CN102507777B - Quality control method for Weichang'an pills - Google Patents
Quality control method for Weichang'an pills Download PDFInfo
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- CN102507777B CN102507777B CN 201110340438 CN201110340438A CN102507777B CN 102507777 B CN102507777 B CN 102507777B CN 201110340438 CN201110340438 CN 201110340438 CN 201110340438 A CN201110340438 A CN 201110340438A CN 102507777 B CN102507777 B CN 102507777B
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Abstract
The invention relates to a quality control method for Weichang'an pills. The composition of the traditional Chinese medicine comprises costustoot, agilawood, bitter orange, sandalwood, rheum, magnolia bark, cinnabar, musk, defatted croton seed powder, fructus jujubae and rhizoma Chuanxiong. The quality of the Weichang'an pills can be effectively controlled by the quality control method.
Description
Technical field
The present invention relates to a kind of drug quality control method, relate to specifically a kind of method of quality control of gastrointestinal disease treating pill.
Background technology
Diarrhoea can be divided into infectious and non-infectious two classes.Infectious diarrhea is divided into again bacterium to be infected and virus infections; Noninfectious diarrhea then can be caused by the change of improper diet, food hypersenstivity, rule of life, abrupt change of climate even the many reasons such as nervous.Motherland's medical science thinks to have loose bowels and refers to that defecation frequency increases, ight soil is rare clearly, even such as water sample.The major lesions of having loose bowels is taste and intestine and small intestine.Its pathogenesis has being invaded by exogenous pathogen,invasion of exogenous pathogen, injury due to diet, seven human emotions discord, damp evil internal resistance and internal organs weakness etc.The clinical findings damp evil is caused a disease cold-dampness and damp and hot dividing.Spleen and stomach function is swollen to be hindered is to be caused by many factors, has outer evil impact, taste weakness itself, incoordination between the liver and the spleen and kidney intestines deficiency etc. all can cause spleen and stomach function not normal and have loose bowels.Enquiry data shows that diarrhoea incidence of disease in urban population reaches 0.4 time/people, and the people in the countryside incidence of disease reaches 0.5 time/people.Although diarrhoea is minor illness, pathogenic factor also is diversified, and changes with epoch, environment.Can say that the diarrhoea of today and the diarrhoea before 20 years have had the change of essence from pathogenesis.Along with the development in epoch, people's living standard attains the well-off standard substantially, and sanitary condition is improved greatly, fewer and feweri by the diarrhoea ratio that the bacterium infection causes, on the contrary, because rhythm of life is accelerated, struggle for existence is fierce, and the functional diarrhea ratio that pressure causes greatly obviously rises.One studies show that, the diarrhoeal diseases people of China about 30% needs antibiosis usually to treat, and 70% does not need should not use antibiotic therapy yet.The consumer also more and more notices the bad reaction of the products such as berberine, orfloxacin, and the harm that brings of abuse of antibiotics.Diarrhoea market is except the low side antibiotic products such as berberine, orfloxacin, some non-antibiotic products have also been introduced in recent years, close such as thinking: as to reach, Birid Triple Viable etc., but be positioned at high-end consumer groups, for most of consumer groups, its price positioning does not conform to the consumption location of such minor illness of suffering from diarrhoea with the consumer.Analysis expert thinks, mainly is take viral as main in urban market diarrhoea, and take bacterial infection as main, if according to the principle of the market segments, at present a lot of products all are difficult to cover the whole market in the rural area.For intestinal bacilli illness person, available little ecological active bacteria formulation provides beneficial bacterium, improves intestinal environment, improves intestinal absorption, motion state.As: bifidobacteria viable bacteria preparation (Bifidobiogen), Peifeikang Capsule, bacillus cicheniformis (whole intestines rubber capsule); The intestinal mucosa protective agent: two eight body smectites (dioctahedral smectite), the protection intestinal mucosa can suppress fixedly mycin, promotes the intestinal mucosal lesion reparation; Contain the creosote component preparation: the excessive secretion that can suppress intestinal juice.Gastrointestinal disease treating pill is mainly used in treating the diarrhoea that indigestion causes, enteritis, bacillary dysentery, abdominal fullness and distention, stomachache, dyspepsia breast is long-pending, its pharmacological action is higher than like product: anti diar rhea, antibiotic, antiviral, regulate four kinds of functions of gastrointestinal function and deposit.But the complicacy of Chinese medicine self component makes Chinese patent drug be difficult to guarantee the stable of its product quality.
Summary of the invention
Problem to be solved by this invention provides a kind of method of quality control of gastrointestinal disease treating pill, by this method of quality control, can control the quality of this gastrointestinal disease treating pill.
Gastrointestinal disease treating pill of the present invention is to be made by the bulk drug of following weight proportion: the banksia rose 100～600g, agalloch eaglewood 100～600g, Fructus Aurantii 100～600g, santal 90～360g, rheum officinale 90～360g, cinnabar 75～300g, the bark of official magnolia 100～600g, Moschus 4.5～18g, defatted croton seed powder 60～240g, Ligusticum wallichii 90～360g and date 500～2000g.
The preferred gastrointestinal disease treating pill of the present invention is to be made by the bulk drug of following weight proportion: banksia rose 300g, agalloch eaglewood 300g, Fructus Aurantii 300g, santal 180g, rheum officinale 180g, cinnabar 150g, bark of official magnolia 300g, Moschus 9g, defatted croton seed powder 120g, Ligusticum wallichii 180g and date 1000g.
The gastrointestinal disease treating pill of the best of the present invention, Fructus Aurantii wherein are stir-baked FRUCTUS AURANTII in bran; The bark of official magnolia is that ginger is processed the bark of official magnolia; Date is that date, the Moschus of stoning is the muscone.
The method of quality control of gastrointestinal disease treating pill of the present invention, wherein the method comprises one or both in the following assay:
A, forulic acid C
10H
10O
4The mensuration of content:
Use high effective liquid chromatography for measuring: be filling agent with octadecylsilane chemically bonded silica; Acetonitrile-0.085% phosphoric acid is mobile phase; The detection wavelength is 316nm; Number of theoretical plate calculates by the forulic acid peak should be not less than 5000;
The preparation of reference substance solution: get forulic acid reference substance 5～20mg, put in 50～200ml measuring bottle, add the dissolving of 35～85% methyl alcohol and be diluted to scale, shake up; Get forulic acid reference substance solution 1.5～6ml and put in 20～100ml measuring bottle, add 35～85% methyl alcohol to scale, shake up, and get final product;
The preparation of need testing solution: get this product powder 1～4g, accurately weighed, put in 50～200mL tool plug conical flask accurate 35～85% methyl alcohol, the 10～50ml that adds, weighed weight, ultrasonic processing 15～60 minutes lets cool, more weighed weight, supply the weight that subtracts mistake with 35～85% methyl alcohol, shake up, filter through filter membrane, and get final product;
Determination method: precision is drawn reference substance solution and each 2.5～10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product;
B, archen C
15H
10O
5With Chrysophanol C
15H
10O
4The mensuration of content:
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filling agent; Methyl alcohol-0.1% phosphoric acid is mobile phase; The detection wavelength is 254nm; Number of theoretical plate calculates by the archen peak should be not less than 3000;
The preparation of reference substance solution: precision takes by weighing archen reference substance 5～20mg, and Chrysophanol reference substance 7.5～30mg puts respectively in 50～200ml measuring bottle, with methyl alcohol dissolving and be diluted to scale, shakes up; Precision is measured archen respectively, each 0.5～2ml of Chrysophanol solution puts in 5～20ml measuring bottle, adds methyl alcohol to scale, shakes up, and get final product;
The preparation of need testing solution: get this product powder 1～4g, accurately weighed, put in 50～200mL tool plug conical flask, the accurate methyl alcohol 10～50ml that adds, weighed weight added hot reflux 0.5～2 hour, let cool, weighed weight is supplied the weight that subtracts mistake with methyl alcohol again, shake up, filter, precision is measured subsequent filtrate 2.5～10ml again, put in the flask, fling to solvent, add 4～16% hydrochloric acid solutions, 5～20ml, ultrasonic processing 1～4 minute, with a small amount of methenyl choloride washing container, incorporate in the separating funnel, divide and get the methenyl choloride layer, acid solution is extracted 2～3 times with methenyl choloride again, each 5～20mL merges methenyl choloride liquid, and decompression and solvent recovery is to doing, residue adds methyl alcohol makes dissolving, be transferred in 5～20ml volumetric flask, add methyl alcohol to scale, shake up, filter through filter membrane, and get final product;
Determination method: precision is drawn reference substance solution and each 2.5～10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The method of quality control of the preferred gastrointestinal disease treating pill of the present invention, wherein the method comprises one or both in the following assay:
A, forulic acid C
10H
10O
4The mensuration of content:
Use high effective liquid chromatography for measuring: be filling agent with octadecylsilane chemically bonded silica; Acetonitrile-0.085% phosphoric acid is mobile phase; The detection wavelength is 316nm; Number of theoretical plate calculates by the forulic acid peak should be not less than 5000;
The preparation of reference substance solution: get forulic acid reference substance 8～12mg, put in 80～120ml measuring bottle, add the dissolving of 50～75% methyl alcohol and be diluted to scale, shake up; Get forulic acid reference substance solution 2～4ml and put in 40～60ml measuring bottle, add 50～75% methyl alcohol to scale, shake up, and get final product;
The preparation of need testing solution: get this product powder 1.5～3g, accurately weighed, put in 80～120mL tool plug conical flask accurate 50～75% methyl alcohol, the 20～30ml that adds, weighed weight, ultrasonic processing 20～40 minutes lets cool, more weighed weight, supply the weight that subtracts mistake with 50～75% methyl alcohol, shake up, filter through filter membrane, and get final product;
Determination method: precision is drawn reference substance solution and each 4～6 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product;
B, archen C
15H
10O
5With Chrysophanol C
15H
10O
4The mensuration of content:
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filling agent; Methyl alcohol-0.1% phosphoric acid is mobile phase; The detection wavelength is 254nm; Number of theoretical plate calculates by the archen peak should be not less than 3000;
The preparation of reference substance solution: precision takes by weighing archen reference substance 8～12mg, and Chrysophanol reference substance 10～20mg puts respectively in 80～120ml measuring bottle, with methyl alcohol dissolving and be diluted to scale, shakes up; Precision is measured archen respectively, each 0.8～1.5ml of Chrysophanol solution puts in 8～15ml measuring bottle, adds methyl alcohol to scale, shakes up, and get final product;
The preparation of need testing solution: get this product powder 1.5～3g, accurately weighed, put in 80～120mL tool plug conical flask, the accurate methyl alcohol 20～30ml that adds, weighed weight added hot reflux 0.5～1.5 hour, let cool, weighed weight is supplied the weight that subtracts mistake with methyl alcohol again, shake up, filter, precision is measured subsequent filtrate 4～6ml again, put in the flask, fling to solvent, add 6～10% hydrochloric acid solutions, 8～15ml, ultrasonic processing 1～3 minute, with a small amount of methenyl choloride washing container, incorporate in the separating funnel, divide and get the methenyl choloride layer, acid solution is extracted 3 times with methenyl choloride again, each 8～12mL merges methenyl choloride liquid, and decompression and solvent recovery is to doing, residue adds methyl alcohol makes dissolving, be transferred in 8～15ml volumetric flask, add methyl alcohol to scale, shake up, filter through filter membrane, and get final product;
Determination method: precision is drawn reference substance solution and each 4～6 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The method of quality control of the preferred gastrointestinal disease treating pill of the present invention, wherein the method comprises one or both in the following assay:
A, forulic acid C
10H
10O
4Mensuration:
Use high effective liquid chromatography for measuring: be filling agent with octadecylsilane chemically bonded silica; Acetonitrile-0.085% phosphoric acid is mobile phase, wherein acetonitrile: 0.085% phosphoric acid volume ratio is 17: 83; The detection wavelength is 316nm; Number of theoretical plate calculates by the forulic acid peak should be not less than 5000;
The preparation of reference substance solution: get forulic acid reference substance 10mg, put in the 100ml measuring bottle, add the dissolving of 70% methyl alcohol and be diluted to scale, shake up; Get forulic acid reference substance solution 3ml and put in the 50ml measuring bottle, add 70% methyl alcohol to scale, shake up, and get final product;
The preparation of need testing solution: get this product powder 2g, accurately weighed, put in the 100mL tool plug conical flask the accurate 70% methyl alcohol 25ml that adds, weighed weight, ultrasonic processing 30 minutes lets cool, more weighed weight, supply the weight that subtracts mistake with 70% methyl alcohol, shake up, filter through 0.45 μ m filter membrane, and get final product;
Determination method: precision is drawn reference substance solution and each 5 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product;
B, archen C
15H
10O
5With Chrysophanol C
15H
10O
4Mensuration:
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filling agent; Methyl alcohol-0.1% phosphoric acid is mobile phase, wherein methyl alcohol: 0.1% phosphoric acid volume ratio is 85: 15; The detection wavelength is 254nm; Number of theoretical plate calculates by the archen peak should be not less than 3000;
The preparation of reference substance solution: precision takes by weighing archen reference substance 10mg, and Chrysophanol reference substance 15mg puts respectively in the 100ml measuring bottle, with methyl alcohol dissolving and be diluted to scale, shakes up; Precision is measured archen respectively, each 1ml of Chrysophanol solution puts in the 10ml measuring bottle, adds methyl alcohol to scale, shakes up, and get final product;
The preparation of need testing solution: get the about 2g of this product powder (crossing 80 mesh sieves), accurately weighed, put in the 100mL tool plug conical flask, the accurate methyl alcohol 25ml that adds, weighed weight added hot reflux 1 hour, let cool, weighed weight is supplied the weight that subtracts mistake with methyl alcohol again, shake up, filter, precision is measured subsequent filtrate 5ml again, put in the flask, fling to solvent, add 8% hydrochloric acid solution 10ml, ultrasonic processing 2 minutes, with a small amount of methenyl choloride washing container, incorporate in the separating funnel, divide and get the methenyl choloride layer, acid solution is extracted three times with methenyl choloride again, each 10mL merges methenyl choloride liquid, and decompression and solvent recovery is to doing, residue adds methyl alcohol makes dissolving, be transferred in the 10ml volumetric flask, add methyl alcohol to scale, shake up, filter through 0.45 μ m filter membrane, and get final product;
Determination method: precision is drawn reference substance solution and each 5 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The method of quality control of gastrointestinal disease treating pill of the present invention can also comprise following assay in the method for above-mentioned assay:
Magnolol C
18H
18O
2With honokiol C
18H
18O
2Assay:
Chromatographic condition and system suitability: be filling agent with octadecylsilane chemically bonded silica; Methyl alcohol-acetonitrile-water is mobile phase, and the ratio of methyl alcohol-acetonitrile-water is 50: 20: 40; The detection wavelength is 294nm; Number of theoretical plate calculates by the magnolol peak should be not less than 4000;
The preparation of reference substance solution: get respectively the magnolol reference substance, the honokiol reference substance is an amount of, and is accurately weighed, add methyl alcohol and make respectively every 1ml and contain magnolol 60 μ g, every 1ml and contain the solution of honokiol 10 μ g, and get final product;
The preparation of need testing solution: get this product 3g, porphyrize is got 0.5g, and is accurately weighed, put in the tool plug conical flask accurate chloroform 50ml, the weighed weight of adding, hold over night, ultrasonic processing 1.5 hours lets cool, weighed weight is supplied the weight that subtracts mistake with chloroform again, filters, precision is measured subsequent filtrate 15ml, evaporate to dryness, and residue dissolves with methyl alcohol and is transferred in the 5ml measuring bottle, add methyl alcohol to scale, shake up, and get final product;
Determination method: precision is drawn reference substance solution and each 20 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
In the method for quality control of gastrointestinal disease treating pill of the present invention, the configuration proportion of mobile phase solution is to prepare by volume.
In the method for quality control of gastrointestinal disease treating pill of the present invention, the every gram of this product gastrointestinal disease treating pill contains Ligusticum wallichii with forulic acid C
10H
10O
4Meter must not be less than 0.040mg.
In the method for quality control of gastrointestinal disease treating pill of the present invention, the every gram of this product gastrointestinal disease treating pill contains rheum officinale with archen C
15H
10O
5With Chrysophanol C
15H
10O
4The total amount meter must not be less than 0.20mg.
In the method for quality control of gastrointestinal disease treating pill of the present invention, the every gram of this product gastrointestinal disease treating pill contains the bark of official magnolia with magnolol C
18H
18O
2With honokiol C
18H
18O
2The total amount meter, must not be less than 1.0mg.
This product described in the present invention refers to gastrointestinal disease treating pill.
To those skilled in the art, technology contents disclosed according to the present invention, those skilled in the art will very clear other embodiment of the present invention, and the embodiment of the invention is only as example.In the situation of not violating purport of the present invention and scope, can carry out various changes and improvements to the present invention.For example, the measurement result of using different detecting instruments to obtain may be different, but as long as use method of quality control of the present invention, all within protection domain of the present invention.
For the present invention, control according to method of quality control provided by the invention the gastrointestinal disease treating pill sergeant the peace strychnia content with control gastrointestinal disease treating pill of the present invention quality, with the curative effect of true gastrointestinal disease treating pill.
Below by medicine gastrointestinal disease treating pill of the present invention (obtaining according to embodiment 6 preparation methods) active constituent content measuring the beneficial effect of content assaying method of the present invention is described.
Test example 1
1. raw material (medicinal material) quality standard
1.1 the banksia rose
This product is the dry root of feverfew banksia rose Aucklandia lappa Decne..Autumn, two seasons of winter excavate, and remove silt and fibrous root, segment, and large again vertical profile becomes lobe, hits tertia after the drying.
This product should meet the relevant regulations under the 41st page of banksia rose item of Chinese Pharmacopoeia version First in 2005.
1.2 agalloch eaglewood
This product is the timber that Isolated From Thymelaeaceae Species suspension culture of Aquilaria sinensis Aquilaria sinensis (Lour.) Gilg contains resin.All can gather the whole year, extracts resiniferous timber, removes not resiniferous part, dries in the shade.
This product should meet the relevant regulations under the 128th page of agalloch eaglewood item of Chinese Pharmacopoeia version First in 2005.
1.3 Fructus Aurantii (bran stir-fry)
This product is the dry immature fruit of rutaceae bitter orange Citrus aurantium L. and variety thereof.Gather when pericarp is still green July, is two halves from the middle part crosscut, dries or low temperature drying.
[process of preparing Chinese medicine] Fructus Aurantii is removed impurity, cleans, run through, shave, dry after sieve remove the broken flesh nuclear that falls.
This product is irregular arcuation bar shaped thin slice, reaches 5cm, the wide 1.3cm that reaches.Tangent plane exocarp sepia is to brown, and the mesocarp yellow-white is to yellowish-brown, and nearly outer rim has 1～2 row point-like grease chamber, and the inboard has a small amount of puce pulp.
Stir-baked FRUCTUS AURANTII in bran is got the Fructus Aurantii sheet, fries method (appendix II D) according to bran and fries to look and deepen.
This product is irregular arcuation bar shaped thin slice, and look darker, and what have has a focal spot.
This product should meet the relevant regulations under the 171st page of Fructus Aurantii item of Chinese Pharmacopoeia version First in 2005.
1.4 santal
This product is the heartwood of Santalaceae plant santal Santalum album L. trunk.
This product should meet the relevant regulations under the 264th page of santal item of Chinese Pharmacopoeia version First in 2005.
1.5 rheum officinale
This product is the dry root and rhizome of the ancient especially big yellow Rheum tanguticum Maxim.ex Balf. of polygonum rheum palmatum Rheum palmatum L., Tang or Rheum officinale Rheum officinale Baill..Autumn Mo in the withered or inferior spring of cauline leaf excavates before germinateing, and removes radicula, scrapes off crust, valve cutting or section, and rope is worn bunchiness drying or convection drying.
This product should meet the relevant regulations under the 17th page of rheum officinale item of Chinese Pharmacopoeia version First in 2005.
1.6 the bark of official magnolia (ginger system)
This product is dry dry hide, Gen Pi and the branch skin of Magnoliacea plant bark of official magnolia Magnolia officinalis Rehd.et Wils. or Magnolia bilola Magnolia officinalisRehd.et Wils.var.biloba Rehd.et Wils..Strip 4～June, Gen Pi and branch skin Directly Dried in Shadow; Dry hide is put in the boiling water after little the boiling, the dark and damp place of banking up, and " sweating " during to inside surface purpling brown or sepia, steams softly, takes out, and is rolled into tubular, drying.
[process of preparing Chinese medicine] bark of official magnolia scrapes off tertia, cleans, and runs through, and chopping is dried.
This product is crooked strand shape, section fibrous, outside surface yellowish-brown, the dark purple brown of interior table.
Stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice is got bark of official magnolia silk, according to stir frying with ginger juice method (appendix II D) fried dry.
This product is crooked strand shape, and section fibrous is puce.
This product should meet the relevant regulations under the 176th page of bark of official magnolia item of Chinese Pharmacopoeia version First in 2005.
1.7 cinnabar
This product is sulfide-based mineral cinnabar family cinnabar, main Containing Sulfur mercury (HgS).After excavating, choose pure person, with the impurity of magnet exhaustion iron content, water is washed in a pan impurity elimination stone and silt again.
This product should meet the relevant regulations under the 92nd page of cinnabar item of Chinese Pharmacopoeia version First in 2005.
1.8 Moschus
This product is the dry secretion in the ripe male body note capsule of animal in deer family woods musk deer Moschus berezovskii Flerov, horse musk deer Moschus sifanicus Przewalski or former musk deer Moschus moschiferus Linnaeus.How wild musk deer is hunted to time spring in the winter time, after trapping, extracts sachet, dries in the shade, and practises claiming " hair shell Moschus "; Cut sachet open, remove softgel shell, practise title " Moschus benevolence ".The family musk deer is directly taken out Moschus benevolence from its sachet, dry in the shade or use the exsiccator close drying.
This product should meet the relevant regulations under the 266th page of Moschus item of Chinese Pharmacopoeia version First in 2005.
1.9 defatted croton seed powder
This product is the Preparation process product of crotons.
This product should meet the relevant regulations under the 55th page of defatted croton seed powder item of Chinese Pharmacopoeia version First in 2005.
1.10 date (stoning)
This product is the dry mature fruit of Rhamnaceae plant jujube Ziziphus jujuba Mill..Gather during fruit maturation autumn, dries.
[process of preparing Chinese medicine] removes impurity, cleans, and dries.Time spent breaks or stoning.
This product should meet the relevant regulations under the 15th page of date item of Chinese Pharmacopoeia version First in 2005.
1.11 Ligusticum wallichii
This product is the dry rhizome of samphire Ligusticum wallichii Ligusticum chuanxiong Hort..Summer, the joint dish on the stem was significantly outstanding, and slightly excavated during purple, removed silt, and a heatable brick bed done after shining, and removes fibrous root again.
This product should meet the relevant regulations under the 28th page of Ligusticum wallichii item of Chinese Pharmacopoeia version First in 2005.
[assay] measured according to high performance liquid chromatography (appendix VI D).
1. instrument and reagent
1.1 instrument condition
Instrument: Shimadzu LC-2010AHT type high performance liquid chromatograph
Detecting device: UV/VIS
Detect wavelength: 316nm
Flow velocity: 0.80mL/min
Column temperature: 25 ℃
Post is pressed: 6.2Mpa
Sample size: 5 μ L
Ultrasound Instrument: KUDOS SK8200LH (Shanghai High Kudos Science Instrument Co., Ltd.)
Electronic balance: Sartorius CP225D/CP224S (Beijing Sai Duolisi instrument system company limited)
1.2 chromatographic condition
Chromatographic column: Diamonsil 5 μ C18 250 * 4.6mm
Mobile phase: acetonitrile-0.085% phosphoric acid (17: 83)
1.3 reagent and reagent
Forulic acid reference substance lot number: 110773-200611;
All available from Nat'l Pharmaceutical ﹠ Biological Products Control Institute (for assay)
It is pure that reagent is analysis; Acetonitrile is chromatographically pure (fisher science); Water is deionized water.
Gastrointestinal disease treating pill: (lot number: 20070625,20080425,20080429); Provided by Lerentang Pharmaceutical Factory, Zhongxin Pharmaceutical Group Co., Ltd., Tianj.
2. the investigation of experimental technique
2.1 chromatographic condition and system suitability
Be filling agent with octadecylsilane chemically bonded silica; Acetonitrile-0.085% phosphoric acid (17: 83) is mobile phase; The detection wavelength is 316nm.Number of theoretical plate calculates by the forulic acid peak should be not less than 5000.
2.2 the selection of extraction conditions
Because Ligusticum wallichii is that former powder is used as medicine, and the 28th page of Ligusticum wallichii of Chinese Pharmacopoeia version First in 2005 be without [assay], thus this experiment according to the 89th page of Chinese Pharmacopoeia version First in 2005 be all samphire when being classified as reference and according to preparing test sample under [assay] need testing solution preparation.
2.3 the selection of condition determination
2.3.1 the selection of mobile phase
Experimental result shows that with acetonitrile-0.085% phosphoric acid (17: 83) be mobile phase, and the forulic acid chromatographic peak separates well with the chromatographic peak of other compositions.
2.3.2 the selection of wavelength
According to selecting 316nm for detecting wavelength under the assay item of the 89th page of Radix Angelicae Sinensis of Chinese Pharmacopoeia version First in 2005.
2.3.3 the preparation of reference substance solution
The preparation of forulic acid reference substance stock solution: take by weighing forulic acid reference substance 25.65mg, accurately weighed, put in the 100mL measuring bottle, add the methyl alcohol dissolving and be diluted to scale, shake up, make the reference substance solution that every 1mL contains 0.2565mg, as forulic acid reference substance stock solution.
The preparation of forulic acid reference substance solution: precision is measured above-mentioned reference substance stock solution 1mL and is put in the 25mL measuring bottle, adds methyl alcohol and is diluted to scale, shakes up, and makes the reference substance solution that every 1mL contains 0.01026mg, as the forulic acid reference substance solution.
2.4 methodology experiment
2.4.1 chromatographic condition and system suitability experiment
Be filling agent with octadecylsilane chemically bonded silica; Acetonitrile-0.085% phosphoric acid (17: 83) is mobile phase; The detection wavelength is 316nm.Number of theoretical plate calculates by the forulic acid peak should be not less than 5000.
2.4.2 linear relationship is investigated
Accurate above-mentioned reference substance solution 1.0,2.0,4.0,5.0,6.0,8.0, the 10.0 μ l of drawing, peak area is measured in successively sample introduction analysis, the results are shown in Table 1.
Take sample size as horizontal ordinate, peak area is ordinate, and the drawing standard curve is seen Fig. 1.
Learn by statistics and calculate regression equation: Y=7.236 * 10
6 X-3.643 * 10
3
r＝0.9999
The result shows that forulic acid is good in 0.01026～0.1026 μ g scope internal linear relation.
2.4.3 precision test
Forulic acid reference substance precision test
Accurate forulic acid (concentration is 10.26 μ g/ml) the reference substance solution 5 μ L that draw repeat sample introduction 6 times, measure the peak area integrated value by above-mentioned chromatographic condition, and calculating relative standard deviation is 1.78%, the results are shown in Table 2.
Table 2 forulic acid reference substance Precision Experiment result
Experimental result shows that the precision peak area mean value of reference substance is 372200; Relative standard deviation is 1.78%, meets the requirements.
Sample precision test (forulic acid)
Accurate need testing solution (lot number is 20070625) the 5 μ L that draw repeat sample introduction 6 times, measure the peak area integrated value by above-mentioned chromatographic condition, and calculating relative standard deviation is 1.96%, the results are shown in Table 3.
Table 3 sample Precision Experiment result
Experimental result shows that the peak area mean value of forulic acid is 174467.3 in the sample; Relative standard deviation is 1.96%, meets the requirements.
2.4.4 recovery test
(lot number is: 20070625 to get this product powder; Cross 80 mesh sieves) 1g, totally 6 parts, accurately weighed, put in the 25ml measuring bottle, add respectively an amount of (C=0.2565mg/mL of forulic acid reference substance; V=0.50mL), press the test sample preparation and measure a lower operation, calculate recovery rate, the forulic acid recovery is 99.60%, relative standard deviation RSD is 0.50%, the results are shown in Table 4
Table 4 forulic acid recovery test result
Experimental result shows that the forulic acid recovery is 99.60%, and relative standard deviation RSD is 0.50%, meets the requirements.
2.4.5 reappearance test
(lot number is: sample powder 20070625) (crossing 80 mesh sieves) takes by weighing 6 parts, about 2.0g to get same lot number, accurately weighed, press the test sample preparation and measure a lower operation, measure the peak area integrated value, the relative standard deviation of calculating forulic acid is 1.51%, the results are shown in Table 5.
Table 5 reproducible test results (n=2)
Experimental result shows that reappearance experiment relative standard deviation RSD is 1.87%, meets the requirements.
2.4.6 specificity test
Get flavour of a drug except Ligusticum wallichii by sample prescription, prepare negative sample according to [method for making] lower operation, make the negative control sample by the test sample preparation method, measure with the chromatographic condition identical with test sample, the result shows that the forulic acid of negative control sample in Ligusticum wallichii goes out the place, peak without the peak, sees accompanying drawing.
2.4.7 stability test
With the need testing solution sample introduction analysis for preparing, every 2 hours sample introductions, measure the peak area integrated value by above-mentioned chromatographic condition, calculating relative standard deviation RSD is 1.53%.Show that test sample is stable in 8 hours, the results are shown in Table 6.
Table 6 stability test result
Experimental result shows that stability experiment relative standard deviation RSD is 0.90%, meets the requirements.
2.4.8 the assay result of forulic acid in the different lot number gastrointestinal disease treating pills
The preparation precision of reference substance solution takes by weighing forulic acid reference substance 10mg, puts in the 100ml measuring bottle, adds the dissolving of 70% methyl alcohol and is diluted to scale, shakes up; Precision is measured forulic acid reference substance solution 3ml and is put in the 50ml measuring bottle, adds 70% methyl alcohol to scale, shakes up, and namely gets (every 1ml contains forulic acid 6 μ g).
The about 2g of this product powder (crossing 80 mesh sieves) is got in the preparation of need testing solution, accurately weighed, put in the 100mL tool plug conical flask the accurate 70% methyl alcohol 25ml that adds, weighed weight, ultrasonic processing 30 minutes lets cool, more weighed weight, supply the weight that subtracts mistake with 70% methyl alcohol, shake up, filter through 0.45 μ m filter membrane, and get final product.
Determination method is accurate reference substance solution and each 5 μ l of need testing solution of drawing respectively, and the injection liquid chromatography is measured, and be get final product.Measure altogether the content of forulic acid in 3 batches of gastrointestinal disease treating pills, the results are shown in Table 7.
Ferulaic acid content measurement result in table 7 sample
Limit the quantity of: the every gram of this product contains Ligusticum wallichii with forulic acid (C
10H
10O
4) must not count and be less than 0.040mg.
180g * 0.10% (supposing theoretical value) ÷ 3019g=0.05962mg/g (theoretical content value)
Active constituent content measuring in test example 2 this product
[assay] measured according to high performance liquid chromatography (appendix VI D).
1. instrument and reagent
1.1 instrument condition
Instrument: Shimadzu LC-2010AHT type high performance liquid chromatograph
Detecting device: UV/VIS
Detect wavelength: 254nm
Flow velocity: 1.0mL/min
Column temperature: 40 ℃
Post is pressed: 6.0Mpa
Sample size: 5 μ L
Ultrasound Instrument: KUDOS SK8200LH (Shanghai High Kudos Science Instrument Co., Ltd.)
Electronic balance: Sartorius CP225D/CP224S (Beijing Sai Duolisi instrument system company limited)
1.2 chromatographic condition
Chromatographic column: Diamonsil 5 μ C18 250 * 4.6mm
Mobile phase: methyl alcohol-0.1% phosphoric acid (85: 15)
1.3 reagent and reagent
Archen reference substance lot number is: 110756-200110
Chrysophanol reference substance lot number is: 110796-200615
All available from Nat'l Pharmaceutical ﹠ Biological Products Control Institute (for assay)
It is pure that reagent is analysis; Methyl alcohol is chromatographically pure (fisher science); Water is deionized water.
Gastrointestinal disease treating pill: (lot number: 20070625,20080425,20080429); Provided by Lerentang Pharmaceutical Factory, Zhongxin Pharmaceutical Group Co., Ltd., Tianj.
2. the investigation of experimental technique
2.1 chromatographic condition and system suitability
Be filling agent with octadecylsilane chemically bonded silica; Methyl alcohol-0.1% phosphoric acid (85: 15) is mobile phase; The detection wavelength is 254nm.Number of theoretical plate calculates by the archen peak should be not less than 3000.
2.2 the selection of extraction conditions
Because rheum officinale is that former powder is used as medicine, so this experiment is according to preparing test sample under the 17th page of rheum officinale assay need testing solution of Chinese Pharmacopoeia version First in 2005 preparation.
2.3 the selection of condition determination
2.3.1 the selection of mobile phase
Experimental result shows that with methyl alcohol-0.1% phosphoric acid (85: 15) be mobile phase, and archen separates well with the chromatographic peak of other compositions with the Chrysophanol chromatographic peak.
2.3.2 the selection of wavelength
According to selecting 254nm for detecting wavelength under the assay item of the 17th page of rheum officinale of Chinese Pharmacopoeia version First in 2005.
2.3.3 the preparation of reference substance solution
The preparation of archen reference substance stock solution: take by weighing archen reference substance 10.10mg, accurately weighed, put in the 100mL measuring bottle, add the methyl alcohol dissolving and be diluted to scale, shake up, make every 1mL and contain the reference substance solution of 0.1010mg as archen reference substance stock solution.
The preparation of Chrysophanol reference substance stock solution: take by weighing Chrysophanol reference substance 16.18mg, accurately weighed, put in the 100mL measuring bottle, add the methyl alcohol dissolving and be diluted to scale, shake up, make every 1mL and contain the reference substance solution of 0.1618mg as Chrysophanol reference substance stock solution.
Archen and Chrysophanol mix the preparation of reference substance solution: above-mentioned each 1mL of reference substance stock solution of accurate absorption puts in the same 10mL measuring bottle, add methyl alcohol and be diluted to scale, shake up, make the mixing reference substance solution that every 1mL contains archen 10.10 μ g and Chrysophanol 16.18 μ g.
2.4 methodology experiment
2.4.1 chromatographic condition and system suitability experiment
Be filling agent with octadecylsilane chemically bonded silica; Methyl alcohol-0.1% phosphoric acid (85: 15) is mobile phase; The detection wavelength is 254nm.Number of theoretical plate calculates by the archen peak should be not less than 3000.
2.4.2 linear relationship is investigated
Archen is linear
Accurate above-mentioned reference substance solution 1.0,2.0,4.0,6.0,8.0, the 10.0 μ l of drawing, peak area is measured in successively sample introduction analysis, the results are shown in Table 8.
Table 8 archen linear relationship is investigated the result
Take sample size as horizontal ordinate, peak area is ordinate, and the drawing standard curve is seen Fig. 6.
Learn by statistics and calculate regression equation: Y=4.778 * 10
6 X-6.730 * 10
3
r＝0.9999
The result shows that archen is good in 0.01010～0.1010 μ g scope internal linear relation.
Chrysophanol is linear
Accurate above-mentioned reference substance solution 1.0,2.0,4.0,6.0,8.0, the 10.0 μ l of drawing, peak area is measured in successively sample introduction analysis, the results are shown in Table 9.
Table 9 Chrysophanol linear relationship is investigated the result
Take sample size as horizontal ordinate, peak area is ordinate, and the drawing standard curve is seen Fig. 7.
Learn by statistics and calculate regression equation: Y=6.599 * 10
6 X-2.215 * 10
4
r＝0.9999
The result shows that archen is good in 0.01618～0.1618 μ g scope internal linear relation.
2.4.3 precision test
Reference substance precision test (archen)
Accurate archen (concentration is 10.10 μ g/ml) the reference substance solution 5 μ L that draw repeat sample introduction 6 times, measure the peak area integrated value by above-mentioned chromatographic condition, and calculating relative standard deviation is 1.48%, the results are shown in Table 10.
Table 10 Precision Experiment result
Experimental result shows that reference substance precision relative standard deviation is 1.48%, meets the requirements.
Reference substance precision test (Chrysophanol)
Accurate archen (concentration is 16.18 μ g/ml) the reference substance solution 5 μ L that draw repeat sample introduction 6 times, measure the peak area integrated value by above-mentioned chromatographic condition, and calculating relative standard deviation is 1.40%, the results are shown in Table 11.
Table 11 Precision Experiment result
Experimental result shows that reference substance precision relative standard deviation is 1.40%, meets the requirements.
Sample precision test (archen)
Accurate need testing solution (lot number is 20070625) the 5 μ .L that draw repeat sample introduction 6 times, measure the peak area integrated value by above-mentioned chromatographic condition, and calculating relative standard deviation is 1.05%, the results are shown in Table 12.
Table 12 sample Precision Experiment result
Experimental result shows that reference substance precision relative standard deviation is 1.05%, meets the requirements.
Sample precision test (Chrysophanol)
Accurate need testing solution (lot number is 20070625) the 5 μ L that draw repeat sample introduction 6 times, measure the peak area integrated value by above-mentioned chromatographic condition, and calculating relative standard deviation is 0.38%, the results are shown in Table 13.
Table 13 sample Precision Experiment result
Experimental result shows that reference substance precision relative standard deviation is 0.38%, meets the requirements.
2.4.4 recovery test (archen)
(lot number is: 20070625 to get this product powder; Cross 80 mesh sieves) 1g, totally 6 parts, accurately weighed, it is an amount of to add respectively the archen reference substance, and press the test sample preparation and measure a lower operation, calculate recovery rate, the archen recovery is 96.77%, relative standard deviation RSD is 0.10%, the results are shown in Table 14.
Table 14 archen recovery test result
Experimental result shows that the archen recovery is 96.77%, and relative standard deviation RSD is 0.10%, meets the requirements.
Recovery test (Chrysophanol)
(lot number is: 20070625 to get this product powder; Cross 80 mesh sieves) 1g, totally 6 parts, accurately weighed, it is an amount of to add respectively the Chrysophanol reference substance, and press the test sample preparation and measure a lower operation, calculate recovery rate, the Chrysophanol recovery is 97.94%, relative standard deviation RSD is 1.69%, the results are shown in Table 15.
Table 15 archen recovery test result
Experimental result shows that the Chrysophanol recovery is 97.94%, and relative standard deviation RSD is 1.69%, meets the requirements.
2.4.5 reappearance test (archen)
(lot number is: sample powder 20070625) (crossing 80 mesh sieves) takes by weighing 6 parts, about 2.0g to get same lot number, accurately weighed, press the test sample preparation and measure a lower operation, measure the peak area integrated value, the relative standard deviation of calculating archen is 1.51%, the results are shown in Table 16.
Table 16 reproducible test results (n=2)
Experimental result shows that reappearance experiment relative standard deviation RSD is 1.51%, meets the requirements.
Reappearance test (Chrysophanol)
(lot number is: sample powder 20070625) (crossing 80 mesh sieves) takes by weighing 6 parts, about 2.0g to get same lot number, accurately weighed, press the test sample preparation and measure a lower operation, measure the peak area integrated value, the relative standard deviation of calculating Chrysophanol is 1.33%, the results are shown in Table 17.
Table 17 reproducible test results (n=2)
Experimental result shows that reappearance experiment relative standard deviation RSD is 1.33%, meets the requirements.
2.4.6 specificity test
Get flavour of a drug except rheum officinale by sample prescription, prepare negative sample according to [method for making] lower operation, make the negative control sample by the test sample preparation method, measure with the chromatographic condition identical with test sample, the result shows that the negative control sample goes out the place, peak without the peak at rheum officinale, sees accompanying drawing.
2.4.7 stability test (archen)
With the need testing solution sample introduction analysis for preparing, every 2 hours sample introductions, measure the peak area integrated value by above-mentioned chromatographic condition, calculating relative standard deviation RSD is 1.53%.Show that test sample is stable in 8 hours, the results are shown in Table 18.
Table 18 stability test result (archen)
Experimental result shows that stability experiment relative standard deviation RSD is 1.53%, meets the requirements.
Stability test (Chrysophanol)
With the need testing solution sample introduction analysis for preparing, every 2 hours sample introductions, measure the peak area integrated value by above-mentioned chromatographic condition, calculating relative standard deviation RSD is 1.09%.Show that test sample is stable in 8 hours, the results are shown in Table 19.
Table 19 stability test result (Chrysophanol)
Experimental result shows that stability experiment relative standard deviation RSD is 1.09%, meets the requirements.
2.4.8 the assay result of archen and Chrysophanol in the different lot number gastrointestinal disease treating pills
The preparation precision of reference substance solution takes by weighing archen reference substance 10mg, and Chrysophanol reference substance 15mg puts respectively in the 100ml measuring bottle, with methyl alcohol dissolving and be diluted to scale, shakes up; Precision is measured archen respectively, each 1ml of Chrysophanol solution puts in the 10ml measuring bottle, adds methyl alcohol to scale, shakes up, and namely gets (contain among the every 1ml of archen among 10 μ g, the every 1ml of Chrysophanol and contain 15 μ g).
The about 2g of this product powder (crossing 80 mesh sieves) is got in the preparation of need testing solution, and is accurately weighed, puts in the 100mL tool plug conical flask, the accurate methyl alcohol 25ml that adds, weighed weight added hot reflux 1 hour, let cool, weighed weight is supplied the weight that subtracts mistake with methyl alcohol again, shake up, filter, precision is measured subsequent filtrate 5ml again, put in the flask, fling to solvent, add 8% hydrochloric acid solution 10ml, ultrasonic processing 2 minutes, with a small amount of methenyl choloride washing container, incorporate in the separating funnel, divide and get the methenyl choloride layer, acid solution is extracted three times with methenyl choloride again, each 10mL merges methenyl choloride liquid, and decompression and solvent recovery is to doing, residue adds methyl alcohol makes dissolving, be transferred in the 10ml volumetric flask, add methyl alcohol to scale, shake up, filter through 0.45 μ m filter membrane, and get final product.
Determination method is accurate reference substance solution and each 5 μ l of need testing solution of drawing respectively, and the injection liquid chromatography is measured, and be get final product.Measure altogether the content of archen and Chrysophanol in 3 batches of gastrointestinal disease treating pills, the results are shown in Table 20.
Archen and Determination of chrysophanol measurement result in table 20 sample
Limit the quantity of: the every gram of this product contains rheum officinale with archen (C
15H
10O
5) and Chrysophanol (C
15H
10O
4) the total amount meter must not be less than 0.20mg.
Description of drawings
Fig. 1: forulic acid (110773-200611) reference substance
Fig. 2: gastrointestinal disease treating pill (lot number: 20070625) test sample
Fig. 3: gastrointestinal disease treating pill (lot number: 20070625) sample mark-on
Fig. 4: negative sample and reference substance
Fig. 5: forulic acid Line Chart
Fig. 6: archen Line Chart
Fig. 7: Chrysophanol linear graph
Fig. 8: archen (110756-200110) and Chrysophanol (110796-200615) reference substance
Fig. 9: gastrointestinal disease treating pill (lot number: 20070625) test sample
Figure 10: gastrointestinal disease treating pill (lot number: 20070625) sample mark-on
Figure 11: negative sample
Embodiment
Further set forth by the following examples the preparation method of medicine of the present invention.
A. it is for subsequent use to get banksia rose 100g, agalloch eaglewood 100g, Fructus Aurantii 100g, santal 90g, rheum officinale 90g, cinnabar 75g, bark of official magnolia 100g, muscone 4.5g, defatted croton seed powder 60g, Ligusticum wallichii 90g and date 500g;
B. above ten simply, and defatted croton seed powder, Moschus are ground into respectively fine powder; Cinnabar water flies into impalpable powder; Eight flavors such as all the other agalloch eaglewood are ground into fine powder, and with defatted croton seed powder, Moschus powder facing-up, mixing sieves, and uses water pill, and the cinnabar dressing is used in low temperature drying, and polishing is dried in the shade, and get final product.
Embodiment 2
A. it is for subsequent use to get banksia rose 600g, agalloch eaglewood 600g, Fructus Aurantii 600g, santal 360g, rheum officinale 360g, cinnabar 300g, bark of official magnolia 600g, Moschus 18g, defatted croton seed powder 240g, Ligusticum wallichii 360g and date 2000g;
B. above ten simply, and defatted croton seed powder, Moschus are ground into respectively fine powder; Cinnabar water flies into impalpable powder; Eight flavors such as all the other agalloch eaglewood are ground into fine powder, and with defatted croton seed powder, Moschus powder facing-up, mixing sieves, and uses water pill, and the cinnabar dressing is used in low temperature drying, and polishing is dried in the shade, and get final product.
Embodiment 3
A. it is for subsequent use to get banksia rose 150g, agalloch eaglewood 200g, Fructus Aurantii 200g, santal 360g, rheum officinale 90g, cinnabar 150g, bark of official magnolia 300g, Moschus 5g, defatted croton seed powder 100g, Ligusticum wallichii 150g and date 800g;
B. above ten simply, and defatted croton seed powder, Moschus are ground into respectively fine powder; Cinnabar water flies into impalpable powder; Eight flavors such as all the other agalloch eaglewood are ground into fine powder, and with defatted croton seed powder, Moschus powder facing-up, mixing sieves, and uses water pill, and the cinnabar dressing is used in low temperature drying, and polishing is dried in the shade, and get final product.
Embodiment 4
A. it is for subsequent use to get banksia rose 400g, agalloch eaglewood 300g, Fructus Aurantii 400g, santal 200g, rheum officinale 200g, cinnabar 250g, bark of official magnolia 500g, muscone 10g, defatted croton seed powder 200g, Ligusticum wallichii 180g and date 1500g;
B. above ten simply, and defatted croton seed powder, Moschus are ground into respectively fine powder; Cinnabar water flies into impalpable powder; Eight flavors such as all the other agalloch eaglewood are ground into fine powder, and with defatted croton seed powder, Moschus powder facing-up, mixing sieves, and uses water pill, and the cinnabar dressing is used in low temperature drying, and polishing is dried in the shade, and get final product.
A. it is for subsequent use to get banksia rose 500g, agalloch eaglewood 5000g, Fructus Aurantii 100g, santal 90g, rheum officinale 360g, cinnabar 75g, bark of official magnolia 600g, Moschus 18g, defatted croton seed powder 60g, Ligusticum wallichii 90g and date 2000g;
B. above ten simply, and defatted croton seed powder, Moschus are ground into respectively fine powder; Cinnabar water flies into impalpable powder; Eight flavors such as all the other agalloch eaglewood are ground into fine powder, and with defatted croton seed powder, Moschus powder facing-up, mixing sieves, and uses water pill, and the cinnabar dressing is used in low temperature drying, and polishing is dried in the shade, and get final product.
Embodiment 6
A. it is for subsequent use to get the date 1000g that banksia rose 300g, agalloch eaglewood 300g, stir-baked FRUCTUS AURANTII in bran 300g, santal 180g, rheum officinale 180g, cinnabar 150g, ginger processs bark of official magnolia 300g, muscone 9g, defatted croton seed powder 120g, Ligusticum wallichii 180g and stoning;
B. above ten simply, and defatted croton seed powder, Moschus are ground into respectively fine powder; Cinnabar water flies into impalpable powder; Eight flavors such as all the other agalloch eaglewood are ground into fine powder, and with defatted croton seed powder, Moschus powder facing-up, mixing sieves, and uses water pill, and the cinnabar dressing is used in low temperature drying, and polishing is dried in the shade, and get final product.
Claims (5)
1. archen C in the gastrointestinal disease treating pill
15H
10O
5With Chrysophanol C
15H
10O
4Detection method is characterized in that, the method is as follows:
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filling agent; Methyl alcohol-0.1% phosphoric acid is mobile phase, wherein methyl alcohol: 0.1% phosphoric acid volume ratio is 85: 15; The detection wavelength is 254nm; Number of theoretical plate calculates by the archen peak should be not less than 3000;
The preparation of reference substance solution: precision takes by weighing archen reference substance 10mg, and Chrysophanol reference substance 15mg puts respectively in the 100ml measuring bottle, with methyl alcohol dissolving and be diluted to scale, shakes up; Precision is measured archen respectively, each 1ml of Chrysophanol solution puts in the 10ml measuring bottle, adds methyl alcohol to scale, shakes up, and get final product;
The preparation of need testing solution: get the about 2g of this product powder, cross 80 mesh sieves, accurately weighed, put in the 100mL tool plug conical flask accurate methyl alcohol 25ml, the weighed weight of adding, added hot reflux 1 hour, and let cool, more weighed weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, precision is measured subsequent filtrate 5ml again, puts in the flask, flings to solvent, add 8% hydrochloric acid solution 10ml, ultrasonic processing 2 minutes is with a small amount of methenyl choloride washing container, incorporate in the separating funnel, divide and get the methenyl choloride layer, acid solution is extracted three times with methenyl choloride again, each 10mL, merge methenyl choloride liquid, decompression and solvent recovery is to doing, and residue adds methyl alcohol makes dissolving, is transferred in the 10ml volumetric flask, add methyl alcohol to scale, shake up, filter through 0.45 μ m filter membrane, and get final product;
Determination method: precision is drawn reference substance solution and each 5 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
2. the described detection method of claim 1 is characterized in that, the every gram of this product contains rheum officinale with archen C
15H
10O
5With Chrysophanol C
15H
10O
4The total amount meter must not be less than 0.20mg.
3. the described detection method of claim 1, it is characterized in that described gastrointestinal disease treating pill is to be made by the bulk drug of following weight proportion: the banksia rose 100～600g, agalloch eaglewood 100～600g, Fructus Aurantii 100～600g, santal 90～360g, rheum officinale 90～360g, cinnabar 75～300g, the bark of official magnolia 100～600g, Moschus 4.5～18g, defatted croton seed powder 60～240g, Ligusticum wallichii 90～360g and date 500～2000g.
4. the described detection method of claim 3, it is characterized in that described gastrointestinal disease treating pill is to be made by the bulk drug of following weight proportion: banksia rose 300g, agalloch eaglewood 300g, Fructus Aurantii 300g, santal 180g, rheum officinale 180g, cinnabar 150g, bark of official magnolia 300g, Moschus 9g, defatted croton seed powder 120g, Ligusticum wallichii 180g and date 1000g.
5. the described detection method of claim 4 is characterized in that, Fructus Aurantii is stir-baked FRUCTUS AURANTII in bran; The bark of official magnolia is that ginger is processed the bark of official magnolia; Date is that date, the Moschus of stoning is the muscone.
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| CN105853598A (en) * | 2016-04-01 | 2016-08-17 | 天津中新药业集团股份有限公司乐仁堂制药厂 | Application of Weichang Anwan in combination with artemether in treating gastrointestinal form of malaria |
| CN105726784A (en) * | 2016-04-01 | 2016-07-06 | 天津中新药业集团股份有限公司乐仁堂制药厂 | Application of Weichangan to preparation of alcoholic gastric ulcer resistant drugs |
| CN105770196A (en) * | 2016-04-01 | 2016-07-20 | 天津中新药业集团股份有限公司乐仁堂制药厂 | Pharmaceutical composition for treating gastrointestinal form of malaria and application of pharmaceutical composition |
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