the dropper of 6.0mm, drip 70 ℃ of system temperature, dripping speed is 25～30d/min, dripping distance is 5cm, splashing in the long cooling column of 120cm, is liquid coolant again with the methyl-silicone oil, and adopt the gradient cooling: the Temperature Distribution of gradient liquid coolant is 40 ℃～50 ℃, 10 ℃～30 ℃, 0 ℃～4 ℃, pill, promptly.
The method of quality control of hundred stamen pharmaceutical preparatioies comprises assay, differentiates etc.; Assay is an index with nimbecetin, total flavones, differentiates and adopts physics and chemistry and thin layer to differentiate.
Assay is such:
(1) with methanol: 0.5% phosphoric acid=60: 40 is mobile phase; The detection wavelength is 368nm; It is an amount of that precision takes by weighing the nimbecetin reference substance, adds methanol and make the solution that every 1ml contains nimbecetin 10 μ g, promptly gets reference substance solution; Get 20 of this product, the accurate title, decide, and porphyrize is got 1g, and accurate title is fixed, adds 70% ethanol 30ml, 25% hydrochloric acid 5ml, water-bath refluxed 1 hour, put coldly, quantitatively was transferred in the 100ml measuring bottle, added 70% ethanol dilution to scale, shake up, filter, get subsequent filtrate, centrifugal, promptly get need testing solution; Accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly;
(2) precision takes by weighing at the control substance of Rutin 15mg of 120 ℃ of drying under reduced pressure to constant weight, puts in the 100ml measuring bottle, with dissolve with methanol and be diluted to scale, shakes up, and promptly gets the reference substance solution that contains anhydrous rutin 0.15mg among every 1ml; Reference substance solution 1.0,2.0,3.0,4.0 and 5.0ml are measured in the preparation of standard curve, precision, put respectively in the 25ml measuring bottle, respectively add methanol to 5.0ml, add 10% aluminum trichloride solution 1.0ml, shake up, add acetic acid-sodium-acetate buffer pH55.0ml, ethanol 10.0ml, shake up, add water to scale, shake up, placed 15 minutes, and, measured trap at the wavelength place of 405nm according to spectrophotography, with the trap is that vertical coordinate, concentration are abscissa, the drawing standard curve chart; Get this product content, porphyrize, precision takes by weighing 1.5g, puts in the apparatus,Soxhlet's, adds an amount of ether, reflux 4 hours discards ether solution, and medicinal residues are waved most ether, adds an amount of methanol again, reflux moves in the 100ml measuring bottle till the extracting liquid colourless, adds methanol to scale, shakes up; Precision is measured each 5ml, put respectively in two 25ml measuring bottles of first, second, add 10% aluminum trichloride solution 1.0ml in the first bottle, shake up, in two bottles, add acetic acid sodium-acetate buffer (pH5) 5.0ml and ethanol 10.0ml then respectively, add water to scale, shake up, placing 15 minutes, is blank with the second bottle, measures trap at 405nm wavelength place.Read the amount of rutin the need testing solution from standard curve, calculate, promptly.
Discriminating is such:
(1) get this product, porphyrize is put in the tool plug conical flask, add methanol 20ml, flooded 1 hour, constantly vibration, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, add hydrochloric acid 2ml, reflux 1 hour, cooling immediately, with ether extraction 2 times, each 25ml merges ether extracted liquid, volatilize, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets Herba Thesii control medicinal material 1g, shines medical material solution in pairs with legal system.Get the nimbecetin reference substance again, add methanol 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 three kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene: Ethyl formate: formic acid=5: 4: 1 is developing solvent, launches, take out, dry, put under the daylight and inspect, in the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color; Put ultra-violet lamp 365nm and observe down, in the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show identical color fluorescence speckle;
(2) get this product, porphyrize adds methanol 30ml, and reflux, extract, 1 hour filters, and filtrate is put and is concentrated into about 5ml in the water-bath, as need testing solution; Other gets Herba Thesii control medicinal material 3g, shines medical material solution in pairs with legal system; According to thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate: formic acid: water=8: 1: 1 is developing solvent, launch, take out, dry, spray, is put under the ultra-violet lamp 365nm and is inspected after waiting to do with the aluminum chloride test solution; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
(3) get this product, porphyrize adds methanol 20ml, warm 15 minutes, filters; Get each 1ml of filtrate, split in two test tubes, add in the pipe that magnesium powder is a small amount of to drip with the salt acid number, show redness; Add 1 of liquor ferri trichloridi in another pipe, show crineous.
Compared with prior art, hundred stamen pharmaceutical preparatioies provided by the invention and preparation method thereof and its method of quality control; The method of quality control that needs in drop pill with characteristics such as covering bitterness, easy to carry, good mouthfeel, absorption are fast, steady quality and the production process particularly is provided.That its drop pill has is easy to carry, cover bitterness, characteristics such as absorbing soon can be good, good anti-moisture ability; Product has overcome the problem that prior art, product exist, and product has heat clearing and inflammation relieving, effects such as relieving cough and resolving phlegm; Be used for acute and chronic pharyngolaryngitis, tracheitis, rhinitis, cold, fever, pneumonia etc.; The method of quality control that is provided has solved in the actual production process for the problem of the quality control of product, the quality of product is effectively guaranteed; Reached the purpose of invention.
The applicant finds under study for action: the factor that influences drop pill preparation among the present invention has many aspects, as medicine, substrate, coolant, temperature, drip apart from, drip in speed, the type of cooling, the drip external diameter etc.The applicant weighs the influence that each factor has been investigated in two aspects from roundness and the ball that influences drop pill, establishing the optimum condition of preparation preparation drop pill of the present invention, the supplementary product kind of preparation process condition, use of the most suitable this product and consumption, ratio etc. have been found by experiment; Guarantee its science, reasonable, feasible; The preparation that obtains has superperformance and therapeutic effect.
Experimental example 1: craft screening
1. the proportioning of medicine and substrate
Medicine and substrate (Macrogol 4000) proportioning
Medicine and substrate composition merge the situation denseness and drip the system situation
1: 1 difficult thick difficulty
1: 2 easy moderate difficulty
1: 3 easy moderate difficulty
1: 4 easily rare easy
1: 5 easily rare easy
2. the coolant and the type of cooling are selected
The coolant and the type of cooling are selected: with methyl-silicone oil, liquid paraffin is coolant, and medicine and substrate were dripped system in 1: 4 behind the ratio mixing.Drip the system condition: system is dripped in (80 ± 2) ℃ insulation, and the drip internal diameter is 4.0mm, external diameter 6.0mm.Coolant temperature adopts gradient or non-gradient mode, and the gradient chilling temperature is distributed as: 40 ℃～50 ℃, 10 ℃～30 ℃, 0 ℃～4 ℃ (3 temperature-averagings are cut apart the length of cooling column), non-gradient is cooled to 0 ℃～10 ℃.Dripping speed is 20～30/min.Evaluation index: the roundness of drop pill (the minor axis of drop pill/major diameter＞0.8) qualification rate.
Group coolant cools mode cooling column height/cm roundness qualification rate/%
1 methyl-silicone oil gradient 120 90.3 90.1
The non-gradient 140 86.1 82.5 of 2 methyl-silicone oils
3 liquid paraffin gradients 140 75.8 70.9
The non-gradient 120 73.2 72.4 of 4 liquid paraffin
3. drip distance, drip selection fast, temperature
Drip distance, drip selection fast, temperature: the interior external diameter of drip is fixed as 4.1,6.1mm.Evaluation index: the heavy qualification rate of ball is by mass discrepancy requirement of Pharmacopoeia of the People's Republic of China version in 2000: meet ± 7.5% within.
Group temperature/℃ drip a distance/cm drips the ball weight qualification rate/% of speed/(dmin-1)
1 90 5 10～20 79.2
2 90 7 20～25 86.1
3 90 9 25～30 82.0
4 80 5 20～25 67.2
5 80 7 25～30 85.4
6 80 9 10～20 90.2
7 70 5 25～30 93.7
8 70 7 10～20 95.4
9 70 9 20～25 84.8
The result shows, the optimum condition of preparation drop pill of the present invention: with the Macrogol 4000 is substrate, according to medicine: the part by weight of substrate=1: 4 adds Macrogol 4000, mixing, the employing internal diameter is that 4.0mm, external diameter are the dropper of 6.0mm, and dripping system temperature 70 ℃, droplet speed is that 25～30d/min, a distance are 5cm, splashes in the long cooling column of 120cm, be liquid coolant again with the methyl-silicone oil, adopt the gradient cooling: the Temperature Distribution of gradient liquid coolant is 40 ℃～50 ℃, 10 ℃～30 ℃, 0 ℃～4 ℃.
Experimental example 2: pharmacodynamic experiment
1, the influence of xylol induced mice auricle edema
Get 40 of mices, male and female half and half, body weight 20 ± 2g is divided into matched group at random, BAIRUI HANPIAN group, BAIRUI JIAONANG group, drop pill group of the present invention.Irritate stomach 0.5ml/d respectively for every group, be equivalent to medicine 0.24g/kg, matched group gavages distilled water 0.5ml.Successive administration 5d, behind the last administration 1h, every mice left side ear is coated with the 0.05ml caused by dimethylbenzene xylene and swells, and auris dextra is made normal control, puts to death mice behind the 1h, and deducting auris dextra weight with left ear weight is the swelling degree, and the antiinflammatory action of comparative drug the results are shown in following table.
The influence of table 1 xylol induced mice auricle edema
Group dosage (g/kg) swelling degree suppression ratio %
Matched group---0.91 ± 0.38
BAIRUI HANPIAN group 0.24 0.51 ± 0.21 43.96
BAIRUI JIAONANG group 0.24 0.48 ± 0.16 47.25
Drop pill group 0.24 0.50 ± 0.31 45.05 of the present invention
2, to the influence of the phenol red secretory volume of mice trachea
Get 40 of mices, male and female half and half, body weight 20 ± 2g is divided into matched group at random, BAIRUI PIAN group, BAIRUI JIAONANG group, drop pill group of the present invention.After water 12h is can't help in fasting, irritate stomach medicinal liquid 0.5ml respectively for every group, matched group gavages distilled water 0.5ml.Behind the gastric infusion 0.5h, ip phenol red solution 0.2ml/10g, injection back 0.5h blocks the mice mouth and nose with wet cloth, makes its death by suffocation.It is fixing that mice is faced upward the position, peels off trachea, clamps from thyroid cartilage one section trachea to the trachea bifurcation and cut with small artery, puts into the test tube that fills the 2ml normal saline, adds 0.1mlNaOH again, its trap value of usefulness spectrophotometric determination.Calculate phenol red content (ng/ml) according to standard curve again.The results are shown in following table.
The influence of the table 2 pair phenol red secretory volume of mice trachea
The phenol red secretory volume of group dosage (g/kg) (ng/ml)
Matched group---9.51 ± 5.68
BAIRUI PIAN agent group 0.24 17.25 ± 10.51
BAIRUI JIAONANG group 0.24 21.09 ± 8.95
Drop pill group 0.24 26.74 ± 3.15 of the present invention
The influence of 3, mice ammonia being drawn the effect of coughing
Get 40 of mices, male and female half and half, body weight 20 ± 2g is divided into matched group at random, BAIRUI FENSANPIAN group, BAIRUI JUJUEBIAN group, drop pill group of the present invention.After water 12h is can't help in fasting, irritate stomach medicinal liquid 0.5ml respectively for every group, matched group gavages distilled water 0.5ml.Behind the gastric infusion 0.5h, respectively 5 mices (respectively organizing 1) are put in the 3000ml sealed glass container each all constant-pressure atomization strong aqua ammonia (25%～28%NH
4OH) 30s stimulation mice causes and coughs, and animal is rested on 30s in the container, takes out animal, number of observation/min and incubation period, the results are shown in following table.
Table 3 pair mice ammonia draws the influence of the effect of coughing
Group dosage (g/kg) cough number of times (/min) cough latent period (s)
Matched group---32.18 ± 8.74 12.75 ± 9.66
BAIRUI FENSANPIAN group 0.24 16.24 ± 6.05 26.02 ± 4.91
BAIRUI JUJUEBIAN group 0.24 18.57 ± 4.39 22.84 ± 6.34
Drop pill group 0.24 14.91 ± 5.33 32.70 ± 9.15 of the present invention
The result shows: product of the present invention can obviously suppress auricle edema effect due to the dimethylbenzene, can improve the phenol red excretion of mice trachea, and the mice strong aqua ammonia drawn to cough all significant antitussive action, can significantly reduce mice per minute cough number of times and increase the incubation period of coughing, and effect is better than the existing preparation of hundred commercially available stamens.
Concrete embodiment:
Embodiments of the invention 1: Herba Thesii 630g
Get Herba Thesii, the decocting that adds 10 times of amounts boils secondary, each 2 hours, collecting decoction filters, and filtrate concentrates, adding ethanol makes and contains alcohol amount and reach 70%, stir evenly, left standstill 24 hours, filter, filtrate recycling ethanol, with the Macrogol 4000 is substrate, and according to medicine: the part by weight of substrate=1: 4 adds Macrogol 4000, mixing, the employing internal diameter is 4.0mm, external diameter is the dropper of 6.0mm, drip 70 ℃ of system temperature, dripping speed is 25～30d/min, dripping apart from being 5cm, splash in the long cooling column of 120cm, is liquid coolant again with the methyl-silicone oil, the cooling of employing gradient: the Temperature Distribution of gradient liquid coolant is 40 ℃～50 ℃, 10 ℃～30 ℃, 0 ℃～4 ℃, pill promptly gets drop pill, this product oral, three times on the one, each 2.
Embodiments of the invention 2: Herba Thesii 630g
Get Herba Thesii, decoct with water secondary, 2 hours for the first time, 1.5 hours for the second time, filter, merging filtrate, concentrating under reduced pressure is put coldly, adds doubling dose 75% ethanol, stirs evenly; Add equivalent ethanol again, stir evenly.After leaving standstill 12 hours, the leaching supernatant, reclaim ethanol, concentrating under reduced pressure, with the Macrogol 4000 is substrate, according to medicine: the part by weight of substrate=1: 4 adds Macrogol 4000, mixing, the employing internal diameter is that 4.0mm, external diameter are the dropper of 6.0mm, and dripping system temperature 70 ℃, droplet speed is that 25～30d/min, a distance are 5cm, splashes in the long cooling column of 120cm, be liquid coolant again with the methyl-silicone oil, the cooling of employing gradient: the Temperature Distribution of gradient liquid coolant is 40 ℃～50 ℃, 10 ℃～30 ℃, 0 ℃～4 ℃, and pill promptly gets drop pill.
Embodiments of the invention 3: Herba Thesii 630g
Get Herba Thesii, decoct with water 1.5 hours, filter, filtrate concentrates, put coldly, successively add 70% by concentrated solution weight, each one times of amount of 95% ethanol stirs evenly, leave standstill, get supernatant, filter filtrate decompression, with the Macrogol 4000 is substrate, according to medicine: the part by weight of substrate=1: 4 adds Macrogol 4000, mixing, and the employing internal diameter is 4.0mm, external diameter is the dropper of 6.0mm, drip 70 ℃ of system temperature, dripping speed is 25～30d/min, dripping distance is 5cm, splashing in the long cooling column of 120cm, is liquid coolant again with the methyl-silicone oil, and adopt the gradient cooling: the Temperature Distribution of gradient liquid coolant is 40 ℃～50 ℃, 10 ℃～30 ℃, 0 ℃～4 ℃, pill promptly gets drop pill.
Embodiments of the invention 4: Herba Thesii 400g
Get Herba Thesii, the decocting that adds 5 times of amounts boiled 1 hour, and collecting decoction filters, and filtrate concentrates, and adds ethanol precipitation, made to contain the alcohol amount and reach 60%, stirred evenly, and left standstill, and filtered, and filtrate recycling ethanol concentrates, and filtrate is condensed into thick paste, adds carbomer, makes gel.
Embodiments of the invention 5: Herba Thesii 800g
Get Herba Thesii, the decocting that adds 12 times of amounts boils 3 times, and each 3 hours, collecting decoction filtered, and filtrate concentrates, add ethanol precipitation 3 times, make to contain alcohol amount and reach 95%, stir evenly, leave standstill, filter, filtrate recycling ethanol concentrates, and adds sodium carboxymethyl cellulose, and tabletting is made dispersible tablet.
Embodiments of the invention 6: assay
(1) with methanol: 0.5% phosphoric acid=60: 40 is mobile phase; The detection wavelength is 368nm; It is an amount of that precision takes by weighing the nimbecetin reference substance, adds methanol and make the solution that every 1ml contains nimbecetin 10 μ g, promptly gets reference substance solution; Get 20 of this product, the accurate title, decide, and porphyrize is got 1g, and accurate title is fixed, adds 70% ethanol 30ml, 25% hydrochloric acid 5ml, water-bath refluxed 1 hour, put coldly, quantitatively was transferred in the 100ml measuring bottle, added 70% ethanol dilution to scale, shake up, filter, get subsequent filtrate, centrifugal, promptly get need testing solution; Accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly;
(2) precision takes by weighing at the control substance of Rutin 15mg of 120 ℃ of drying under reduced pressure to constant weight, puts in the 100ml measuring bottle, with dissolve with methanol and be diluted to scale, shakes up, and promptly gets the reference substance solution that contains anhydrous rutin 0.15mg among every 1ml; Reference substance solution 1.0,2.0,3.0,4.0 and 5.0ml are measured in the preparation of standard curve, precision, put respectively in the 25ml measuring bottle, respectively add methanol to 5.0ml, add 10% aluminum trichloride solution 1.0ml, shake up, add acetic acid-sodium-acetate buffer pH55.0ml, ethanol 10.0ml, shake up, add water to scale, shake up, placed 15 minutes, and, measured trap at the wavelength place of 405nm according to spectrophotography, with the trap is that vertical coordinate, concentration are abscissa, the drawing standard curve chart; Get this product content, porphyrize, precision takes by weighing 1.5g, puts in the apparatus,Soxhlet's, adds an amount of ether, reflux 4 hours discards ether solution, and medicinal residues are waved most ether, adds an amount of methanol again, reflux moves in the 100ml measuring bottle till the extracting liquid colourless, adds methanol to scale, shakes up; Precision is measured each 5ml, put respectively in two 25ml measuring bottles of first, second, add 10% aluminum trichloride solution 1.0ml in the first bottle, shake up, in two bottles, add acetic acid sodium-acetate buffer (pH5) 5.0ml and ethanol 10.0ml then respectively, add water to scale, shake up, placing 15 minutes, is blank with the second bottle, measures trap at 405nm wavelength place.Read the amount of rutin the need testing solution from standard curve, calculate, promptly.
Embodiments of the invention 7: differentiate
(1) get this product, porphyrize is put in the tool plug conical flask, add methanol 20ml, flooded 1 hour, constantly vibration, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, add hydrochloric acid 2ml, reflux 1 hour, cooling immediately, with ether extraction 2 times, each 25ml merges ether extracted liquid, volatilize, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets Herba Thesii control medicinal material 1g, shines medical material solution in pairs with legal system.Get the nimbecetin reference substance again, add methanol 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 three kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene: Ethyl formate: formic acid=5: 4: 1 is developing solvent, launches, take out, dry, put under the daylight and inspect, in the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color; Put ultra-violet lamp 365nm and observe down, in the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show identical color fluorescence speckle;
(2) get this product, porphyrize adds methanol 30ml, and reflux, extract, 1 hour filters, and filtrate is put and is concentrated into about 5ml in the water-bath, as need testing solution; Other gets Herba Thesii control medicinal material 3g, shines medical material solution in pairs with legal system; According to thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate: formic acid: water=8: 1: 1 is developing solvent, launch, take out, dry, spray, is put under the ultra-violet lamp 365nm and is inspected after waiting to do with the aluminum chloride test solution; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
(3) get this product, porphyrize adds methanol 20ml, warm 15 minutes, filters; Get each 1ml of filtrate, split in two test tubes, add in the pipe that magnesium powder is a small amount of to drip with the salt acid number, show redness; Add 1 of liquor ferri trichloridi in another pipe, show crineous.
Claims (9)
1, hundred stamen pharmaceutical preparatioies is characterized in that: it mainly 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 or membrane with Herba Thesii 400-800g or with the extract of corresponding weight portion.
2, according to the described hundred stamen pharmaceutical preparatioies of claim 1, it is characterized in that: be made into dropping pill formulation with Herba Thesii or its extract.
3, the preparation method of hundred stamen pharmaceutical preparatioies as claimed in claim 1 or 2 is characterized in that: get Herba Thesii, add the decocting that 5-12 doubly measures and boil 1-3 time, each 1-3 hour, collecting decoction filtered, filtrate concentrates, and adds ethanol precipitation 1-3 time, makes to contain alcohol and measure and reach 60-95%, stir evenly, leave standstill, filter filtrate recycling ethanol, concentrate, make different preparations then respectively.
4, preparation method according to the described hundred stamen pharmaceutical preparatioies of claim 3, it is characterized in that: drop pill of the present invention is preparation like this: get Herba Thesii, the decocting that adds 10 times of amounts boils secondary, each 2 hours, collecting decoction filtered, filtrate concentrates, add ethanol and make and contain alcohol amount and reach 70%, stir evenly, left standstill 24 hours, filter, filtrate recycling ethanol is a substrate with the Macrogol 4000, and according to medicine: the part by weight of substrate=1: 4 adds Macrogol 4000, mixing, the employing internal diameter is 4.0mm, external diameter is the dropper of 6.0mm, drips 70 ℃ of system temperature, dripping speed is 25～30d/min, drip apart from being 5cm, splash in the long cooling column of 120cm, be liquid coolant again with the methyl-silicone oil, the cooling of employing gradient: the Temperature Distribution of gradient liquid coolant is 40 ℃～50 ℃, 10 ℃～30 ℃, 0 ℃～4 ℃, pill, promptly.
5, according to the preparation method of claim 3 or 4 described hundred stamen pharmaceutical preparatioies, it is characterized in that: drop pill of the present invention is preparation like this: get Herba Thesii, decoct with water secondary, 2 hours for the first time, 1.5 hours for the second time, filter, merging filtrate, concentrating under reduced pressure is put cold, add doubling dose 75% ethanol, stir evenly; Add equivalent ethanol again, stir evenly, after leaving standstill 12 hours, the leaching supernatant, reclaim ethanol, concentrating under reduced pressure is a substrate with the Macrogol 4000, and according to medicine: the part by weight of substrate=1: 4 adds Macrogol 4000, mixing, the employing internal diameter is that 4.0mm, external diameter are the dropper of 6.0mm, and dripping system temperature 70 ℃, droplet speed is that 25～30d/min, a distance are 5cm, splashes in the long cooling column of 120cm, be liquid coolant again with the methyl-silicone oil, the cooling of employing gradient: the Temperature Distribution of gradient liquid coolant is 40 ℃～50 ℃, 10 ℃～30 ℃, 0 ℃～4 ℃, pill, promptly.
6, preparation method according to the described hundred stamen pharmaceutical preparatioies of claim 3, it is characterized in that: drop pill of the present invention is preparation like this: get Herba Thesii, decoct with water 1.5 hours, filter, filtrate concentrates, and puts cold, successively add 70% by concentrated solution weight, each one times of amount of 95% ethanol, stir evenly, leave standstill, get supernatant, filter, filtrate decompression is a substrate with the Macrogol 4000, and according to medicine: the part by weight of substrate=1: 4 adds Macrogol 4000, mixing, the employing internal diameter is 4.0mm, external diameter is the dropper of 6.0mm, drips 70 ℃ of system temperature, dripping speed is 25～30d/min, drip apart from being 5cm, splash in the long cooling column of 120cm, be liquid coolant again with the methyl-silicone oil, the cooling of employing gradient: the Temperature Distribution of gradient liquid coolant is 40 ℃～50 ℃, 10 ℃～30 ℃, 0 ℃～4 ℃, pill, promptly.
7, the method for quality control of hundred stamen pharmaceutical preparatioies as claimed in claim 1 or 2, it comprises assay, differentiates etc.; It is characterized in that: the assay in the quality control is an index with nimbecetin, total flavones, differentiates and adopts physics and chemistry and thin layer to differentiate.
8, according to the method for quality control of the described hundred stamen pharmaceutical preparatioies of claim 7, it is characterized in that: assay is such:
(1) with methanol: 0.5% phosphoric acid=60: 40 is mobile phase; The detection wavelength is 368nm; It is an amount of that precision takes by weighing the nimbecetin reference substance, adds methanol and make the solution that every 1ml contains nimbecetin 10 μ g, promptly gets reference substance solution; Get 20 of this product, the accurate title, decide, and porphyrize is got 1g, and accurate title is fixed, adds 70% ethanol 30ml, 25% hydrochloric acid 5ml, water-bath refluxed 1 hour, put coldly, quantitatively was transferred in the 100ml measuring bottle, added 70% ethanol dilution to scale, shake up, filter, get subsequent filtrate, centrifugal, promptly get need testing solution; Accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly;
(2) precision takes by weighing at the control substance of Rutin 15mg of 120 ℃ of drying under reduced pressure to constant weight, puts in the 100ml measuring bottle, with dissolve with methanol and be diluted to scale, shakes up, and promptly gets the reference substance solution that contains anhydrous rutin 0.15mg among every 1ml; Reference substance solution 1.0,2.0,3.0,4.0 and 5.0ml are measured in the preparation of standard curve, precision, put respectively in the 25ml measuring bottle, respectively add methanol to 5.0ml, add 10% aluminum trichloride solution 1.0ml, shake up, add acetic acid-sodium-acetate buffer pH5 5.0ml, ethanol 10.0ml, shake up, add water to scale, shake up, placed 15 minutes, and, measured trap at the wavelength place of 405nm according to spectrophotography, with the trap is that vertical coordinate, concentration are abscissa, the drawing standard curve chart; Get this product content, porphyrize, precision takes by weighing 1.5g, puts in the apparatus,Soxhlet's, adds an amount of ether, reflux 4 hours discards ether solution, and medicinal residues are waved most ether, adds an amount of methanol again, reflux moves in the 100ml measuring bottle till the extracting liquid colourless, adds methanol to scale, shakes up; Precision is measured each 5ml, put respectively in two 25ml measuring bottles of first, second, add 10% aluminum trichloride solution 1.0ml in the first bottle, shake up, in two bottles, add sodium-acetate buffer 5.0ml and the ethanol 10.0ml of acetic acid pH=5 then respectively, add water to scale, shake up, placing 15 minutes, is blank with the second bottle, measures trap at 405nm wavelength place.Read the amount of rutin the need testing solution from standard curve, calculate, promptly.
9, according to the method for quality control of the described hundred stamen pharmaceutical preparatioies of claim 7, it is characterized in that: discriminating is such:
(1) get this product, porphyrize is put in the tool plug conical flask, add methanol 20ml, flooded 1 hour, constantly vibration, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, add hydrochloric acid 2ml, reflux 1 hour, cooling immediately, with ether extraction 2 times, each 25ml merges ether extracted liquid, volatilize, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets Herba Thesii control medicinal material 1g, shines medical material solution in pairs with legal system; Get the nimbecetin reference substance again, add methanol 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 three kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene: Ethyl formate: formic acid=5: 4: 1 is developing solvent, launches, take out, dry, put under the daylight and inspect, in the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color; Put ultra-violet lamp 365nm and observe down, in the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show identical color fluorescence speckle;
(2) get this product, porphyrize adds methanol 30ml, and reflux, extract, 1 hour filters, and filtrate is put and is concentrated into about 5ml in the water-bath, as need testing solution; Other gets Herba Thesii control medicinal material 3g, shines medical material solution in pairs with legal system; According to thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate: formic acid: water=8: 1: 1 is developing solvent, launch, take out, dry, spray, is put under the ultra-violet lamp 365nm and is inspected after waiting to do with the aluminum chloride test solution; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
(3) get this product, porphyrize adds methanol 20ml, warm 15 minutes, filters; Get each 1ml of filtrate, split in two test tubes, add in the pipe that magnesium powder is a small amount of to drip with the salt acid number, show redness; Add 1 of liquor ferri trichloridi in another pipe, show crineous.
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| CN 200510049768 CN1698758A (en) | 2005-05-09 | 2005-05-09 | Pharmaceutical preparation of bastardtoad flax and its preparation method and quality control method |
| CNB2006102004093A CN100557440C (en) | 2005-05-09 | 2006-04-29 | The detection method of hundred stamen pharmaceutical preparations |
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| CN 200510049768 CN1698758A (en) | 2005-05-09 | 2005-05-09 | Pharmaceutical preparation of bastardtoad flax and its preparation method and quality control method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102057777A (en) * | 2010-10-28 | 2011-05-18 | 南京农业大学 | Method for breaking Thesium chinense seed dormancy for promoting germination |
| CN107389850A (en) * | 2017-08-02 | 2017-11-24 | 楚雄医药高等专科学校 | A kind of method of quality control of pine needle medicinal material |
| CN108802208A (en) * | 2018-03-08 | 2018-11-13 | 安徽九华华源药业有限公司 | The mass analysis method of BAIRUI PIAN |
| CN111024881A (en) * | 2020-01-08 | 2020-04-17 | 河北中医学院 | Rapid double-information thin-layer identification method for thesium Chinese medicinal materials, granules and target decoction dry powder |
| CN113813391A (en) * | 2021-09-28 | 2021-12-21 | 上海雷允上药业有限公司 | Auxiliary material, application of auxiliary material composition, core of thesium Chinese tablets, film-coated thesium Chinese tablets and preparation method of film-coated thesium Chinese tablets |
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2005
- 2005-05-09 CN CN 200510049768 patent/CN1698758A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102057777A (en) * | 2010-10-28 | 2011-05-18 | 南京农业大学 | Method for breaking Thesium chinense seed dormancy for promoting germination |
| CN102057777B (en) * | 2010-10-28 | 2012-07-04 | 南京农业大学 | Method for breaking Thesium chinense seed dormancy for promoting germination |
| CN107389850A (en) * | 2017-08-02 | 2017-11-24 | 楚雄医药高等专科学校 | A kind of method of quality control of pine needle medicinal material |
| CN107389850B (en) * | 2017-08-02 | 2020-08-07 | 楚雄医药高等专科学校 | Quality control method of pine needle medicinal material |
| CN108802208A (en) * | 2018-03-08 | 2018-11-13 | 安徽九华华源药业有限公司 | The mass analysis method of BAIRUI PIAN |
| CN111024881A (en) * | 2020-01-08 | 2020-04-17 | 河北中医学院 | Rapid double-information thin-layer identification method for thesium Chinese medicinal materials, granules and target decoction dry powder |
| CN111024881B (en) * | 2020-01-08 | 2021-08-31 | 河北中医学院 | Rapid double-information thin-layer identification method for thesium Chinese medicinal materials, granules and target decoction dry powder |
| CN113813391A (en) * | 2021-09-28 | 2021-12-21 | 上海雷允上药业有限公司 | Auxiliary material, application of auxiliary material composition, core of thesium Chinese tablets, film-coated thesium Chinese tablets and preparation method of film-coated thesium Chinese tablets |
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