CN102507756A - Quality control method of WeiChangAn pill - Google Patents
Quality control method of WeiChangAn pill Download PDFInfo
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Abstract
The invention relates to a quality control method of a WeiChangAn pill, wherein the traditional Chinese medicine composition is prepared from elecampane, agilawood, fructus aurantii, sandalwood, rheum officinale, mangnolia officinalis, cinnabar, musk, defatted croton seed powder, Chinese-date and rhizoma ligustici wallichii. The quality of the WeiChangAn pill can be effectively controlled by the quality control method provided by the invention.
Description
Technical field
The present invention relates to a kind of drug quality control method, relate to a kind of method of quality control of gastrointestinal disease treating pill specifically.
Background technology
Diarrhoea can be divided into infectious and non-infectious two types.Infectious diarrhea is divided into bacterial infection and virus infections again; Noninfectious diarrhea then can be caused by the change of improper diet, food hypersenstivity, rule of life, abrupt change of climate even multiple reason such as nervous.Motherland's medical science thinks to have loose bowels and is meant that defecation frequency increases, ight soil is rare clearly, even like 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 has cold-dampness and damp and hot branch.Spleen and stomach function expands, and to hinder be to be caused by multiple factor, has outer evil influence, 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.Though diarrhoea is minor illness, pathogenic factor also is diversified, and changes with epoch, environment.We can say that the diarrhoea of today and the diarrhoea before 20 years see that from pathogenesis the change of essence has been arranged.Along with development of times, people's living standard attains the well-off standard basically, and sanitary condition is improved greatly; Diarrhoea ratio by bacterial infection causes is fewer and feweri, 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.A research shows 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 products such as berberine, orfloxacin, and the harm that abuse of antibiotics brought.Diarrhoea market is except 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, urban market diarrhoea mainly be with viral be main, be main in the rural area with bacterial infection, if according to the principle of the market segments, at present a lot of products all are difficult to cover the whole market.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 (the happy capsule of beautiful pearl intestines), Birid Triple Viable 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 the diarrhoea that causes of treatment indigestion, enteritis, bacillary dysentery, abdominal fullness and distention, stomachache, the 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, through this method of quality control, and the quality of this gastrointestinal disease treating pill of may command.
Gastrointestinal disease treating pill of the present invention is to be processed by following materials of weight proportions medicine: 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 processed by following materials of weight proportions medicine: 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 that the present invention is best, Fructus Aurantii wherein is a 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 this method comprises one or both in the following assay:
A, forulic acid C
10H
10O
4Determination on content:
Use high effective liquid chromatography for measuring: use octadecylsilane chemically bonded silica to be filling agent; Acetonitrile-0.085% phosphoric acid is moving 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 35～85% dissolve with methanol 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, shake up, promptly get to scale;
The preparation of need testing solution: get these article powder 1～4g, the accurate title, decide, and puts in 50～200mL tool plug conical flask; Accurate 35～85% methyl alcohol, the 10～50ml that adds claims to decide weight, sonicated 15～60 minutes; Put coldly, claim again to decide weight, supply the weight that subtracts mistake with 35～85% methyl alcohol; Shake up, filter, promptly get through filter membrane;
Determination method: accurate respectively reference substance solution and each 2.5～10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
B, archen C
15H
10O
5With Chrysophanol C
15H
10O
4Determination on content:
Chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filling agent; Methyl alcohol-0.1% phosphoric acid is moving 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 dissolve with methanol 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 promptly gets;
The preparation of need testing solution: get these article powder 1～4g, the accurate title, decide, and puts in 50～200mL tool plug conical flask, and the accurate methyl alcohol 10～50ml that adds claims to decide weight; Reflux 0.5～2 hour is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with methyl alcohol, shakes up; Filter, precision is measured subsequent filtrate 2.5～10ml again, puts in the flask, flings to solvent, adds 4～16% hydrochloric acid solutions, 5～20ml; Sonicated 1～4 minute with a small amount of methenyl choloride washing container, is incorporated in the separating funnel, obtains the methenyl choloride layer, and 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, and residue adds methyl alcohol makes dissolving, is transferred in 5～20ml volumetric flask; Add methyl alcohol to scale, shake up, filter, promptly get through filter membrane;
Determination method: accurate respectively reference substance solution and each 2.5～10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get.
The method of quality control of the preferred gastrointestinal disease treating pill of the present invention, wherein this method comprises one or both in the following assay:
A, forulic acid C
10H
10O
4Determination on content:
Use high effective liquid chromatography for measuring: use octadecylsilane chemically bonded silica to be filling agent; Acetonitrile-0.085% phosphoric acid is moving 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 50～75% dissolve with methanol 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, shake up, promptly get to scale;
The preparation of need testing solution: get these article powder 1.5～3g, the accurate title, decide, and puts in 80～120mL tool plug conical flask; Accurate 50～75% methyl alcohol, the 20～30ml that adds claims to decide weight, sonicated 20～40 minutes; Put coldly, claim again to decide weight, supply the weight that subtracts mistake with 50～75% methyl alcohol; Shake up, filter, promptly get through filter membrane;
Determination method: accurate respectively reference substance solution and each 4～6 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
B, archen C
15H
10O
5With Chrysophanol C
15H
10O
4Determination on content:
Chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filling agent; Methyl alcohol-0.1% phosphoric acid is moving 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 dissolve with methanol 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 promptly gets;
The preparation of need testing solution: get these article powder 1.5～3g, the accurate title, decide, and puts in 80～120mL tool plug conical flask, and the accurate methyl alcohol 20～30ml that adds claims to decide weight; Reflux 0.5～1.5 hour is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with methyl alcohol, shakes up; Filter, precision is measured subsequent filtrate 4～6ml again, puts in the flask, flings to solvent, adds 6～10% hydrochloric acid solutions, 8～15ml; Sonicated 1～3 minute with a small amount of methenyl choloride washing container, is incorporated in the separating funnel, obtains the methenyl choloride layer, and 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, and residue adds methyl alcohol makes dissolving, is transferred in 8～15ml volumetric flask; Add methyl alcohol to scale, shake up, filter, promptly get through filter membrane;
Determination method: accurate respectively reference substance solution and each 4～6 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get.
The method of quality control of the preferred gastrointestinal disease treating pill of the present invention, wherein this method comprises one or both in the following assay:
A, forulic acid C
10H
10O
4Mensuration:
Use high effective liquid chromatography for measuring: use octadecylsilane chemically bonded silica to be filling agent; Acetonitrile-0.085% phosphoric acid is moving 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 70% dissolve with methanol 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, shake up, promptly get to scale;
The preparation of need testing solution: get these article powder 2g, the accurate title, decide, and puts in the 100mL tool plug conical flask, the accurate 70% methyl alcohol 25ml that adds; Claim decide weight, sonicated 30 minutes is put coldly, and weight decided in title again; Supply the weight that subtracts mistake with 70% methyl alcohol, shake up, filter, promptly get through 0.45 μ m filter membrane;
Determination method: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
B, archen C
15H
10O
5With Chrysophanol C
15H
10O
4Mensuration:
Chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filling agent; Methyl alcohol-0.1% phosphoric acid is moving 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 dissolve with methanol 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 promptly gets;
The preparation of need testing solution: get the about 2g of these article powder (crossing 80 mesh sieves), the accurate title, decide, and puts in the 100mL tool plug conical flask, and the accurate methyl alcohol 25ml that adds claims to decide weight; Reflux 1 hour is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with methyl alcohol, shakes up; Filter, precision is measured subsequent filtrate 5ml again, puts in the flask, flings to solvent, adds 8% hydrochloric acid solution 10ml; Sonicated 2 minutes with a small amount of methenyl choloride washing container, is incorporated in the separating funnel, obtains the methenyl choloride layer, and acid solution is extracted three times with methenyl choloride again; Each 10mL merges methenyl choloride liquid, and 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, promptly get through 0.45 μ m filter membrane;
Determination method: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get.
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 test: use octadecylsilane chemically bonded silica to be filling agent; Methyl alcohol-acetonitrile-water is a moving 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 the magnolol reference substance respectively, the honokiol reference substance is an amount of, accurately claim surely, add methyl alcohol and process every 1ml respectively and contain the solution that magnolol 60 μ g, every 1ml contain honokiol 10 μ g, promptly get;
The preparation of need testing solution: get these article 3g, porphyrize is got 0.5g, and accurate the title decides, and puts in the tool plug conical flask; The accurate chloroform 50ml that adds claims to decide weight, hold over night, and sonicated 1.5 hours is put cold; Claim to decide weight again, supply the weight that subtracts mistake with chloroform, filter, precision is measured subsequent filtrate 15ml, evaporate to dryness; Residue is with dissolve with methanol and be transferred in the 5ml measuring bottle, adds methyl alcohol to scale, shakes up, and promptly gets;
Determination method: accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get.
In the method for quality control of gastrointestinal disease treating pill of the present invention, the configuration proportion of moving 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 these article 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 these article 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 these article 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.
These article described in the present invention are meant 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 an example.Under the situation of not violating purport of the present invention and scope, can carry out various changes and improvement to the present invention.For example, the mensuration the possibility of result that uses the different detection instrument to be obtained is 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.
Explain through medicine gastrointestinal disease treating pill of the present invention (obtaining) active constituent content measuring below according to embodiment 6 preparation methods
The beneficial effect of content assaying method of the present invention.
Test Example 1
1. raw material (medicinal material) quality standard
1.1 the banksia rose
These article are the dry root of feverfew banksia rose Aucklandia lappa Decne..Autumn, two seasons of winter excavate, and remove silt and fibrous root, segment, and big vertical profile again becomes lobe, hits tertia after the drying.
These article should meet the relevant regulations under first the 41st page of banksia rose item of Chinese Pharmacopoeia version in 2005.
1.2 agalloch eaglewood
These article contain the timber of resin for fragrant Aquilaria sinensis (Lour.) Gilg of Thymelaeceae plant whitewood.All can gather the whole year, extracts resiniferous timber, removes not resiniferous part, dries in the shade.
These article should meet the relevant regulations under first the 128th page of agalloch eaglewood item of Chinese Pharmacopoeia version in 2005.
1.3 Fructus Aurantii (bran stir-fry)
These article are the dry immature fruit of rutaceae bitter orange Citrus aurantium L. and variety thereof.Gather when pericarp is still green July, and crosscut is two halves from the middle part, dries or low temperature drying.
[process of preparing Chinese medicine] Fructus Aurantii is removed impurity, cleans, and runs through, and shave, dry back sieve remove the broken flesh nuclear that falls.
These article are irregular arcuation bar shaped thin slice, reach 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 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.
These article are irregular arcuation bar shaped thin slice, and look darker, and what have has a focal spot.
These article should meet the relevant regulations under first the 171st page of Fructus Aurantii item of Chinese Pharmacopoeia version in 2005.
1.4 santal
These article are the heartwood of Santalaceae plant santal Santalum album L. trunk.
These article should meet the relevant regulations under first the 264th page of santal item of Chinese Pharmacopoeia version in 2005.
1.5 rheum officinale
These article are the dry root and rhizome of 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.
These article should meet the relevant regulations under first the 17th page of rheum officinale item of Chinese Pharmacopoeia version in 2005.
1.6 the bark of official magnolia (ginger system)
These article are 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, and Gen Pi and branch skin directly dry in the shade; Dry hide is put in the boiling water after little the boiling, and the dark and damp place of banking up when " sweating " 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.
These article are 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, fries according to stir frying with ginger juice method (appendix II D) and does.
These article are crooked strand shape, and section fibrous is puce.
These article should meet the relevant regulations under first the 176th page of bark of official magnolia item of Chinese Pharmacopoeia version in 2005.
1.7 cinnabar
These article are 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.
These article should meet the relevant regulations under first the 92nd page of cinnabar item of Chinese Pharmacopoeia version in 2005.
1.8 Moschus
These article are 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.Wild musk deer how hunt by the extremely inferior in the winter time spring, after trapping, extracts sachet, dries in the shade, and practises and claim " hair shell Moschus "; Cut sachet open, remove softgel shell, practise and claim " 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.
These article should meet the relevant regulations under first the 266th page of Moschus item of Chinese Pharmacopoeia version in 2005.
1.9 defatted croton seed powder
These article are the process of preparing Chinese medicine processed goods of crotons.
These article should meet the relevant regulations under first the 55th page of defatted croton seed powder item of Chinese Pharmacopoeia version in 2005.
1.10 date (stoning)
These article are the dry mature fruit of Rhamnaceae plant jujube Ziziphus jujuba Mill..Gather during fruit maturation autumn, dries.
[process of preparing Chinese medicine] removed impurity, cleans, and dries.Time spent breaks or stoning.
These article should meet the relevant regulations under first the 15th page of date item of Chinese Pharmacopoeia version in 2005.
1.11 Ligusticum wallichii
These article are the dry rhizome of samphire Ligusticum wallichii Ligusticum chuanxiong Hort..Summer, the joint dish on the stem was significantly outstanding, and excavated when having a little purple, removed silt, shone the back a heatable brick bed and did, and removed fibrous root again.
These article should meet the relevant regulations under first the 28th page of Ligusticum wallichii item of Chinese Pharmacopoeia version in 2005.
[assay] measured according to high performance liquid chromatography (appendix VI D).
1. instrument and reagent
1.1 instrument condition
Instrument: Tianjin, island LC-2010A
HTThe 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
Moving 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 (supplying assay to use)
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); Provide by Lerentang Pharmaceutical Factory, Zhongxin Pharmaceutical Group Co., Ltd., Tianj.
2. the investigation of experimental technique
2.1 chromatographic condition and system suitability test
Use octadecylsilane chemically bonded silica to be filling agent; Acetonitrile-0.085% phosphoric acid (17: 83) is moving 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 first the 28th page of Ligusticum wallichii of Chinese Pharmacopoeia version in 2005 do not have [assay], thus this experiment according to first one the 89th page of Chinese Pharmacopoeia version in 2005 be all samphire when be classified as with reference to and prepare test sample according under [assay] need testing solution preparation.
2.3 the selection of condition determination
2.3.1 the selection of moving phase
Experimental result shows that with acetonitrile-0.085% phosphoric acid (17: 83) be moving phase, and the forulic acid chromatographic peak separates well with the chromatographic peak of other compositions.
2.3.2 the selection of wavelength
Select 316nm for detecting wavelength down according to the assay item of first the 89th page of Radix Angelicae Sinensis of Chinese Pharmacopoeia version 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, the accurate title, decide, and puts in the 100mL measuring bottle, adds dissolve with methanol and be diluted to scale, shakes up, and processes 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 processes 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
Use octadecylsilane chemically bonded silica to be filling agent; Acetonitrile-0.085% phosphoric acid (17: 83) is moving 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
Above-mentioned reference substance solution 1.0,2.0,4.0,5.0,6.0,8.0, the 10.0 μ l of accurate absorption, peak area is measured in sample introduction analysis successively, and the result sees table 1.
With the sample size is horizontal ordinate, and peak area is an ordinate, and the drawing standard curve is seen Fig. 1.
Obtain regression equation through statistical calculations: 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
The test of forulic acid reference substance precision
Accurate forulic acid (concentration is 10.26 μ g/ml) the reference substance solution 5 μ L that draw repeat sample introduction 6 times, by above-mentioned chromatostrip
Part is measured the peak area integrated value, and calculating relative standard deviation is 1.78%, and the result sees table 2.
Table 2 forulic acid reference substance precision experimental 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%, and the result sees table 3.
Table 3 sample precision experimental 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 these article of getting powder: 20070625; Cross 80 mesh sieves) 1g, totally 6 parts, the accurate title, decide, and puts in the 25ml measuring bottle, adds an amount of (C=0.2565mg/mL of forulic acid reference substance respectively; V=0.50mL), press the test sample preparation and measure an operation down, calculate recovery rate, the forulic acid recovery is 99.60%, and relative standard deviation RSD is 0.50%, and the result sees 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; Accurate title is fixed, presses the test sample preparation and measures item operation down, measures the peak area integrated value; The relative standard deviation of calculating forulic acid is 1.51%, and the result sees 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 the flavour of a drug except that Ligusticum wallichii by the sample prescription, operate the preparation negative sample down, process the negative control sample by the test sample preparation method according to [method for making] item; Use the chromatographic condition identical to measure with test sample; The result shows that the forulic acid of negative control sample in Ligusticum wallichii goes out the place, peak does not have the peak, sees accompanying drawing.
2.4.7 stability test
With the need testing solution sample introduction analysis for preparing, every at a distance from 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 result sees 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 content of ferulic acid is measured the result 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 70% dissolve with methanol 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 promptly gets (every 1ml contains forulic acid 6 μ g).
The about 2g of these article powder (crossing 80 mesh sieves) is got in the preparation of need testing solution, and accurate the title decides, and puts in the 100mL tool plug conical flask; The accurate 70% methyl alcohol 25ml that adds claims to decide weight, sonicated 30 minutes; Put coldly, claim again to decide weight, supply the weight that subtracts mistake with 70% methyl alcohol; Shake up, filter, promptly get through 0.45 μ m filter membrane.
Accurate respectively reference substance solution and each the 5 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, and promptly get.Measured content of ferulic acid in 3 batches of gastrointestinal disease treating pills altogether, the result sees table 7.
Ferulaic acid content is measured the result in table 7 sample
Limit the quantity of: the every gram of these article 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 2 article of Test Example
[assay] measured according to high performance liquid chromatography (appendix VI D).
1. instrument and reagent
1.1 instrument condition
Instrument: Tianjin, island LC-2010A
HTThe 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
Moving 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 (supplying assay to use)
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); Provide by Lerentang Pharmaceutical Factory, Zhongxin Pharmaceutical Group Co., Ltd., Tianj.
2. the investigation of experimental technique
2.1 chromatographic condition and system suitability test
Use octadecylsilane chemically bonded silica to be filling agent; Methyl alcohol-0.1% phosphoric acid (85: 15) is moving 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 prepares test sample down according to first the 17th page of rheum officinale assay need testing solution preparation of Chinese Pharmacopoeia version in 2005 item.
2.3 the selection of condition determination
2.3.1 the selection of moving phase
Experimental result shows that with methyl alcohol-0.1% phosphoric acid (85: 15) be moving phase, and archen separates well with the chromatographic peak of other compositions with the Chrysophanol chromatographic peak.
2.3.2 the selection of wavelength
Select 254nm for detecting wavelength down according to the assay item of first the 17th page of rheum officinale of Chinese Pharmacopoeia version 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, accurate claim surely, put in the 100mL measuring bottle, add dissolve with methanol and be diluted to scale, shake up, process reference substance solution that every 1mL contains 0.1010mg as archen reference substance stock solution.
The preparation of Chrysophanol reference substance stock solution: take by weighing Chrysophanol reference substance 16.18mg, accurate claim surely, put in the 100mL measuring bottle, add dissolve with methanol and be diluted to scale, shake up, process reference substance solution that every 1mL contains 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, process 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
Use octadecylsilane chemically bonded silica to be filling agent; Methyl alcohol-0.1% phosphoric acid (85: 15) is moving 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
Above-mentioned reference substance solution 1.0,2.0,4.0,6.0,8.0, the 10.0 μ l of accurate absorption, peak area is measured in sample introduction analysis successively, and the result sees table 8.
Table 8 archen linear relationship is investigated the result
With the sample size is horizontal ordinate, and peak area is an ordinate, and the drawing standard curve is seen Fig. 6.
Obtain regression equation through statistical calculations: 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
Above-mentioned reference substance solution 1.0,2.0,4.0,6.0,8.0, the 10.0 μ l of accurate absorption, peak area is measured in sample introduction analysis successively, and the result sees table 9.
Table 9 Chrysophanol linear relationship is investigated the result
With the sample size is horizontal ordinate, and peak area is an ordinate, and the drawing standard curve is seen Fig. 7.
Obtain regression equation through statistical calculations: 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%, and the result sees table 10.
Table 10 precision experimental 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%, and the result sees table 11.
Table 11 precision experimental 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%, and the result sees table 12.
Table 12 sample precision experimental 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%, and the result sees table 13.
Table 13 sample precision experimental 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 these article of getting powder: 20070625; Cross 80 mesh sieves) 1g, totally 6 parts, accurate claim surely, it is an amount of to add the archen reference substance respectively, and press the test sample preparation and operate down with measuring, calculate recovery rate, the archen recovery is 96.77%, and relative standard deviation RSD is 0.10%, and the result sees 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 these article of getting powder: 20070625; Cross 80 mesh sieves) 1g, totally 6 parts, accurate claim surely, it is an amount of to add the Chrysophanol reference substance respectively, and press the test sample preparation and operate down with measuring, calculate recovery rate, the Chrysophanol recovery is 97.94%, and relative standard deviation RSD is 1.69%, and the result sees 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; Accurate title is fixed, presses the test sample preparation and measures item operation down, measures the peak area integrated value; The relative standard deviation of calculating archen is 1.51%, and the result sees 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; Accurate title is fixed, presses the test sample preparation and measures item operation down, measures the peak area integrated value; The relative standard deviation of calculating Chrysophanol is 1.33%, and the result sees 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 the flavour of a drug except that rheum officinale by the sample prescription, operate the preparation negative sample down, process the negative control sample by the test sample preparation method according to [method for making] item; Use the chromatographic condition identical to measure with test sample; The result shows that the negative control sample goes out the place, peak at rheum officinale does not have the peak, sees accompanying drawing.
2.4.7 stability test (archen)
With the need testing solution sample introduction analysis for preparing, every at a distance from 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 result sees 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 at a distance from 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 result sees 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 dissolve with methanol 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 promptly 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 these article powder (crossing 80 mesh sieves) is got in the preparation of need testing solution, and accurate the title decides, and puts in the 100mL tool plug conical flask, and the accurate methyl alcohol 25ml that adds claims to decide weight; Reflux 1 hour is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with methyl alcohol, shakes up; Filter, precision is measured subsequent filtrate 5ml again, puts in the flask, flings to solvent, adds 8% hydrochloric acid solution 10ml; Sonicated 2 minutes with a small amount of methenyl choloride washing container, is incorporated in the separating funnel, obtains the methenyl choloride layer, and acid solution is extracted three times with methenyl choloride again; Each 10mL merges methenyl choloride liquid, and 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, promptly get through 0.45 μ m filter membrane.
Accurate respectively reference substance solution and each the 5 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, and promptly get.Measured the content of archen and Chrysophanol in 3 batches of gastrointestinal disease treating pills altogether, the result sees table 20.
Archen and Chrysophanol assay result in table 20 sample
Limit the quantity of: the every gram of these article 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) appearance 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) appearance mark-on
Figure 11: negative sample
Embodiment
Below further set forth the preparation method of medicine of the present invention through embodiment.
A. it is 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 fine powder respectively; 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 promptly gets.
Embodiment 2
A. it is 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 fine powder respectively; 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 promptly gets.
Embodiment 3
A. it is 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 fine powder respectively; 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 promptly gets.
Embodiment 4
A. it is 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 fine powder respectively; 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 promptly gets.
A. it is 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 fine powder respectively; 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 promptly gets.
Embodiment 6
A. getting banksia rose 300g, agalloch eaglewood 300g, stir-baked FRUCTUS AURANTII in bran 300g, santal 180g, rheum officinale 180g, cinnabar 150g, ginger, to process the date 1000g of bark of official magnolia 300g, muscone 9g, defatted croton seed powder 120g, Ligusticum wallichii 180g and stoning subsequent use;
B. above ten simply, and defatted croton seed powder, Moschus are ground into fine powder respectively; 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 promptly gets.
Claims (8)
1. the detection method of a gastrointestinal disease treating pill is characterized in that, this method comprises following two kinds of assays:
A, forulic acid C
10H
10O
4Determination on content:
Use high effective liquid chromatography for measuring: use octadecylsilane chemically bonded silica to be filling agent; Acetonitrile-0.085% phosphoric acid is moving 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 35～85% dissolve with methanol 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, shake up, promptly get to scale;
The preparation of need testing solution: get these article powder 1～4g, the accurate title, decide, and puts in 50～200mL tool plug conical flask; Accurate 35～85% methyl alcohol, the 10～50ml that adds claims to decide weight, sonicated 15～60 minutes; Put coldly, claim again to decide weight, supply the weight that subtracts mistake with 35～85% methyl alcohol; Shake up, filter, promptly get through filter membrane;
Determination method: accurate respectively reference substance solution and each 2.5～10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
B, archen C
15H
10O
5With Chrysophanol C
15H
10O
4Determination on content:
Chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filling agent; Methyl alcohol-0.1% phosphoric acid is moving 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 dissolve with methanol 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 promptly gets;
The preparation of need testing solution: get these article powder 1～4g, the accurate title, decide, and puts in 50～200mL tool plug conical flask, and the accurate methyl alcohol 10～50ml that adds claims to decide weight; Reflux 0.5～2 hour is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with methyl alcohol, shakes up; Filter, precision is measured subsequent filtrate 2.5～10ml again, puts in the flask, flings to solvent, adds 4～16% hydrochloric acid solutions, 5～20ml; Sonicated 1～4 minute with a small amount of methenyl choloride washing container, is incorporated in the separating funnel, obtains the methenyl choloride layer, and 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, and residue adds methyl alcohol makes dissolving, is transferred in 5～20ml volumetric flask; Add methyl alcohol to scale, shake up, filter, promptly get through filter membrane;
Determination method: accurate respectively reference substance solution and each 2.5～10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get.
2. the detection method of the said gastrointestinal disease treating pill of claim 1 is characterized in that, this method comprises following two kinds of assays:
A, forulic acid C
10H
10O
4Determination on content:
Use high effective liquid chromatography for measuring: use octadecylsilane chemically bonded silica to be filling agent; Acetonitrile-0.085% phosphoric acid is moving 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 50～75% dissolve with methanol 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, shake up, promptly get to scale;
The preparation of need testing solution: get these article powder 1.5～3g, the accurate title, decide, and puts in 80～120mL tool plug conical flask; Accurate 50～75% methyl alcohol, the 20～30ml that adds claims to decide weight, sonicated 20～40 minutes; Put coldly, claim again to decide weight, supply the weight that subtracts mistake with 50～75% methyl alcohol; Shake up, filter, promptly get through filter membrane;
Determination method: accurate respectively reference substance solution and each 4～6 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
B, archen C
15H
10O
5With Chrysophanol C
15H
10O
4Determination on content:
Chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filling agent; Methyl alcohol-0.1% phosphoric acid is moving 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 dissolve with methanol 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 promptly gets;
The preparation of need testing solution: get these article powder 1.5～3g, the accurate title, decide, and puts in 80～120mL tool plug conical flask, and the accurate methyl alcohol 20～30ml that adds claims to decide weight; Reflux 0.5～1.5 hour is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with methyl alcohol, shakes up; Filter, precision is measured subsequent filtrate 4～6ml again, puts in the flask, flings to solvent, adds 6～10% hydrochloric acid solutions, 8～15ml; Sonicated 1～3 minute with a small amount of methenyl choloride washing container, is incorporated in the separating funnel, obtains the methenyl choloride layer, and 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, and residue adds methyl alcohol makes dissolving, is transferred in 8～15ml volumetric flask; Add methyl alcohol to scale, shake up, filter, promptly get through filter membrane;
Determination method: accurate respectively reference substance solution and each 4～6 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get.
3. the detection method of the said gastrointestinal disease treating pill of claim 2 is characterized in that, method is following:
A, forulic acid C
10H
10O
4Mensuration:
Use high effective liquid chromatography for measuring: use octadecylsilane chemically bonded silica to be filling agent; Acetonitrile-0.085% phosphoric acid is moving 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 70% dissolve with methanol 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, shake up, promptly get to scale;
The preparation of need testing solution: get these article powder 2g, the accurate title, decide, and puts in the 100mL tool plug conical flask, the accurate 70% methyl alcohol 25ml that adds; Claim decide weight, sonicated 30 minutes is put coldly, and weight decided in title again; Supply the weight that subtracts mistake with 70% methyl alcohol, shake up, filter, promptly get through 0.45 μ m filter membrane;
Determination method: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
B, archen C
15H
10O
5With Chrysophanol C
15H
10O
4Mensuration:
Chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filling agent; Methyl alcohol-0.1% phosphoric acid is moving 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 dissolve with methanol 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 promptly gets;
The preparation of need testing solution: get the about 2g of these article powder (crossing 80 mesh sieves), the accurate title, decide, and puts in the 100mL tool plug conical flask, and the accurate methyl alcohol 25ml that adds claims to decide weight; Reflux 1 hour is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with methyl alcohol, shakes up; Filter, precision is measured subsequent filtrate 5ml again, puts in the flask, flings to solvent, adds 8% hydrochloric acid solution 10ml; Sonicated 2 minutes with a small amount of methenyl choloride washing container, is incorporated in the separating funnel, obtains the methenyl choloride layer, and acid solution is extracted three times with methenyl choloride again; Each 10mL merges methenyl choloride liquid, and 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, promptly get through 0.45 μ m filter membrane;
Determination method: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get.
4. the detection method of the arbitrary said gastrointestinal disease treating pill of claim 1～3 is characterized in that, the every gram of these article contains Ligusticum wallichii with forulic acid C
10H
10O
4Meter must not be less than 0.040mg.
5. the detection method of the arbitrary said gastrointestinal disease treating pill of claim 1～3 is characterized in that, the every gram of these article contains rheum officinale with archen C
15H
10O
5With Chrysophanol C
15H
10O
4The total amount meter must not be less than 0.20mg.
6. the arbitrary said gastrointestinal disease treating pill of claim 1～5; It is characterized in that, be to be processed by following materials of weight proportions medicine: 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.
7. the said gastrointestinal disease treating pill of claim 6; It is characterized in that, be to be processed by following materials of weight proportions medicine: 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.
8. the said gastrointestinal disease treating pill of claim 6 is characterized in that, Fructus Aurantii is a 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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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN114166958A (en) * | 2021-10-29 | 2022-03-11 | 合肥创新医药技术有限公司 | Fingerprint detection method and application of traditional Chinese medicine compound cang huo pingwei granules |
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2008
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN114166958A (en) * | 2021-10-29 | 2022-03-11 | 合肥创新医药技术有限公司 | Fingerprint detection method and application of traditional Chinese medicine compound cang huo pingwei granules |
| CN114166958B (en) * | 2021-10-29 | 2024-03-29 | 合肥创新医药技术有限公司 | Detection method of fingerprint of traditional Chinese medicine compound herba xanthil stomach-calming particles and application thereof |
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