CN1799575A - Chinese medicinal dispersible tablet, its preparation process and quality control method - Google Patents
Chinese medicinal dispersible tablet, its preparation process and quality control method Download PDFInfo
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Abstract
The invention discloses a dispersible tablet of Phlomis rotata Benth, which is prepared from Phlomis rotata Benth extract, cross bonding polyvinylpyrrolidone, low substituted methylcellulose propylene glycol ether, crystalline cellulose and micro powder silica gel. The invention also discloses the process for preparing the dispersing tablet and the quality control method.
Description
Technical field
The raw material that the present invention relates to a kind of dispersible tablets of Chinese medicine is formed, and has also related to the preparation method and the method for quality control of this dispersible tablet simultaneously, belongs to the field of Chinese medicines.
Background technology
Enlarged edition of Pharmacopoeia of the People's Republic of China version in 2000 has been announced a kind of Chinese medicine Radix Lamiophlomidis Rotatae sheet, by hemostasis, analgesia, antibacterial, acute, subacute toxicity test, immunologic function test and antitumor test, confirm the Radix Lamiophlomidis Rotatae sheet have preferably stop blooding, analgesia and antibacterial action, toxicity is little, and few side effects can also improve specificity and non-specific immunity.Its dosage changing form preparation Radix Lamiophlomidis Rotatae capsule, can obviously prolong pain and react time of occurrence, significantly shorten the mice bleeding time, improve macrophage phagocytic rate, macrophage phagocytic index, E-garland formation rate and esterase dyeing positive rate, and mice transplantability ehrlich carcinoma (EC) had inhibitory action, and the tumor animal spleen heavily there is the trend of the increase of making.Radix Lamiophlomidis Rotatae has determined curative effect, safety is good, the wide characteristics of clinical adaptation, but the general formulation of Radix Lamiophlomidis Rotatae exists wretched insufficiency parts such as disintegration rate is slow, onset is slow, bioavailability is low as the hemostatic analgesia medicine.Rapid as pain easing and hemostasis medicine disintegrate, rapid-action, the bioavailability height is very crucial.
At the existing deficiency of the existing preparation of Radix Lamiophlomidis Rotatae, develop the important content that disintegration rate is fast, absorption is fast, bioavailability Radix Lamiophlomidis Rotatae oral formulations high, good stability has become Radix Lamiophlomidis Rotatae research in recent years, as Radix Lamiophlomidis Rotatae capsule, Duyiwei soft capsule etc., the Duyiwei soft capsule content is liquid or semisolid, orally be dispersed or dissolved in the gastro-intestinal Fluid very soon, help that the inhalation effects soft capsule absorbs the speed limit process be the disintegration rate of capsule shells, soft capsule is generally 4 disintegration? minute.Can be as soft capsule in the disintegration of regulation of disintegrate fully in the scope, then bioavailability of medicament is very high, but, at present, the soft capsule ubiquity disintegrate problem of China's development, softgel shell is easily aging, disintegration rate increases along with the increase of the aged degree of softgel shell, the not even disintegrate that has, so still there is bigger defective in soft capsule preparation on stability problem, capsule is the same with conventional tablet, it all is traditional handicraft, do not have the raising of matter on the bioavailability problem than tablet, therefore there is above significantly deficiency in the oral formulations of existing Radix Lamiophlomidis Rotatae, presses for the oral formulations of the new better effects if of exploitation.
Dispersible tablet is the soft good way that addresses the above problem, but because dispersible tablet is applied to monomer component always is main chemical drugs, the Chinese medicine that is applied to complicated component is still difficult, thereby must study at prescription, solves correlation techniques such as its shaping, stability, disintegration time and asks.
Summary of the invention
The purpose of this invention is to provide a kind of dispersible tablets of Chinese medicine. because the national drug standards require dispersible tablet disintegrate in 3 minutes to finish, and ingredient there is the dissolution requirement, this molding to dispersible tablets of Chinese medicine has caused very big difficulty, and different Chinese medicines are made dispersible tablet, the adjuvant of using in its moulding process all can be different, must be according to the characteristics design moulding process of prescription Chinese crude drug, the present invention has gone out the moulding process that suitable Radix Lamiophlomidis Rotatae medicinal substances extract is made dispersible tablet by experimental study, and the present invention also provides preparation method, the quality standard of this dispersible tablet.
The preparation method technical scheme of dispersible tablets of Chinese medicine:
The weight of dispersible tablets of Chinese medicine raw material of the present invention consists of: 200～300 parts of Radix Lamiophlomidis Rotatae extracts, 40～150 parts of crospolyvinylpyrrolidone, 20～60 parts of low-substituted hydroxypropyl celluloses, 50～150 parts of microcrystalline Cellulose, 1～3 part of micropowder silica gel.
Extraction process:
The extraction process of Radix Lamiophlomidis Rotatae medical material is the extraction process according to an enlarged edition Zhao of Pharmacopoeia of the People's Republic of China version in 2000 Radix Lamiophlomidis Rotatae sheet, and through further quadrature screening, the process for refining parameter obtains:
The Radix Lamiophlomidis Rotatae medical material is pulverized, and decocts with water three times, and amount of water is respectively 10,8,8 times, and each 1 hour, collecting decoction filtered, and filtrate is condensed into the clear paste that relative density is about 1.30 (85 ℃), dry (60 ℃ ,-0.08Mpa), dried cream powder becomes fine powder.
Moulding process:
It is fast to the purpose of this invention is to provide a kind of disintegrate, the medicine stripping is dispersible tablet rapidly, and for reaching this purpose, the moulding process of dispersible tablet is most important, for effectively controlling the quality of dispersible tablet, be fit to proper auxiliary materials our characteristics, the disintegrate of energy rapid release by experiment sieving.
1. with Radix Lamiophlomidis Rotatae extract 240 weight portions, crospolyvinylpyrrolidone (PVPP) 50 weight portions, lactose 150 weight portions, 60 parts in mannitol, mix homogeneously, with 50% ethanol wet granulation, 50 ℃ of dryings, granulate, add magnesium stearate 1 weight portion, mix homogeneously, tabletting.The dispersible tablet that this moulding process is pressed into, the dispersible tablet mouldability is bad, a large amount of loose sheets, sliver phenomenon occur, and surperficial piebaldism is serious, and is unilateral rough.Analysis causes the reason of above-mentioned phenomenon to be that Chinese medicine extract is different with single chemical constituent, can not remove to suppress dispersible tablets of Chinese medicine with single disintegrating agent, should suitably add the molding that some adjuvants are assisted dispersible tablets of Chinese medicine in addition, and Chinese medicine extract, alcohol granulation with low concentration, granule is hard, and bad molding when tabletting is so should improve the used concentration of alcohol of granulating.
2. with Radix Lamiophlomidis Rotatae extract 240 weight portions, crospolyvinylpyrrolidone (PVPP) 50 weight portions, microcrystalline Cellulose (MCC) 150 weight portions, lactose 59 weight portions, mix homogeneously, with 70% ethanol wet granulation, 50 ℃ of dryings, granulate, add magnesium stearate 1 weight portion, mix homogeneously, tabletting.The dispersible tablet that this moulding process is pressed into, the dispersible tablet mouldability is better, illustrate that the adding of microcrystalline Cellulose has improved the molding of dispersible tablet significantly, the phenomenon that loose sheet no longer occurs, but unilateral rough, have the part dispersible tablet to have piebaldism, and disintegration time is long, undesirable, so still need screen proper auxiliary materials.
3. with Radix Lamiophlomidis Rotatae extract 240 weight portions, crospolyvinylpyrrolidone (PVPP) 40 weight portions, microcrystalline Cellulose (MCC) 150 weight portions, low-substituted hydroxypropyl cellulose 70 weight portions, mix homogeneously, with 70% ethanol wet granulation, 50 ℃ of dryings, granulate adds micropowder silica gel 1 weight portion, mix homogeneously, tabletting.The dispersible tablet that this moulding process is pressed into, the dispersible tablet good moldability, unilateral smooth, but the shortcoming of this mouldability technology is, dispersible tablet still can not disintegrate fully in 3 minutes, and disperses inhomogeneous.Therefore the disintegration time that adopts the method for the consumption that strengthens disintegrating agent to remove to improve dispersible tablet is impracticable.
4. for improving the disintegration time of dispersible tablet, with disintegrating agent, and behind granulate, add an amount of disintegrating agent again in this research finally is adopted when wet granulation, this inside and outside the method for the efficient disintegrating agent of adding, improve the disintegration rate of dispersible tablet.With Radix Lamiophlomidis Rotatae extract 240 weight portions, crospolyvinylpyrrolidone 60 weight portions, low-substituted hydroxypropyl cellulose 40 weight portions, microcrystalline Cellulose 100 weight portions, mixing, alcohol granulation with 75%; Wet granular adds crospolyvinylpyrrolidone 40 weight portions, mixes thoroughly, dry (50 ℃), granulate add micropowder silica gel 1 weight portion, and it is an amount of to add crospolyvinylpyrrolidone, to 500 weight portions, mixing, tabletting.The dispersible tablet of this moulding process compacting, good moldability does not have loose sheet, sliver phenomenon, dispersible tablet surface-brightening, and disintegrate fully in 3 minutes, and be uniformly dispersed, the therefore inside and outside method that adds efficient disintegrating agent has solved the disintegrate problem of this prescription dispersible tablet.Test is also attempted using and the carboxymethylstach sodium of the crospolyvinylpyrrolidone equivalent efficient disintegrating agent as inside and outside adding, the result is also fine with the dispersible tablet mouldability that carboxymethylstach sodium replaces the moulding process of crospolyvinylpyrrolidone to suppress, there is no loose sheet, sliver phenomenon, therefore, the disintegrating agent that adds when wet granulation and granulate can be selected in crospolyvinylpyrrolidone and the carboxymethylstach sodium any.This method that the disintegrating agent segmentation is added, not seeing in traditional handicraft has application, is one of characteristics of the present invention.
According to above great deal of experimental, determine that dispersible tablets of Chinese medicine raw material weight ratio of components of the present invention is:
240 parts of Radix Lamiophlomidis Rotatae extracts, 100～120 parts of crospolyvinylpyrrolidone, 40 parts of low-substituted hydroxypropyl celluloses, 100 parts of microcrystalline Cellulose, 1 part of micropowder silica gel.
For effectively controlling the quality of dispersible tablet of the present invention, the inventor has also formulated the method for quality control of this dispersible tablet:
(1) differentiate: get 5 of this product, porphyrize takes by weighing 0.5g, adds ethanol 10ml, puts water-bath (70 ℃) and goes up heating 10 minutes, filters, and gets subsequent filtrate as need testing solution.Other gets Radix Lamiophlomidis Rotatae control medicinal material 3g, adds water 30ml and decocts 1 hour, filters, and filtrate is put evaporate to dryness in the water-bath, and residue adds ethanol 10ml, puts in the water-bath and heats 10 minutes, filters, and filtrate compares medical material solution.According to thin layer chromatography test, draw above-mentioned two kinds of each 6ul of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with chloroform-methanol (8: 1), launch, take out, dry, spray is with the phosphomolybdic acid test solution, 105 ℃ be heated to speckle develop the color clear.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(2) inspection of n-butanol extract
N-butanol extract: get 5 of this product, porphyrize, the accurate title, decide, put in the tool plug conical flask, precision adds water 50ml, and supersound process made dissolving in 15 minutes, centrifugal, precision is measured supernatant 10ml, extracts 3 times (20ml, 20ml, 15ml) with water saturated n-butyl alcohol jolting, merges n-butanol extracting liquid, the water 10ml saturated with n-butyl alcohol washs 1 time, get n-butyl alcohol liquid, put dry putting in the evaporating dish of constant weight, behind evaporate to dryness in the water-bath, in 105 ℃ of dryings 3 hours, cooled off 30 minutes to exsiccator, weight decided in accurate rapidly title, promptly.
(3) assay
Ultraviolet method is measured content of total flavone:
The preparation precision of reference substance solution takes by weighing at the control substance of Rutin 20mg of 120 ℃ of drying under reduced pressure to constant weight, puts in the 100ml measuring bottle, adds 70% ethanol 80ml, ultrasonic dissolution is put coldly, adds 70% ethanol to scale, shake up, promptly get (containing anhydrous rutin 0.2mg among every 1ml).
The preparation precision of standard curve is measured reference substance solution 1.0ml, 2.0ml, 3.0ml, 4.0ml, 5.0ml, puts respectively in the 25ml measuring bottle, adds water to 5ml, add 5% sodium nitrite solution 1ml, mixing was placed 6 minutes, added 10% aluminum nitrate solution 1ml, shake up, placed 6 minutes, hydro-oxidation sodium test solution 10ml adds water to scale again, shake up, placed 15 minutes; With corresponding solution is blank.According to spectrophotography (an appendix V of Chinese Pharmacopoeia version in 2000 B), measure trap at 500nm wavelength place, be that vertical coordinate, concentration are abscissa with the trap, the drawing standard curve.
It is an amount of that algoscopy is got this product, the accurate title, decide, and puts in the 100ml ground triangular flask, adds hot water 25ml, stir and supersound process (power 250W, frequency 40KHz) 20 minutes, put coldly, extract once (15ml) with petroleum ether (60-90 ℃), water layer quantitatively is transferred in the 100ml measuring bottle, the accurate again dehydrated alcohol 70ml that adds, supersound process (power 250W, frequency 40KHz) is 10 minutes again, put cold, add water to scale, shake up, centrifugal (3000 rev/mins) 5 minutes, precision is measured supernatant 1ml, put in the 25ml measuring bottle, the method under the preparation of sighting target directrix curve is from " adding water to 5ml ", measure trap in accordance with the law, read the content of rutin the need testing solution from standard curve, calculate, promptly.
High performance liquid chromatography is to the assay of Quercetin
Chromatographic condition: mobile phase: methanol-0.4% phosphoric acid (55: 45); Flow velocity 1.0ml/min; Detect wavelength 370nm; 30 ℃ of column temperatures; Number of theoretical plate calculates by the Quercetin peak should be not less than 3000.
The learn from else's experience Quercetin reference substance of phosphorus pentoxide dried overnight of the preparation of reference substance solution is an amount of, accurately claims surely, adds methanol and makes the solution that every 1ml contains 30 μ g, promptly.
This product 150mg under the determination of total flavonoids item is got in the preparation of need testing solution, and accurate the title decides, and puts in the 25ml measuring bottle, add 2.5mol/L methanol hydrochloride solution 20ml, supersound process (250W, 40Hz) 30 minutes, put coldly, be diluted to scale, shake up with the 2.5mol/L methanol hydrochloride solution, filter, precision is measured subsequent filtrate 10ml, puts in the 50ml round-bottomed flask, heating hydrolysis is 30 minutes in 90 ℃ of water-baths, puts coldly, is transferred in the 25ml measuring bottle, add methanol to scale, shake up, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly
Beneficial effect:
(1) dispersible tablets of Chinese medicine of the present invention is the dosage form improvement on Radix Lamiophlomidis Rotatae common oral preparation (tablet and capsule) basis, collapses agent and good mixed with excipients by the extract of principal agent and specific speed, and tabletting forms, stable quality after long time storage.
(2) disintegrate and stripping are the speed limit processes that oral formulations absorbs. dispersible tablets of Chinese medicine collapses agent by medicine and specific speed and good excipient is formed, and before tabletting, added specific speed and collapsed agent, with conventional tablet, capsule is compared, homodisperse fine particle can promptly be resolved in oral back in water, its effective ingredient total flavones can stripping 75% 10 minutes the time in rutin, helping the medicine stripping absorbs, because they are just rapidly disintegrate and being uniformly dispersed in 3 minutes, and conventional tablet, capsule is disintegrate in 30 minutes then, therefore have incomparable disintegrate of ordinary tablet and dissolving out capability, it is fast to take post-absorption, the bioavailability height.
(3) taking convenience, dispersible tablets of Chinese medicine can add after the aqueous dispersion oral, suck to obey in mouthful to become to swallow, and take more convenient.
(4) steady quality:
By the room temperature reserved sample observing method and the accelerated test of heating dispersible tablets of Chinese medicine is observed.(1) room temperature reserved sample observing method: (T=25 ℃ ± 2 ℃, RH=60 ± 10%) at ambient temperature, carry out continuous six months study on the stability at the appointed time; (2) accelerated test of heating: (T=40 ± 2 ℃ under the constant temperature and humidity condition, RH=75% ± 5%), sample is placed with in the saturated exsiccator of saturated sodium-chloride, be placed on again in 40 ℃ of calorstats, carry out continuous trimestral study on the stability at the appointed time, the result shows, every inspections such as its character, discriminating, assay and dissolution, dispersing uniformity, tablet weight variation, disintegration, microbial limit, every index has no significant change, and illustrates that the product that the present invention makes is stable.
The specific embodiment:
Below further specify technical scheme of the present invention by specific embodiment:
Embodiment one:
Get the Radix Lamiophlomidis Rotatae medical material, pulverize, decoct with water three times, amount of water is respectively 10,8,8 times, and each 1 hour, collecting decoction filtered, and filtrate is condensed into the clear paste that relative density is about 1.30 (85 ℃), dry (60 ℃ ,-0.08Mpa), dried cream powder becomes fine powder.Get fine powder 240g, add crospolyvinylpyrrolidone 60g, low-substituted hydroxypropyl cellulose 40g, microcrystalline Cellulose 100g, mixing, alcohol granulation with 75%; Wet granular adds crospolyvinylpyrrolidone 40g, mixes thoroughly, dry (60 ℃), and granulate adds micropowder silica gel 1g, and crospolyvinylpyrrolidone is an amount of, to 500g, and mixing, tabletting.
Embodiment two:
Get the Radix Lamiophlomidis Rotatae medical material, pulverize, decoct with water three times, amount of water is respectively 10,8,8 times, each 1 hour, collecting decoction filtered (160 mesh sieve), and filtrate is condensed into the clear paste that relative density is about 1.30 (85 ℃), dry (60 ℃ ,-0.08Mpa), dried cream powder becomes fine powder.Get fine powder 280kg, add crospolyvinylpyrrolidone 120kg, low-substituted hydroxypropyl cellulose 50kg, microcrystalline Cellulose 60kg, mixing, alcohol granulation with 75%; Wet granular adds carboxymethylstach sodium 40kg, mixes thoroughly, dry (60 ℃), granulate adds micropowder silica gel 1kg, and carboxymethylstach sodium is an amount of, mixing, tabletting.
Claims (7)
1. dispersible tablets of Chinese medicine, its raw material consists of Radix Lamiophlomidis Rotatae extract and adjuvant, the weight ratio that it is characterized in that each ingredient is: 200～300 parts of Radix Lamiophlomidis Rotatae extracts, 40～150 parts of crospolyvinylpyrrolidone, 20～60 parts of low-substituted hydroxypropyl celluloses, 50～150 parts of microcrystalline Cellulose, 1～3 part of micropowder silica gel.
2. dispersible tablets of Chinese medicine as claimed in claim 1 is characterized in that its raw material weight ratio is: 240 parts of Radix Lamiophlomidis Rotatae extracts, 100～120 parts of crospolyvinylpyrrolidone, 40 parts of low-substituted hydroxypropyl celluloses, 100 parts of microcrystalline Cellulose, 1 part of micropowder silica gel.
3. the preparation method of dispersible tablets of Chinese medicine as claimed in claim 1 or 2 is characterized in that adopting the step of following order:
A. get the Radix Lamiophlomidis Rotatae medical material, pulverize, decoct with water three times, amount of water is respectively 10,8,8 times, and each 1 hour, collecting decoction filtered, and relative density was about 1.30 clear paste when filtrate was condensed into 85 ℃, drying, and dried cream powder becomes fine powder.
B. with the Radix Lamiophlomidis Rotatae extract fine powder, 60 parts of crospolyvinylpyrrolidone, low-substituted hydroxypropyl cellulose, microcrystalline Cellulose, evenly mixed.
C. make wetting agent system soft material with 75% ethanol, and add 40 parts of crospolyvinylpyrrolidone in wet granular, mix thoroughly, wet granular carries out drying under 50～80 ℃ of conditions.
D. during granulate, add micropowder silica gel, and add crospolyvinylpyrrolidone to making total amount, mixing, tabletting.
4. the preparation method of dispersible tablets of Chinese medicine as claimed in claim 3 is characterized in that: the also available carboxymethylstach sodium of the crospolyvinylpyrrolidone that adds in step c, d or other efficient disintegrating agent equivalent replacements.
5. the method for quality control of dispersible tablets of Chinese medicine as claimed in claim 1 or 2, its feature comprises following content: get 5 of invention dispersible tablets, porphyrize, take by weighing 0.5g, add ethanol 10ml, put in 70 ℃ of water-baths and heated 10 minutes, filter, get subsequent filtrate as need testing solution; Other gets Radix Lamiophlomidis Rotatae control medicinal material 3g, adds water 30ml and decocts 1 hour, filters, and filtrate is put evaporate to dryness in the water-bath, and residue adds ethanol 10ml, puts in the water-bath and heats 10 minutes, filters, and filtrate compares medical material solution.According to thin layer chromatography test, draw above-mentioned two kinds of each 6ul of solution, put respectively on same silica gel g thin-layer plate, with chloroform: methanol is that 8: 1 mixture is developing solvent, launches, and takes out, and dries, and spray is with the phosphomolybdic acid test solution, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
6. the method for quality control of dispersible tablets of Chinese medicine as claimed in claim 5, its feature also comprises following content: get 5 of dispersible tablets of the present invention, and porphyrize, the accurate title, decide, put in the tool plug conical flask, precision adds water 50ml, and supersound process made dissolving in 15 minutes, and is centrifugal, precision is measured supernatant 10ml, extract 3 times with water saturated n-butyl alcohol jolting, each consumption is respectively 20ml, 20ml, 15ml merges n-butanol extracting liquid, the water 10ml saturated with n-butyl alcohol washs 1 time, get n-butyl alcohol liquid, put dry putting in the evaporating dish of constant weight, behind evaporate to dryness in the water-bath, in 105 ℃ of dryings 3 hours, cooled off 30 minutes to exsiccator, weight decided in accurate rapidly title, promptly.
7. the method for quality control of dispersible tablets of Chinese medicine as claimed in claim 6, its feature also comprises following content:
A, ultraviolet method are measured content of total flavone:
The preparation of reference substance solution: precision takes by weighing at the control substance of Rutin 20mg of 120 ℃ of drying under reduced pressure to constant weight, puts in the 100ml measuring bottle, adds 70% ethanol 80ml, and ultrasonic dissolution is put coldly, adds 70% ethanol to scale, shakes up, promptly;
Outside the preparation of standard curve: precision is measured reference substance solution 1.0ml, 2.0ml, 3.0ml, 4.0ml, 5.0ml, puts respectively in the 25ml measuring bottle, adds water to 5ml, add 5% sodium nitrite solution 1ml, mixing was placed 6 minutes, added 10% aluminum nitrate solution 1ml, shake up, placed 6 minutes, hydro-oxidation sodium test solution 10ml adds water to scale again, shake up, placed 15 minutes; With corresponding solution is blank.Pressing spectrophotography, measure trap at 500nm wavelength place, is that vertical coordinate, concentration are abscissa with the trap, the drawing standard curve;
Algoscopy: it is an amount of to get the product that the present invention gets, and accurately claims surely, puts in the 100ml ground triangular flask, add hot water 25ml, stirring and supersound process 20 minutes are put cold, with the 15ml Petroleum ether extraction once, water layer quantitatively is transferred in the 100ml measuring bottle, the accurate again dehydrated alcohol 70ml that adds, supersound process is 10 minutes again, put cold, add water to scale, shake up, centrifugal 5 minutes with 3000 rev/mins speed, precision is measured supernatant 1ml, put in the 25ml measuring bottle, the method under the preparation of sighting target directrix curve is from " adding water to 5ml ", measure trap in accordance with the law, read the content of rutin the need testing solution from standard curve, calculate, promptly.
B, high performance liquid chromatography are to the assay of Quercetin
Chromatographic condition: mobile phase: methanol-0.4% phosphoric acid (55: 45); Flow velocity 1.0ml/min; Detect wavelength 370nm; 30 ℃ of column temperatures; Number of theoretical plate calculates by the Quercetin peak should be not less than 3000.
The preparation of reference substance solution: the Quercetin reference substance of the phosphorus pentoxide dried overnight of learning from else's experience is an amount of, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 30 μ g, promptly.
The preparation of need testing solution: get the sample 150mg under a item, the accurate title, decide, and puts in the 25ml measuring bottle, add 2.5mol/L methanol hydrochloride solution 20ml, supersound process 30 minutes is put cold, be diluted to scale with the 2.5mol/L methanol hydrochloride solution, shake up, filter, precision is measured subsequent filtrate 10ml, puts in the 50ml round-bottomed flask, and heating hydrolysis is 30 minutes in 90 ℃ of water-baths, put coldly, be transferred in the 25ml measuring bottle, add methanol to scale, shake up, promptly.
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
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| CN107045035A (en) * | 2017-04-18 | 2017-08-15 | 普正药业股份有限公司 | A kind of method for building up of Duyiwei effervescent tablet HPLC finger-prints |
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| CN1559550A (en) * | 2004-02-16 | 2005-01-05 | 沈阳药科大学 | New type medicina preparation with one chinese medicinal herb extract ant its preparation method |
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| CN107045035A (en) * | 2017-04-18 | 2017-08-15 | 普正药业股份有限公司 | A kind of method for building up of Duyiwei effervescent tablet HPLC finger-prints |
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