CN101653491A - Preparation technology and quality control method of preparation containing cassia twig and tuckahoe - Google Patents
Preparation technology and quality control method of preparation containing cassia twig and tuckahoe Download PDFInfo
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- CN101653491A CN101653491A CN200910158020A CN200910158020A CN101653491A CN 101653491 A CN101653491 A CN 101653491A CN 200910158020 A CN200910158020 A CN 200910158020A CN 200910158020 A CN200910158020 A CN 200910158020A CN 101653491 A CN101653491 A CN 101653491A
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Abstract
The invention provides a new preparation method and a quality control method of a pill containing cassia twig and tuckahoe, The preparation method have the advantages of few production steps, short production cycle, high production mechanization, stable preparation quality, high content of effective ingredients, fast disintegration, high bioavailability, small dose, convenient administration and the like. The invention also provides the quality control method of cinnamyl aldehyde, cinnamic acid, paeonol, peoniflorin and amygdalin in the pill containing cassia twig and tuckahoe.
Description
Technical field
The present invention relates to a kind of preparation technology and method of quality control of cassia twig and poria cocos preparation.
Background technology
Ramulus Cinnamomi Poria pill is stated from the middle women's gestation abnormal pulse disease of Zhang Zhongjing " Medical Treasures of the Golden Chamber " and controls the 20, and being apt to control the married woman place has the Disorder piece, pregnant fetal diseases, and persistent vaginal bloody discharge, and dysmenorrhea amenorrhea due to the congestion, Disorder ties mass in the abdomen, is famous blood circulation promoting and blood stasis dispelling prescription.Be principal agent temperature promoting blood circulation with Ramulus Cinnamomi in the side; Fetus nourishing is set upright in Poria spleen invigorating eliminating dampness by diuresis; Radix Paeoniae is nourished blood and seeks; Semen Persicae, Cortex Moutan repercussive blood, Po mass in the abdomen, promoting tissue regeneration by removing blood stasis; Close and the side of being, make and assault fortified position and just do not hinder, repercussive and non-impairment of YIN is a blood circulation promoting and blood stasis dispelling, eliminating stagnation disappears, effective prescription of treatment Fu Ke mass in the abdomen.Be widely used in common gynecological disease or frequently-occurring diseases such as lochiorrhea after treatment hysteromyoma of gynecology, ovarian cyst, endometriosis, old ectopic pregnancy, pelvic cavity congestion syndrome, the artificial abortion, infertile habitual abortion in recent years, clinical effectiveness is good.
The Ramulus Cinnamomi Poria pill prescription is Ramulus Cinnamomi, Poria, Paeonia suffruticosa (removing the heart), Semen Persicae (the peeling point is endured), each five equilibrium of Radix Paeoniae in " Medical Treasures of the Golden Chamber ".The right five tastes, the end, refined honey and ball, big as the rabbit dung, obey a ball before the food every day, do not know, adds to three balls.
" Chinese pharmacopoeia one one of version in 2005 is recorded two cassia twig and poria cocos preparation dosage forms altogether, and one is " Ramulus Cinnamomi Poria pill ", prescription: Ramulus Cinnamomi, Poria, Cortex Moutan, Radix Paeoniae Rubra, each 100g of Semen Persicae.One is " GUIZHI FULING JIAONANG ", prescription: Ramulus Cinnamomi, Poria, Cortex Moutan, the Radix Paeoniae Alba, each 100g of Semen Persicae.In addition, a manufacturer production " cassia twig and poria cocos preparation " surplus China has had 40 relates to more than ten novel form, and coverage is extensive.
" Chinese pharmacopoeia versions in 2000 and all recorded " Ramulus Cinnamomi Poria pill " in the version in 2005, said preparation is used as medicine with medicinal powder, Mel is binding agent and forming agent, be prepared into honeyed pill, having production stage, many (medical material cleans, pulverize, refined honey, and top, pill, the plastic casing packing, hang technologies such as wax sealing), production cycle is long, supplementary product consumption is big, bacterium inspection index is restive, volatile ingredient loses easily, the easy moisture absorption in the storage process, easily mouldy or infested, it is big in use to have dose, take and carry inconvenience, and the preparation disintegration rate is slow, and drug effect is slow.Therefore people have carried out a large amount of preparation process research to Ramulus Cinnamomi Poria pill, have prepared the several formulations dosage form, from having solved the shortcoming of above-mentioned pill dosage form to a great extent, and to several formulations technology and dosage form application national patent.As application number is that 03121130.5 invention relates to Chinese medicinal tablet and the preparation technology thereof who makes with the prescription of Ramulus Cinnamomi Poria pill, be characterized in extracting the active substance in the cassia twig tuckahoe prescription after, add adjuvant dried cream powder and microcrystalline Cellulose and make.Application number is that 200510060814.5 patent relates to a kind of cinnamon twig and poria dripping pill and preparation method thereof, be by the cassia twig tuckahoe prescription through after extracting, add that substrate is dripped to make.Application number is 200410069115.2 patent disclosure a kind of cinnamon twig and poria oral disnitegration tablet and preparation method thereof is characterized in that it is made up of effective site of extracting in Chinese medicine Ramulus Cinnamomi, Poria, Cortex Moutan, Radix Paeoniae Rubra, the Semen Persicae and pharmaceutic adjuvant.Application number a kind of preparation method for the treatment of the medicine of gynecological's Blood stasis disease that has been 200410041212.0 patent disclosure, it is a raw material with Chinese herbal medicine Ramulus Cinnamomi, Poria, Cortex Moutan, the Radix Paeoniae Alba and Semen Persicae, it is characterized in that, its step is to produce Ramulus Cinnamomi Semen Persicae extractum, Poria extractum, Cortex Moutan Radix Paeoniae Alba extractum, Oleum Cinnamomi Benexate Hydrochloride, paeonol Benexate Hydrochloride respectively, adds conventional pharmaceutic adjuvant and makes.Application number a kind of preparation method of cassia twig and poria cocos preparation that has been 200710166287.5 patent disclosure.Use the water extraction medicine, concentrated, granulating process in conjunction with modern can be prepared into dosage forms such as granule, tablet, capsule, powder, drop pill.Application number is that 200810150311.0 invention relates to a kind of Cinnamomi and poria composition, and said composition prepares with the following method: Ramulus Cinnamomi, Poria, Semen Persicae, Radix Paeoniae Rubra, the Cortex Moutan five kinds of Chinese medicine of getting mistake 10～24 mesh sieves of equivalent; Ramulus Cinnamomi, Cortex Moutan, Radix Paeoniae Rubra, Semen Persicae four Chinese medicine carry out hybrid extraction, collect extract, and be standby; Above medicinal residues are mixed with Poria carry out carrying out water again after the alcohol extraction and carry, merging filtrate, concentrate extractum; This extractum and above-mentioned extract merge, and mixing is processed into preparation.Application number a kind of Guizhi Fuling solution solid dispersate that has been 200510111422.7 disclosure of the Invention, component and weight content comprise: cassia twig tuckahoe extract 5～40%, solubilizing agent 5～40%, carrier 20～90%.Application number is that inventions such as 200410004560.0,200410100866.6,200410056834.0,200410100867.0,200410080321.3,200510070657.6 all disclose a kind of cassia twig and poria cocos soft capsule and preparation method thereof.Its core is that the medicine in the Ramulus Cinnamomi Poria pill is made soft capsule content after extracting back and auxiliary materials and mixing, and refabrication becomes soft capsule.Application number is that 200410040500.4 and 200510200475.6 invention is that Ramulus Cinnamomi Poria pill is prepared into preparations such as disperseing sheet, soft capsule, micropill or drop pill through extracting equally.Application number provides a kind of cassia twig tuckahoe effervescence tablet and preparation method and method of quality control for 200610200120.1 invention.More than invention all is the research of carrying out at the shortcoming of traditional pill, has that volume is little, portable, preparation stabilization, advantage such as is easy to take.
But, above-mentioned patent does not fully take into account the mechanism of action of compound of Chinese medicine disease and the mutual relation between effective ingredient, studies show that: the clinical efficacy of cassia twig and poria cocos preparation is the coefficient result of plurality of active ingredients in the prescription, wherein just includes the chemical compounds such as cinnamic aldehyde, 2-methoxyl group cinnamic aldehyde, cinnamic acid, cinnamic alcohol, coumarin and protocatechuic acid in the Ramulus Cinnamomi; Chemical compounds such as the paeonol in the Cortex Moutan, paeoniflorin, Radix Paeoniae aglycon, paeonolide, the former glycoside of Cortex Moutan, the new glycoside of Cortex Moutan, 6-Hydroxycoumarin; Compositions such as the amygdaloside of Semen Persicae, Virginia prune glucoside, fatty glyceride, protein; Peoniflorin in the Radix Paeoniae, Hydroxy peoniflorin, lactone glucoside of Radix Paeoniae, benzoyl Hydroxy peoniflorin, benzoylpaeoniflorin, peonin, oxypaeoniflorin, Radix Paeoniae aglycon, lacdtlorin, galloylpaeoniflorin; The triterpenes components that contains in the Poria is as Pilus Caprae seu Ovis steroid-8-alkene type triterpene; Pilus Caprae seu Ovis steroid-7,9 (11)-diene type triterpene; 3,4-open loop-Pilus Caprae seu Ovis steroid-7,9 (11) diene type triterpenes and polysaccharide composition.Therefore, if cassia twig tuckahoe side is extracted, different along with extracting method and solvent can be caused corresponding loss of active ingredients and minimizing, and corresponding clinical efficacy will obviously reduce.Undertaken quantitatively by 10 kinds of index components (cinnamic aldehyde, cinnamic acid, glycerol trioleate, amygdaloside, pachymic acid, benzoic acid, peoniflorin, galloylpaeoniflorin, five galloyl glucoses and paeonol) in the Ramulus Cinnamomi Poria pill as Longzi, the rapids family of Japanese scholar, inquired into the different preparation formulations of cassia twig tuckahoe cause composition in the difference of effective ingredient and the extract preparation process because of the difference of preparation process variation.Result of study shows: amygdaloside, peoniflorin and benzoic acid content are apparently higher than granule in decoct; And derived essential oils such as paeonol and cinnamic aldehyde have only 30%～40%; And have the glycerol trioleate of blood coagulation resisting function and have that tell in the town, the pachymic acid of antiinflammatory action is undetected in decoct.Therefore, think that there is notable difference in the composition of decoct and crude drug powder.Further studies show that: adopt the extractum of spray drying method for preparation, then contain paeonol and cinnamic aldehyde hardly; The relative amount of amygdaloside and five galloyl glucoses is reduced to 1/2 and 1/3 respectively, and other compositions also reduce to some extent.Because the greatest differences of effective ingredient quantity and content in the preparation, cause the obvious difference of curative effect clinically, Japan's scholar's research is thought: the cassia twig tuckahoe pill improves the effect that the peripheral circulation effect is better than decoct, when the pill treatment Raynaud phenomenon of usefulness Ramulus Cinnamomi Poria pill decoct such as pool, temple and traditional method preparation and FF were limited, only pill had remarkable result.
Main chemical compositions is carried out quantitative assay in to pill and decoct, found that the content of cinnamic aldehyde in the pill is 2 times of decoct, and the content of paeoniflorin pill is 6 times of decoct.Back find relatively that at honeyed pill and other dosage forms it is minimum that the contact area of honeyed pill and air is reduced to, and can prevent contained fatty acid material oxidations in air such as Semen Persicae, can suppress the dissipation of volatile ingredients such as cinnamic aldehyde, prevents because of the humidity enzymolysis.Therefore, compare with other dosage forms, it is best that microcirculation improvement is taken the honeyed pill effect.
We have also compared the content of cinnamic acid, cinnamic aldehyde, paeonol in GUIZHI FULING JIAONANG that China has gone on the market and Ramulus Cinnamomi Poria pill, the result shows: with the cubage of 3 compositions in each dose, the content of cinnamic acid is 4.94 times of capsule in the honeyed pill, cinnamic aldehyde content is 9.48 times of capsule, and the content of paeonol is 6.23 times of capsule.Illustrate that active constituent content is starkly lower than honeyed pill in the capsule, can seriously have influence on the clinical efficacy of preparation.
Because the clinical efficacy mechanism of action of cassia twig tuckahoe side is still unclear, the mechanism of structure activity relationship and composition interphase interaction is still indeterminate, therefore, without basisly arbitrarily former preparation being carried out technical study, changes the effectiveness that dosage form all can seriously have influence on medicine, is worthless.
Because traditional honeyed pill of cassia twig tuckahoe is that employing Mel is the big honeyed pills preparation that adhesive is prepared into.Said preparation exists production stage many (medical material cleans, technologies such as pulverizing, refined honey and top, pill, plastic casing packing, the sealing of extension wax) in process of production, the production cycle is long, supplementary product consumption is big, bacterium inspection index is restive, volatile ingredient loses easily; In use have dose big, take and carry inconvenience; The easily moisture absorption, problem such as mouldy or infested in the storage process.Adopt watered pill preparation method, can effectively reduce taking dose, but the preparation method of the watered pill is the adopting process flow process be: type → capping → drying → select ball → coating → polishing → quality examination → packing is made in the preparation → molding of raw material → general.Because the general technology of making type that adopts, have that mechanization degree is low, labor intensity is big, technical process is long, the hygiology index is restive, disintegration is long, different restive, the problem such as tailing is many of the ball method of double differences, therefore badly influences the clinical practice of said preparation.Mel as binding agent in the honeyed pill dosage form accounts for about half of honeyed pill weight, therefore we are on the basis of comprehensive this ancient binding agent of removal Mel, adopt modern binding agent, and add an amount of efficient disintegrating agent, abandon the technology of traditional general method for making in the watered pill, adopt modern pressing technological forming, not only reduced effectively medicine taking dose, but also effectively raise preparation disintegration, shorten the production cycle, the preparation ball method of double differences is different little, reduce the pollution of antibacterial, adopt film coating procedure simultaneously to improve stability of formulation.Facts have proved that this production technology has advantages such as production stage is few, with short production cycle, production mechanization degree height, the quality of the pharmaceutical preparations is stable, patient's taking dose is little, taking convenience.For the modified form of honeyed pill provides new approach.
Summary of the invention
Purpose of the present invention just provides a kind of new method for preparing Ramulus Cinnamomi Poria pill and method of quality control.The present invention is in the problem of the chemical constituent of having furtherd investigate existing cassia twig and poria cocos preparation, the mechanism of action, structure activity relationship and cassia twig and poria cocos preparation dosage form existence at present, new preparation technique has been proposed, further investigate content of effective assay method in the cassia twig tuckahoe simultaneously, proposed the method for quality control of system.Preparation formulation provided by the invention has that production stage is few, with short production cycle, a production mechanization degree height, stable, the advantages such as active constituent content is high, disintegrate is rapid, bioavailability is high, taking dose is little, taking convenience of the quality of the pharmaceutical preparations.
The characteristics of the preparation method of cassia twig and poria cocos preparation of the present invention are the effective ingredient of as far as possible preserving in the cassia twig tuckahoe, reduce loss of active ingredients, therefore the present invention does not change the composition of cassia twig tuckahoe side, and promptly the weight ratio of each medical material (Ramulus Cinnamomi, Poria, Semen Persicae, Radix Paeoniae and Cortex Moutan) is 1: 1: 1 in the cassia twig tuckahoe side: 1: 1.Described Ramulus Cinnamomi is dry twig or the bark of canella Cortex Cinnamomi Cinnamomum cassia Presl, should be the dry bark of canella Cortex Cinnamomi Cinnamomum cassia Presl according to the Ramulus Cinnamomi described in the book on Chinese herbal medicine before textual criticism the Tang Dynasty, after the Tang Dynasty in the book on Chinese herbal medicine Ramulus Cinnamomi progressively develop into the dry twig of canella Cortex Cinnamomi C.cassia Presl, therefore Ramulus Cinnamomi of the present invention should comprise " " Cortex Cinnamomi " that Chinese pharmacopoeia was recorded in the version in 2005 and " Ramulus Cinnamomi ".Described Poria is the dry sclerotia of the fungus Poria Poria cocos of porous mattress section (Schw.) Wolf.Described Cortex Moutan is the dry root bark of Paeonia suffruticosa Paeoniasuffrutico Andr., Sichuan Paeonia suffruticosa P.szechuanica Fang., Herba Melastomatis Candii P.delavayi Franch. and mutation thereof among the cohosh Paeonia suffruticosa group Sect.Paeonia.Described Radix Paeoniae is the Radix Paeoniae Paeonialactiflora Pall. among the cohosh Radix Paeoniae group Sect.Paeonia, Paeonia mairei L P.mairei L é vl., Paeonia sterniana Fletcher in Journ. P.sterniana Fletcher., Paeonia obovata Maxim. P.obovata Maxim., Xinjiang Radix Paeoniae P.sinjiangensis K.Y.Pang., the dry root of Paeonia anomala P.anomala Linn. and CHUANSHAO medicine P.veitchii Lynch. and mutation thereof.Described Semen Persicae is the dry mature seed of rosaceous plant peach Prunuspersica (L.) Batsch or mountain peach P.davidiana (Carr.) Franch..
The concrete preparation technology of the present invention may further comprise the steps, and (1) gets Ramulus Cinnamomi, Poria, Cortex Moutan, Radix Paeoniae, Semen Persicae medical material, chooses decontamination and non-medicinal part respectively.(2) get Ramulus Cinnamomi, Poria, Cortex Moutan, Radix Paeoniae Rubra, Semen Persicae medical material respectively or mixed powder be broken into fine powder, sieve, standby.(3) get above-mentioned medical material fine powder, evenly mixed, add binding agent and mix, granulate, drying, granulate, standby.(4) get the granule for preparing, adding disintegrating agent and mix lubricant are even, put on the tablet machine, are pressed into a spherical ball, and (5) get the pill that step (4) is pressed into, the bag film-coat, promptly.
Further, described Ramulus Cinnamomi is dry twig or the bark of canella Cortex Cinnamomi Cinnamomum cassia Presl, i.e. " " Ramulus Cinnamomi " and " Cortex Cinnamomi " that Chinese pharmacopoeia version in 2005 is recorded, preferred Ramulus Cinnamomi.
Further, described Cortex Moutan is Paeonia suffruticosa Paeonia suffruticoAndr., Sichuan Paeonia suffruticosa P.szechuanica Fang. among the cohosh Paeonia suffruticosa group Sect.Paeonia, the dry root bark of Herba Melastomatis Candii P.delavayi Franch. and mutation thereof.The dry root bark of preferred Paeonia suffruticosa.
Further, described Radix Paeoniae is the Radix Paeoniae Paeonia lactifloraPall. among the cohosh Radix Paeoniae group Sect.Paeonia, Paeonia mairei L P.mairei L é vl., Paeonia sterniana Fletcher in Journ. P.sterniana Fletcher., Paeonia obovata Maxim. P.obovata Maxim., Xinjiang Radix Paeoniae P.sinjiangensis K.Y.Pang., the dry root of Paeonia anomala P.anomala Linn. and CHUANSHAO medicine P.veitchii Lynch. and mutation thereof.The root bark of preferred Radix Paeoniae and CHUANSHAO medicine.
Further, the described pulverizing of step of preparation process (2) also can mix Semen Armeniacae Amarum the back and pulverize, the difficulty that can avoid Semen Armeniacae Amarum to pulverize and sieve with Radix Paeoniae.
Further, the described binding agent of step of preparation process (3) is pharmaceutically acceptable carrier, is the well known typical binders that is used to prepare above-mentioned preparation, for example starch, modified starch, pregelatinized starch, dextrin, white dextrin, maltodextrin; Liquid glucose, scleroglucan, glucose, glucosan, Mel, sucrose, spherical sucrose, compressible sugar, sugar,confectioner's; Resina persicae, maltose alcohol, carrageenin, tamarind gum, high fructose syrup, Nulomoline, fructose, POLY-karaya, gelatin, xanthan gum, guaiac gum, locust bean gum; Alginic acid, sodium alginate, potassium alginate, ammonium alginate, calcium alginate; Pulullan polysaccharide, poloxamer; Ethylmethylcellulose, ethyl cellulose, Powderd cellulose, ethoxy methyl fiber rope, hydroxyethyl-cellulose, hydroxypropyl methylcellulose, hydroxypropyl cellulose, microcrystalline Cellulose, bagasse regrowth, sodium carboxymethyl cellulose, carboxymethylcellulose calcium; Sodium polyacrylate, polyacrylic acid, polyvidone, vinylpyrrolidone-vinyl acetate co-polymer, sodium starch phosphate etc.Also can select for use in the cassia twig tuckahoe prescription Poria as binding agent.Preferred starch, pregelatinized starch, modified starch, dextrin, gelatin, carrageenin, Resina persicae, xanthan gum, methylcellulose, sodium carboxymethyl cellulose, hydroxy ethyl fiber thing, polyvidone, Poria; More be optimized for pregelatinized starch, modified starch, dextrin, xanthan gum, sodium carboxymethyl cellulose, hydroxyethyl-cellulose, polyvidone, Poria.
Further, disintegrating agent described in the step of preparation process (4) is pharmaceutically acceptable carrier, be the well known disintegrating agent commonly used that is used to prepare above-mentioned preparation, for example modified starch, starch, sodium starch glycol, Explotab, pregelatinized starch, carboxymethyl starch sodium, hydroxypropyl starch, methylcellulose, low-substituted hydroxypropyl cellulose, hydroxyethylmethyl-cellulose, microcrystalline Cellulose, Powderd cellulose, carboxymethyl cellulose, carboxymethylcellulose calcium, glycine, cross-linking sodium carboxymethyl cellulose, polyvinylpolypyrrolidone, POLY-karaya, alginic acid, sodium alginate, silicon oxide, silica sol, aluminium-magnesium silicate, microbial alginate, microcrystalline Cellulose, polyethylene azoxy ketone, sucrose fatty acid ester, sucrose monolaurate, sucrose palmitic acid ester.Preferred starch, carboxymethyl starch, hydroxypropyl starch, polyvinylpolypyrrolidone, low-substituted hydroxypropyl cellulose, microcrystalline Cellulose.
Further, lubricant described in the step of preparation process (4) is pharmaceutically acceptable carrier, be the well known conventional lubricants that is used to prepare above-mentioned preparation, for example silicon dioxide, eicosyl sodium sulfate, Stepanol MG, sodium stearyl fumarate, Cera Chinensis, Cyclomethicone, aluminium hydroxide, leucine, polyglycerol fatty acid ester, colloidality silicon dioxide, silicic acid, calcium silicates, aluminium silicate, Aluminum calcium silicate., magnesium silicate, sodium stearate, hard soap, sodium stearate, cobaltous octadecanate, zinc stearate, magnesium stearate, Pulvis Talci, sodium palmitate, Polyethylene Glycol, sucrose fatty acid ester, sucrose monolaurate, sucrose palmitic acid ester, calcium phosphate.Preferred magnesium stearate, Pulvis Talci, Polyethylene Glycol, silicon dioxide.
Further, the pill that is pressed in the step of preparation process (5) is according to the needs of outward appearance, can increase sired results skill, that is, the pill that suppresses be put gradation adds 2～15% drug powders while rolling in the general ball pot, increase circle, with reach the pill rounding, the ball face is bright and clean.
Further, the described coating material of step of preparation process (5) is pharmaceutically acceptable carrier, be the well known bag film-coat material commonly used that is used to prepare above-mentioned preparation, for example cellulose derivative class, polyethylene glycols, acrylic acid and methacrylate copolymer class, polyethylene acetal diethylamine ethyl ester and other filmogen.Wherein the cellulose derivative class has hydroxypropyl emthylcellulose (HPMC), ethyl cellulose (EC), hydroxypropyl cellulose (HPC), methyl hydroxyethylcellulose (MHEC), methylcellulose (MC), sodium carboxymethyl cellulose (CMC-Na) etc.Polyethylene glycols (PEG) molecular weight is 4000～8000.Crylic acid resin, as: acrylic resin,, acrylic acid resin, HPMC and acrylic resin mixture, gastric solubleness acrylic resin number, HPMC and acrylic resin mixture.Acrylic acid and methacrylate copolymer, polyvinyl acetal diethylamine ethyl ester (AEA), Opadry and natural macromolecular material zein (zein), synthetic macromolecular material polyvinylpyrrolidone (polyvidone, PVP), polyethylene-film-coat materials such as vinylpyridine copolymer.
The present invention also provides the method for quality control of effective ingredient in the Ramulus Cinnamomi Poria pill.Promptly adopt high performance liquid chromatography that cinnamic aldehyde, cinnamic acid, paeonol, peoniflorin, amygdaloside in the Ramulus Cinnamomi Poria pill have been carried out assay.For the control method of effectively controlling Ramulus Cinnamomi Poria pill provides scientific basis.Concrete grammar is:
1. the assay of cinnamic acid, cinnamic aldehyde and paeonol in the Ramulus Cinnamomi Poria pill: with octadecylsilane chemically bonded silica is filler; Acetonitrile-phosphoric acid solution is a mobile phase; The detection wavelength is 200～400nm.Get Ramulus Cinnamomi Poria pill, remove coating, pulverize, precision takes by weighing 0.1g, puts in the 10ml measuring bottle, it is an amount of to add 50% methanol, and supersound extraction 30 minutes is taken out, and puts to room temperature, supply solvent to groove, shake up, with the microporous filter membrane filtration of 0.45 μ m, filtrate is as need testing solution.Precision takes by weighing cinnamic acid reference substance, cinnamic aldehyde reference substance, paeonol reference substance in addition, adds 50% dissolve with methanol and be prepared into to contain the solution that every ml solution contains cinnamic acid 10 μ g, cinnamic aldehyde 50 μ g, paeonol 100 μ g, as reference substance solution.Accurate respectively need testing solution, each 10 μ l of reference substance solution of drawing inject chromatograph of liquid under above-mentioned chromatographic condition, measure, promptly.See accompanying drawing 1,2,3,4.
Further, concentration of phosphoric acid is 0.001～5% in the mobile phase that acetonitrile-phosphoric acid solution is formed, and optimizing concentration is 0.01～1%, and more excellent condition is 0.1～0.5%; The detection wavelength is 200～400nm, and optimizing the detection wavelength is 250～350nm, and more excellent condition is 270～300nm, and optimal conditions is that cinnamic acid detects wavelength 270nm, and cinnamic aldehyde and paeonol detect wavelength 280～290nm.
2. paeoniflorin content is measured in the Ramulus Cinnamomi Poria pill: with octadecylsilane chemically bonded silica is filler; Methanol-phosphoric acid mobile phase; The detection wavelength is 230nm; Column temperature is 20～50.Get Ramulus Cinnamomi Poria pill fine powder 1.5g, the accurate title, decide, and puts in the 25ml tool plug conical flask, the accurate 75% ethanol 25ml that adds weighs ultrasonic 30min, put coldly, weigh again, supply the weight that subtracts mistake with 75% ethanol, centrifugal, get supernatant 10ml and put evaporate to dryness in the hot bath, the accurate 2ml water dissolution that adds, cross solid-phase extraction column, use methanol-eluted fractions, collect eluent and put in the 10ml volumetric flask standardize solution.Cross 0.45 μ m microporous filter membrane, collect subsequent filtrate and promptly get need testing solution.The accurate title, decided the peoniflorin reference substance, adds dissolve with methanol and be prepared into the solution that every ml contains 0.5mg, is reference substance solution.Accurate respectively need testing solution, each 10 μ l of reference substance solution of drawing inject chromatograph of liquid under above-mentioned chromatographic condition, measure, promptly.See accompanying drawing 5,6.
Further, concentration of phosphoric acid is 0.001～5% in the mobile phase that methanol-phosphoric acid is formed, and optimizing concentration is 0.01～1%, and more excellent condition is 0.1～0.5%; Column temperature is 20～50 ℃, and optimizing temperature is 30～40 ℃, and more excellent temperature is 30 ℃; Solid-phase extraction column is analytically commonly used, comprises anti-phase solid-phase extraction column, silica gel positive solid-phase extraction column, aluminium oxide solid-phase extraction column, macroporous adsorbent resin solid-phase extraction column, activated carbon solid-phase extraction column, kieselguhr solid-phase extraction column etc.Optimizing solid-phase extraction column is anti-phase solid-phase extraction column, silica gel positive solid-phase extraction column, aluminium oxide solid-phase extraction column, macroporous adsorbent resin solid-phase extraction column.More optimizing solid-phase extraction column is anti-phase solid-phase extraction column, aluminium oxide solid-phase extraction column, macroporous adsorbent resin solid-phase extraction column.The optimization solid-phase extraction column is the aluminium oxide solid-phase extraction column.
3. amygdaloside assay in the Ramulus Cinnamomi Poria pill: with octadecylsilane chemically bonded silica is filler; Mobile phase is methanol-acetonitrile-phosphoric acid solution system; The detection wavelength is 200～250nm; Column temperature is 20～40.Get Ramulus Cinnamomi Poria pill fine powder 3g, the accurate title, decide, and puts in the 50ml tool plug conical flask, the accurate 80% methanol 50ml that adds, weigh, place a night, weigh, supply the weight that subtracts mistake with 80% methanol, ultrasonic 30min is put cold, weigh again, supply the weight that subtracts mistake with 80% methanol, centrifugal, get supernatant 10ml and put evaporate to dryness in the hot bath, accurate 2ml water dissolution, the last solid-phase extraction column of adding, use 50% methanol-eluted fractions, collect eluent and put in the 10ml volumetric flask standardize solution.Cross 0.45 μ m microporous filter membrane, collect subsequent filtrate and promptly get need testing solution.The accurate title, decided the amygdaloside reference substance, adds methanol and be prepared into the solution that every ml contains 1mg, promptly gets reference substance solution.Accurate respectively need testing solution, each 10 μ l of reference substance solution of drawing inject chromatograph of liquid under above-mentioned chromatographic condition, measure, promptly.See accompanying drawing 7,8.
Further, concentration of phosphoric acid is 0.001～5% in the mobile phase that methanol-acetonitrile-phosphoric acid is formed, and optimizing concentration is 0.01～1%, and more excellent condition is 0.1～0.5%; Column temperature is 20～50 ℃, and optimizing temperature is 30～40 ℃, and more excellent temperature is 30 ℃; Solid-phase extraction column is analytically commonly used, comprises anti-phase solid-phase extraction column, silica gel positive solid-phase extraction column, aluminium oxide solid-phase extraction column, macroporous adsorbent resin solid-phase extraction column, activated carbon solid-phase extraction column, kieselguhr solid-phase extraction column etc.Optimizing solid-phase extraction column is anti-phase solid-phase extraction column, silica gel positive solid-phase extraction column, aluminium oxide solid-phase extraction column, macroporous adsorbent resin solid-phase extraction column.More optimizing solid-phase extraction column is anti-phase solid-phase extraction column, aluminium oxide solid-phase extraction column, macroporous adsorbent resin solid-phase extraction column.The optimization solid-phase extraction column is the aluminium oxide solid-phase extraction column.
Adopt that the Ramulus Cinnamomi Poria pill of the present invention's preparation has that production stage is few, with short production cycle, production mechanization degree height, advantage such as the quality of the pharmaceutical preparations is stable, patient's taking dose is little, taking convenience, patient are taken like a shot.Adopt the Ramulus Cinnamomi Poria pill of the present invention's preparation can well keep effective ingredient in the preparation, for the modified form of Chinese medicine pill provides new approach.
The specific embodiment
Further describe the present invention by the following examples, it should be understood that these embodiment only are used for the purpose of illustration, never limit the scope of the invention.
The preparation of embodiment 1. Ramulus Cinnamomi Poria pills
1. write out a prescription: Ramulus Cinnamomi 60g Poria 60g Radix Paeoniae 60g Cortex Moutan 60g Semen Persicae 60g
2. method for making: the above five tastes, Ramulus Cinnamomi, Poria, Cortex Moutan pulverize separately become fine powder, sieve, mixing, standby; Radix Paeoniae, Semen Persicae mixed powder are broken into fine powder, sieve, and be standby; Above-mentioned powder mixes is even, add 5% starch slurry wet granulation, put drying in 50 ℃ of baking ovens, granulate adds gross weight 4% carboxymethyl starch sodium and 0.4% magnesium stearate mix homogeneously, is pressed into 1000 balls, the bag film-coat, promptly.
3. character: this product is pink film-coat pill, and the ball core is shallow brown white, and gas is special, and it is sweet to distinguish the flavor of.
4. specification: 0.3g/ ball.
5. three batch samples have been prepared by above-mentioned production technology, production technology and physicochemical property such as following table
3 crowdes of production technology results
Three batches of result of the tests show that above-mentioned production technology is feasible.Be applicable to big production.
The preparation of embodiment 2. Ramulus Cinnamomi Poria pills
1. write out a prescription: Ramulus Cinnamomi 60g Poria 60g Radix Paeoniae 60g Cortex Moutan 60g Semen Persicae 60g
2. method for making: above five tastes pulverize separately becomes fine powder, sieves, and mixing, standby; Get the 45g Poria and add the 120ml deionized water, put and be heated to Poria dissolving and one-tenth thick liquid, Ramulus Cinnamomi, Semen Persicae and Indian Bread mixing granulation, oven dry, granulate in the water-bath; Add Radix Paeoniae fine powder, Cortex Moutan fine powder, 13.5g PVP (K29/32), 1.5g magnesium stearate, mix homogeneously.Be pressed into 1000 balls, the bag film-coat, promptly.
3. character: this product is pink film-coat pill, and the ball core is shallow brown white, and gas is special, and it is sweet to distinguish the flavor of.
4. specification: 0.3g/ ball.
5. three batch samples have been prepared by above-mentioned production technology, production technology and physicochemical property such as following table
3 crowdes of production technology results
The assay of cinnamic acid in embodiment 3 Ramulus Cinnamomi Poria pills
1. the Ramulus Cinnamomi Poria pill of embodiment 1 preparation is got in the preparation of need testing solution, removes coating, pulverize, precision takes by weighing 0.1g, puts in the 10ml measuring bottle, and it is an amount of to add 50% methanol, supersound extraction 30 minutes, take out, put, supply solvent to scale to room temperature, shake up, microporous filter membrane with 0.45 μ m filters, and filtrate is as need testing solution, promptly.
2. the preparation precision of reference substance solution takes by weighing cinnamic acid reference substance 1.68mg, to the brown measuring bottle of 100ml, with 50% dissolve with methanol and be diluted to scale, shake up, precision is measured 2ml, puts in the 5ml measuring bottle, add 50% methanol and be diluted to scale, shake up, promptly get (every 1ml contains cinnamic acid 7 μ g).
3. chromatographic condition
Chromatographic column: Dikma Diamonsil
TMC
18(4.6 * 250mm, 5 μ) post;
Mobile phase: the mixed solution of acetonitrile-0.1% phosphoric acid (40: 60);
Detect wavelength: 285nm flow velocity: 1.0ml/min; Column temperature: room temperature.
4. accurate respectively above-mentioned need testing solution and each the 10 μ l of need testing solution of drawing of algoscopy measure by above-mentioned chromatographic condition, the results are shown in Table
Cinnamic acid assay result in the Ramulus Cinnamomi Poria pill
Embodiment 4: content of paeoniflorin is measured in the Ramulus Cinnamomi Poria pill
1. the Ramulus Cinnamomi Poria pill under 2 of the embodiment is got in the preparation of need testing solution, removes coating, is ground into fine powder, gets 1.5g, the accurate title, decide, and puts in the 25ml tool plug conical flask, the accurate 75% ethanol 25ml that adds, weigh, ultrasonic 30min is put cold, weigh again, supply the weight that subtracts mistake with 75% ethanol, centrifugal, get supernatant 10ml and put evaporate to dryness in the hot bath, the accurate 2ml water dissolution that adds is crossed neutral alumina (2g) post, use 50% methanol-eluted fractions, collect eluent and put in the 10ml volumetric flask standardize solution.Cross 0.45 μ m microporous filter membrane, collect subsequent filtrate and promptly get need testing solution
[2]
2. the preparation of reference substance solution is accurate claims decide peoniflorin reference substance 1.01mg and puts and add dissolve with methanol in the 2ml volumetric flask and be diluted to scale, must reference substance solution.
3. chromatographic condition: chromatographic column: the Diamonsil C of Di Ma company
18Analytical column (250mm * 4.6mm, 5 μ m); Mobile phase: methanol-0.3% phosphoric acid solution (35: 65); Flow velocity: 1.0ml/min; Detect wavelength: 230nm; Column temperature: 30; Sample size: 10 μ l.
4. sample determination result
Paeoniflorin content measurement result in the Ramulus Cinnamomi Poria pill
Embodiment 5: the assay of paeonol and cinnamic aldehyde in the Ramulus Cinnamomi Poria pill
1. the paeonol reference substance decided in the accurate title of the preparation of reference substance solution, the cinnamic aldehyde reference substance is an amount of, adds dissolve with methanol and be prepared into every ml to contain paeonol 100 μ g, contains the solution of cinnamic aldehyde 50 μ g, promptly gets reference substance solution.
2. 2 following Ramulus Cinnamomi Poria pills of embodiment are got in the preparation of need testing solution, remove coating, porphyrize, get 0.5g, the accurate title, decide, put in the 50ml tool plug conical flask, the accurate 50% methanol 50ml that adds weighs, ultrasonic 30min, put coldly, weigh again, supply the weight that subtracts mistake with 50% methanol, centrifugal, get supernatant.Cross 0.45 μ m microporous filter membrane, collect subsequent filtrate and promptly get need testing solution.
3. chromatographic condition chromatographic column: the Diamonsil C of Di Ma company
18Analytical column (250mm * 4.6mm, 5 μ m); Mobile phase: acetonitrile-0.3% phosphoric acid solution (40: 60); Flow velocity: 1.0ml/min; Detect wavelength: 284nm; Column temperature: 30 ℃; Sample size: 5 μ l.
Cinnamic aldehyde assay result in the Ramulus Cinnamomi Poria pill
Description of drawings
Fig. 1 is the HPLC collection of illustrative plates (cinnamic acid, cinnamic aldehyde, paeonol) of Ramulus Cinnamomi Poria pill
Fig. 2 is the HPLC collection of illustrative plates of cinnamic acid reference substance solution
Fig. 3 is the HPLC collection of illustrative plates (cinnamic aldehyde, paeonol) of Ramulus Cinnamomi Poria pill
Fig. 4 is the HPLC collection of illustrative plates of paeonol reference substance solution
Fig. 5 is the HPLC collection of illustrative plates (peoniflorin) of Ramulus Cinnamomi Poria pill
Fig. 6 is the HPLC collection of illustrative plates of peoniflorin reference substance solution
Fig. 7 is the HPLC collection of illustrative plates (amygdaloside) of Ramulus Cinnamomi Poria pill
Fig. 8 is the HPLC collection of illustrative plates of amygdaloside reference substance solution
Claims (8)
1. the preparation method of a Ramulus Cinnamomi Poria pill.It is characterized in that the medical material and the preparation method of suppressing 1000 balls are:
(1) prescription is: Ramulus Cinnamomi 60g Poria 60g Cortex Moutan 60g Radix Paeoniae 60g Semen Persicae 60g
(2) get Ramulus Cinnamomi, Poria, Cortex Moutan, Radix Paeoniae, Semen Persicae medical material, choose decontamination and non-medicinal part respectively.
(3) get Ramulus Cinnamomi, Poria, Cortex Moutan, Radix Paeoniae Rubra, Semen Persicae medical material pulverize separately or mixed powder and be broken into fine powder, sieve, standby.
(4) get above-mentioned medical material fine powder, add binding agent and mix, granulate, drying, granulate, standby.
(5) get the granule for preparing, adding disintegrating agent and mix lubricant are even, put on the tablet machine, are pressed into a spherical ball.
(6) get the pill that step (4) is pressed into, the bag film-coat.
2. the described Ramulus Cinnamomi of claim 1 is dry twig or the bark of canella Cortex Cinnamomi Cinnamomum cassia Presl.
3. the described Cortex Moutan cohosh of claim 1 Paeonia suffruticosa is organized Paeonia suffruticosa Paeoniasuffrutico Andr., the Sichuan Paeonia suffruticosa P.szechuanica Fang. among the Sect.Paeonia, the dry root bark of Herba Melastomatis Candii P.delavayi Franch. and mutation thereof.The dry root bark of preferred Paeonia suffruticosa.
4. the described Radix Paeoniae cohosh of claim 1 Radix Paeoniae is organized the Radix Paeoniae Paeonia lactifloraPall. among the Sect.Paeonia, Paeonia mairei L P.mairei L é vl., Paeonia sterniana Fletcher in Journ. P.sterniana Fletcher., Paeonia obovata Maxim. P.obovata Maxim., Xinjiang Radix Paeoniae P.sinjiangensis K.Y.Pang., the dry root of Paeonia anomala P.anomala Linn. and CHUANSHAO medicine P.veitchii Lynch. and mutation thereof.The root bark of preferred Radix Paeoniae and CHUANSHAO medicine.
5. the described Ramulus Cinnamomi Poria pill of claim 1 is characterized in that the typical binders known for pharmaceutical field, also can select for use in the cassia twig tuckahoe prescription Poria as binding agent.More preferably pregelatinized starch, modified starch, dextrin, xanthan gum, sodium carboxymethyl cellulose, hydroxyethyl-cellulose, polyvidone, Poria.
6. the described Ramulus Cinnamomi Poria pill of claim 1 is characterized in that disintegrating agent is the disintegrating agent commonly used that pharmaceutical field is known, preferred starch, carboxymethyl starch, hydroxypropyl starch, polyvinylpolypyrrolidone, low-substituted hydroxypropyl cellulose, microcrystalline Cellulose.
7. the content control method of the described Ramulus Cinnamomi Poria pill of claim 1～6, it is characterized in that the content assaying method of cinnamic acid, cinnamic aldehyde and paeonol in this method is: the employing octadecylsilane chemically bonded silica is a filler; Acetonitrile-phosphoric acid solution is a mobile phase; The detection wavelength is 200～400nm.The preparation of need testing solution: get Ramulus Cinnamomi Poria pill, remove coating, pulverize, precision takes by weighing 0.1g, puts in the 10ml measuring bottle, it is an amount of to add 50% methanol, and supersound extraction 30 minutes is taken out, and puts to room temperature, supply solvent to groove, shake up, with the microporous filter membrane filtration of 0.45 μ m, promptly.The preparation of reference substance solution: precision takes by weighing cinnamic acid reference substance, cinnamic aldehyde reference substance, paeonol reference substance in addition, adds 50% dissolve with methanol and be prepared into to contain the solution that every ml solution contains cinnamic acid 10 μ g, cinnamic aldehyde 50 μ g, paeonol 100 μ g, promptly.Algoscopy: accurate respectively need testing solution, each 10 μ l of reference substance solution of drawing, under above-mentioned chromatographic condition, inject chromatograph of liquid, measure, promptly.
8. the content control method of the described Ramulus Cinnamomi Poria pill of claim 1～6, it is characterized in that the content of paeoniflorin assay method is in this method: the employing octadecylsilane chemically bonded silica is a filler; Methanol-phosphoric acid mobile phase; The detection wavelength is 230nm; Column temperature is 20～50.The preparation of need testing solution: get Ramulus Cinnamomi Poria pill fine powder 1.5g, the accurate title, decide, and puts in the 25ml tool plug conical flask, the accurate 75% ethanol 25ml that adds weighs ultrasonic 30min, put coldly, weigh again, supply the weight that subtracts mistake with 75% ethanol, centrifugal, get supernatant 10ml and put evaporate to dryness in the hot bath, the accurate 2ml water dissolution that adds, cross solid-phase extraction column, use methanol-eluted fractions, collect eluent and put in the 10ml volumetric flask standardize solution.Cross 0.45 μ m microporous filter membrane, collect subsequent filtrate and promptly get need testing solution.The preparation of reference substance solution: the accurate title, decided the peoniflorin reference substance, adds dissolve with methanol and be prepared into the solution that every ml contains 0.5mg, is reference substance solution.Algoscopy: accurate respectively need testing solution, each 10 μ l of reference substance solution of drawing, under above-mentioned chromatographic condition, inject chromatograph of liquid, measure, promptly.9. the content control method of the described Ramulus Cinnamomi Poria pill of claim 1～6, it is characterized in that the content assaying method of amygdaloside in this method is: the employing octadecylsilane chemically bonded silica is a filler; Mobile phase is methanol-acetonitrile-phosphoric acid solution system; The detection wavelength is 200～250nm; Column temperature is 20～40.The preparation of need testing solution: get Ramulus Cinnamomi Poria pill fine powder 3g, the accurate title, decide, and puts in the 50ml tool plug conical flask, the accurate 80% methanol 50ml that adds, weigh, place a night, weigh, supply the weight that subtracts mistake with 80% methanol, ultrasonic 30min is put cold, weigh again, supply the weight that subtracts mistake with 80% methanol, centrifugal, get supernatant 10ml and put evaporate to dryness in the hot bath, accurate 2ml water dissolution, the last solid-phase extraction column of adding, use 50% methanol-eluted fractions, collect eluent and put in the 10ml volumetric flask standardize solution.Cross 0.45 μ m microporous filter membrane, collect subsequent filtrate and promptly get need testing solution.The preparation of reference substance solution: the accurate title, decided the amygdaloside reference substance, adds methanol and be prepared into the solution that every ml contains 1mg, promptly gets reference substance solution.Algoscopy: accurate respectively need testing solution, each 10 μ l of reference substance solution of drawing, under above-mentioned chromatographic condition, inject chromatograph of liquid, measure, promptly.
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Application publication date: 20100224 |