CN102008704B - Detection method for composition having middle-warming stomach harmonizing function - Google Patents

Detection method for composition having middle-warming stomach harmonizing function Download PDF

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CN102008704B
CN102008704B CN 201010593650 CN201010593650A CN102008704B CN 102008704 B CN102008704 B CN 102008704B CN 201010593650 CN201010593650 CN 201010593650 CN 201010593650 A CN201010593650 A CN 201010593650A CN 102008704 B CN102008704 B CN 102008704B
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CN102008704A (en
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付立家
付建家
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Beijing Asia East Bio Pharmaceutical Co Ltd
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Beijing Asia East Bio Pharmaceutical Co Ltd
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Abstract

The invention discloses a pharmaceutical composition detection method, material drugs of the pharmaceutical composition are as follows: elecampane, fructus amomi, white atractylodes rhizome, pericarpium citri reticulatae, Poria cocos, Pinellia ternate(prepared), rhizoma cyperi, immature bitter orange, Amomum kravanh, bark official magnolia, Pogostemon cablin and liquorice, and the detection method detects content of Costundide by high performance liquid chromatography.

Description

A kind of detection method with composition of warming middle-JIAO for easing the stomach effect
The present invention is for dividing an application, and the original bill application number is 200710099505.8, and the original bill applying date is on 05 23rd, 2007, and the original bill name is called composition and method of making the same and the method for quality control with warming middle-JIAO for easing the stomach effect.
Technical field
The present invention relates to a kind of Chinese medicine composition and preparation method thereof and method of quality control, particularly relate to a kind of Chinese medicine composition with warming middle-JIAO for easing the stomach effect and preparation method thereof and method of quality control.
Background technology
Taste are ill, certainly will affect the source of nutrition of human body, also are directly connected to the generation of disease, development and prognosis.So-called " flat people's normal gas is reported in stomach, the flat people's of stomach person normal gas also, people's extreme hypofunction of the stomach day is contrary, and is dead against the person." stomach trouble should cause that people's attention is taken precautions against early.
Motherland's medical science is thought: diseases caused by external factors cold-evil, not only the cloudy gas of easy damaged taste affect spleen transporting ability, also easily making cold stagnate in, hinder the operation of gas, cold air is invaded between the stomach lung, and blood can not be gone, gas can not lead to, solid and produce to tremble with fear and ache.Pathology: coldaccumulating abdominalgia, meet cold increasing the weight of, must warm up then and relax, abdomen is full uncomfortable.Modern scholar thinks, people's stomach some near stomach wall, if cold air directly invade and upper abdomen, but reflectivity ground causes stomach and vessel retraction thereof, the stomach motor function gets muddled, thereby produces spasmodic colic, the stomach feeling of repletion, it is poor to receive, even feels sick, vomiting.
Stomach trouble is caused by many reasons, hyperhydrochloria, and pepsinia increases, nerve and endocrine dysfunction, gastrin secretion increases, feeding desorder, smoking, the reasons such as excessive drinking and stomach and intestine bacterium and unusual procreation.General following a few class medicines (1) antacids: relief of symptoms.(2) the Histamine receptors blocking agent generally has spinoff to kidney.(3) anticholinergic agents, price, spinoff is large, unsuitable long-term taking.(4) gastric mucosal protection medicine and improve medicine for stomach dynamic.General antacids, medication is adhered in protection gastric mucosa medicine and antimicrobial collocation; can not frequently change dressings the short time, after meal medication and medication ante cibum will the difference effects midway, and anticholinergic drug should not share by the medicine for stomach dynamic opposite with effect; due to illness and different and, constantly grope curative effect.
Therefore inventing a kind of medicine with warming middle-JIAO for easing the stomach effect is necessary.
Summary of the invention
The object of the invention is to provide a kind of Chinese medicine composition with warming middle-JIAO for easing the stomach effect;
The object of the invention also is to provide a kind of Chinese medicine composition preparation method with warming middle-JIAO for easing the stomach effect;
The object of the invention also is to provide a kind of method of quality control with Chinese medicine composition of warming middle-JIAO for easing the stomach effect.
The present invention seeks to be achieved through the following technical solutions:
Chinese medicine composition with warming middle-JIAO for easing the stomach effect of the present invention is to be made by the bulk drug of following weight ratio:
Banksia rose 30-100g Divine Comedy 150-300g bighead atractylodes rhizome 50-200g
The dried orange peel 50-200g Poria cocos 50-200g tuber of pinellia (system) 50-200g
Rhizoma cyperi (vinegar system) the 30-100g dried immature fruit of citron orange (stir-fry) 30-100g cardamom (shelling) 30-100g
The bark of official magnolia (ginger system) 30-100g pawpaw 30-100g ginger 10-60g
Date 20-100g;
The above-mentioned raw materials optimum ratio is:
Banksia rose 70g Divine Comedy 200g bighead atractylodes rhizome 100g
The dried orange peel 110g Poria cocos 110g tuber of pinellia (system) 110g
Rhizoma cyperi (vinegar system) the 60g dried immature fruit of citron orange (stir-fry) 60g cardamom (shelling) 60g
The bark of official magnolia (ginger system) 60g pawpaw 60g ginger 30g
Date 50g;
Chinese medicine composition with warming middle-JIAO for easing the stomach effect of the present invention can be made by the bulk drug of following weight ratio:
Banksia rose 30-100g fructus amomi 30-100g bighead atractylodes rhizome 50-200g
The dried orange peel 50-200g Poria cocos 50-200g tuber of pinellia (system) 50-200g
Rhizoma cyperi (vinegar system) the 30-100g dried immature fruit of citron orange (stir-fry) 30-100g cardamom (shelling) 30-100g
The bark of official magnolia (ginger system) 30-100g Pogostemon cablin 30-100g Radix Glycyrrhizae 10-90g
Ginger 10-60g date 20-100g;
The above-mentioned raw materials optimum ratio is:
Banksia rose 30-50g fructus amomi 30-50g bighead atractylodes rhizome 120-200g
The dried orange peel 120-200g Poria cocos 120-200g tuber of pinellia (system) 120-200g
Rhizoma cyperi (vinegar system) the 30-60g dried immature fruit of citron orange (stir-fry) 30-60g cardamom (shelling) 30-60g
The bark of official magnolia (ginger system) 30-60g Pogostemon cablin 30-60g Radix Glycyrrhizae 50-90g
Ginger 20-40g date 40-80g;
Composition of the present invention routinely technique adding auxiliary material is made the clinical acceptable formulations such as tablet, capsule, oral liquid, dripping pill, spray, granule; Described auxiliary material comprises solvent, disintegrant, flavouring, antiseptic, colorant, bonding agent, lubricant, matrix etc.
The preparation method of Chinese medicinal composition granules of the present invention is:
The tuber of pinellia and ginger are made solvent with the 60-80% ethanol that medicinal material 5-7 doubly measures, and flood after 20-30 hour, and with the speed diacolation of per minute 1～6ml, the liquid of filtering is for subsequent use; The banksia rose, fructus amomi, the bighead atractylodes rhizome, dried orange peel, the dried immature fruit of citron orange, cardamom, the bark of official magnolia, Pogostemon cablin extract volatile oil with the way of distillation, and the aqueous solution after the distillation in addition device is collected; Three flavor and the dates such as the dregs of a decoction and all the other Poria cocos, boiling 2-3 time, each 1-2.5 hour, collecting decoction, filter, filtrate and above-mentioned aqueous solution merge, concentrated relative density 1.10 (50～55 ℃), let cool, add equivalent ethanol, left standstill 20-30 hour, incline and get supernatant, filter, filtrate and above-mentioned filtrate merge, Recycled ethanol, and being concentrated into relative density is the clear cream of 1.33～1.36 (50～55 ℃), 1 part of qinghuo reagent, cane sugar powder 1-3 part, dextrin 1-3 part, appropriate amount of ethanol, granulation, drying adds above-mentioned volatile oil, mixing, and get final product.
Pharmaceutical composition method of quality control of the present invention comprises one or more in following discrimination method and/or the assay:
Differentiate:
(1) get the quite described composition material medicine of preparation 28-32g, add ethanol-strong ammonia solution (1-2: 1-2) 5ml, wetting, placed 15-30 minute, add chloroform 18-25ml, ultrasonic processing 15-30 minute, filter, filtrate evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution; Other gets the synephrine reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin-layered chromatography, draw need testing solution 20 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, take toluene-ethyl acetate-methyl alcohol-isopropyl alcohol-strong ammonia solution (10-15: 4-9: 2-6: 2-5: 1) as developping agent, put in the chromatography cylinder of ammonia saturated with vapor, launch, take out, dry, spray is with the 0.4-0.7% ethanol solution of ninhydrin, 105 ℃ of bakings about 4-7 minute; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious identical purple dot;
(2) get the quite described composition material medicine of preparation 10g,, porphyrize adds water 20ml, chloroform 20ml, hydrochloric acid 3ml, adds hot reflux 1-2 hour, divides and gets chloroform layer, washes with water to neutrality, volatilizes, and residue adds absolute ethyl alcohol 1ml makes dissolving, as need testing solution; Other removes hydrogen constuslactone reference substance, adds absolute ethyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin-layered chromatography, draw control medicinal material solution 1 μ l, sample solution 2～4 μ l, put respectively on same silica gel g thin-layer plate, take sherwood oil (60～90 ℃)-toluene-ethyl acetate-glacial acetic acid (8-12: 18-22: 5-8: 0.4-0.7) as developping agent, launch, take out, dry, spray is with 1% vanillic aldehyde ethanol solution of sulfuric acid, and hot blast blows to clear spot; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
(3) get the quite described composition material medicine of preparation 28-32g, porphyrize, add water 50ml dissolving, add diethyl ether and 2-4 time (20-30ml that at every turn adds diethyl ether, saturated nacl aqueous solution 5-15ml) of saturated nacl aqueous solution extraction, divide and get ether solution, room temperature volatilizes, residue adds normal hexane 0.5ml dissolving, as need testing solution; Other gets Poria cocos control medicinal material 4g, and the 50ml that adds diethyl ether adds hot reflux 1-2 hour, filters, and the filtrate room temperature volatilizes, and residue adds normal hexane 0.5ml dissolving, in contrast medicinal material solution; Test according to thin-layered chromatography, draw control medicinal material solution 2 μ l, sample solution 8 μ l, put respectively on same silica gel g thin-layer plate, take sherwood oil (30～60 ℃)-acetone and ethyl acetate (80-90: 12-18: 1) as developping agent, presaturation 10-20 minute, launch, take out, dry, observe under the uviol lamp (365nm); In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color;
(4) get the quite described composition material medicine of preparation 10g,, porphyrize, the 30ml that adds diethyl ether adds hot reflux 25-35 minute, lets cool, and filters, and filtrate volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Other gets magnolol, honokiol reference substance, adds respectively methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin-layered chromatography, draw the about 10 μ l of need testing solution, reference substance solution 8 μ l, put respectively on same silica gel g thin-layer plate, take toluene-methyl alcohol (25-30: 1) as developping agent, launch, take out, dry, spray is with 1% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to the spot colour developing at 100 ℃; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
Assay:
(1) according to high effective liquid chromatography for measuring: chromatographic condition and system suitability octadecylsilane chemically bonded silica are filling agent (4.6 * 150mm, 5 μ m); Methanol-water (10-16: 6-9) be mobile phase; The detection wavelength is 225nm, and theoretical cam curve is calculated by costunolide should be not less than 3000;
The preparation of reference substance solution: accurately weighed costunolide reference substance 1mg, put in the 25ml measuring bottle, add the ethyl acetate dissolving, and be diluted to scale, shake up, filter with miillpore filter (0.45 μ m), and get final product;
The preparation of need testing solution: get the quite described composition material medicine of preparation 20g,, put in the tool plug Erlenmeyer flask, the accurate chloroform 100ml that adds, close plug shakes up, weighed weight, placement is spent the night, ultrasonic processing (power 200-400W, frequency 40KH Z) 20-40 minute, take out, let cool, close plug, weighed weight is supplied the weight that subtracts mistake with chloroform again, shake up, filter, precision is measured subsequent filtrate 20ml, put in the evaporating dish, volatilize, residue adds an amount of methyl alcohol, low-grade fever makes dissolving, is transferred in the 5ml measuring bottle, and is diluted to scale, shake up, filter with miillpore filter (0.45 μ m), and get final product;
Determination method: precision is drawn reference substance liquid, each 10 μ l injection liquid chromatography of test sample liquid respectively, measures, and get final product.
(2) according to high effective liquid chromatography for measuring
Chromatographic condition and system suitability are take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile-water-phosphoric acid (18: 82: 0.1) as mobile phase; The detection wavelength is 283nm, and number of theoretical plate is pressed aurantiin and calculated not the end in 2500;
It is an amount of, accurately weighed that the preparation of reference substance solution is taken at 110 ℃ of aurantiin reference substances that are dried to constant weight, adds methyl alcohol and make the solution that every 1ml contains 80 μ g, and get final product;
The preparation of need testing solution: get the quite described composition material medicine of preparation 10g, accurately weighed, put in the tool plug conical flask the accurate methyl alcohol 50ml that adds, close plug, weighed weight, ultrasonic processing (power 250W, frequency 40kHz) 45 minutes, let cool, weighed weight is supplied the weight that subtracts mistake with methyl alcohol again, shake up, filter, precision is measured subsequent filtrate 5ml, put in the 10ml measuring bottle, add methyl alcohol and be diluted to scale, shake up, filter with miillpore filter (0.45 μ m), get subsequent filtrate, and get final product;
Determination method: precision is drawn reference substance solution and need testing solution 10 a μ l respectively, and the injection liquid chromatography is measured, and be get final product.
Pharmaceutical composition method of quality control of the present invention is preferably as follows one or more in discrimination method and/or the assay:
Differentiate:
(1) get present composition granule 15g, add ethanol-strong ammonia solution (1: 1) 5ml, wetting, placed 20 minutes, add chloroform 20ml, ultrasonic processing 20 minutes filters, and filtrate evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution; Other gets the synephrine reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin-layered chromatography, draw need testing solution 20 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, take toluene-ethyl acetate-methyl alcohol-isopropyl alcohol-strong ammonia solution (12: 6: 3: 3: 1) as developping agent, put in the chromatography cylinder of ammonia saturated with vapor, launch, take out, dry, spray is with 0.5% ethanol solution of ninhydrin, about 5 minutes of 105 ℃ of bakings; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious identical purple dot;
(2) get present composition granule 5g, porphyrize adds water 20ml, chloroform 20ml, hydrochloric acid 3ml, adds hot reflux 1 hour, divides and gets chloroform layer, washes with water to neutrality, volatilizes, and residue adds absolute ethyl alcohol 1ml makes dissolving, as need testing solution; Other removes hydrogen constuslactone reference substance, adds absolute ethyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin-layered chromatography, draw control medicinal material solution 1 μ l, sample solution 2～4 μ l, put respectively on same silica gel g thin-layer plate, take sherwood oil (60～90 ℃)-toluene-ethyl acetate-glacial acetic acid (10: 20: 7: 0.5) as developping agent, launch, take out, dry, spray is with 1% vanillic aldehyde ethanol solution of sulfuric acid, and hot blast blows to clear spot; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
(3) get present composition granule 15g, porphyrize adds water 50ml dissolving, add diethyl ether and three times (25ml that at every turn adds diethyl ether, saturated nacl aqueous solution 10ml) of saturated nacl aqueous solution extraction, divide and get ether solution, room temperature volatilizes, residue adds normal hexane 0.5ml dissolving, as need testing solution; Other gets Poria cocos control medicinal material 4g, and the 50ml that adds diethyl ether added hot reflux 1 hour, filters, and the filtrate room temperature volatilizes, and residue adds normal hexane 0.5ml dissolving, in contrast medicinal material solution; Test according to thin-layered chromatography, draw control medicinal material solution 2 μ l, sample solution 8 μ l, put respectively on same silica gel g thin-layer plate, take sherwood oil (30～60 ℃)-acetone and ethyl acetate (84: 15: 1) as developping agent, presaturation 15 minutes launches, and takes out, dry, observe under the uviol lamp (365nm); In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color;
(4) get present composition granule 5g, porphyrize, the 30ml that adds diethyl ether added hot reflux 30 minutes, let cool, and filtered, and filtrate volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Other gets magnolol, honokiol reference substance, adds respectively methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to the thin-layered chromatography test, draw the about 10 μ l of need testing solution, reference substance solution 8 μ l, put respectively on same silica gel g thin-layer plate, take toluene-methyl alcohol (27: 1) as developping agent, launch, take out, dry, spray is with 1% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to the spot colour developing at 100 ℃; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
Assay:
(1) according to high effective liquid chromatography for measuring,
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filling agent (4.6 * 150mm, 5 μ m); Methanol-water (13: 7) is mobile phase; The detection wavelength is 225nm, and theoretical cam curve is calculated by costunolide should be not less than 3000;
The accurately weighed costunolide reference substance of the preparation of reference substance solution 1mg puts in the 25ml measuring bottle, adds the ethyl acetate dissolving, and is diluted to scale, shakes up, and filters with miillpore filter (0.45 μ m), and get final product;
It is an amount of that particle is got under the present composition granule content uniformity in the preparation of need testing solution, porphyrize, and precision takes by weighing about 10g, puts in the tool plug Erlenmeyer flask, the accurate chloroform 100ml that adds, close plug shakes up, weighed weight, placement is spent the night, ultrasonic processing (power 250W, frequency 40KH Z) 30 minutes, take out, let cool, close plug, weighed weight is supplied the weight that subtracts mistake with chloroform again, shake up, filter, precision is measured subsequent filtrate 20ml, put in the evaporating dish, volatilize, residue adds an amount of methyl alcohol, low-grade fever makes dissolving, is transferred in the 5ml measuring bottle, and is diluted to scale, shake up, filter with miillpore filter (0.45 μ m), and get final product;
Determination method: precision is drawn reference substance liquid, each 10 μ l injection liquid chromatography of test sample liquid respectively, measures, and get final product.
(2) according to high effective liquid chromatography for measuring
Chromatographic condition and system suitability are take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile-water-phosphoric acid (18: 82: 0.1) as mobile phase; The detection wavelength is 283nm, and number of theoretical plate is pressed aurantiin and calculated not the end in 2500;
It is an amount of, accurately weighed that the preparation of reference substance solution is taken at 110 ℃ of aurantiin reference substances that are dried to constant weight, adds methyl alcohol and make the solution that every 1ml contains 80 μ g, and get final product;
The preparation of need testing solution: get this product under the content uniformity item, porphyrize is got 5g, and is accurately weighed, put in the tool plug conical flask accurate methyl alcohol 50ml, close plug, the weighed weight of adding, ultrasonic processing (power 250W, frequency 40kHz) 45 minutes lets cool, more weighed weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, precision is measured subsequent filtrate 5ml, put in the 10ml measuring bottle, add methyl alcohol and be diluted to scale, shake up, filter with miillpore filter (0.45 μ m), get subsequent filtrate, and get final product;
Determination method is accurate reference substance solution and the need testing solution 10 μ l of drawing respectively, and the injection liquid chromatography is measured, and be get final product.
Described composition quality control method can be applied to the various formulations of composition, such as clinical acceptable formulations such as tablet, capsule, oral liquid, dripping pill, spray, granules, each formulation is when carrying out quality control, selected sample size all unified conversion is the amount of crude drug, such as " get preparation be equivalent to as described in composition material medicine 10g ", as granule namely quite be: composition granule 5g.
The present composition has good drug effect, compares existing preparation and shows good drug effect.The method of quality control of Chinese medicine composition provided by the present invention, by obtaining behind a large amount of concrete creative experiment sievings, pass through the screening to sample treatment in the discrimination method, the selection of developping agent, so that differentiate that specificity is fine, and method is economic and practical, the result is quick, and can both use different thin layer plates.Pass through the screening to sample, test sample disposal route in the content assaying method, the selection of developping agent, so that content assaying method can effectivelyly carry out quality control to product, and with the product that the method is measured to compare product that additive method measures pharmacological effect show more stable.
Embodiment
Following experimental example and embodiment are used for further specifying but are not limited to the present invention.
Choose medicine group of the present invention and carry out pharmacodynamic experiment research: medicine group I of the present invention (embodiment 1 preparation); Medicine group II of the present invention (embodiment 7 preparations)
Experimental example 1 is on the impact of rat gastric juice secreting function
70 of rats, be divided at random 7 groups, first, second, third group is gavage medicine group of the present invention I suspension 2.0,3.0,4.0g/kg respectively, pharmaceutical preparation 2.0,3.0, the 4.0g/kg of fourth, penta, oneself group gavage medicine group of the present invention II, organize gavage heptan with volume physiological saline, successive administration 7 days, fasting 24 hours (can't help water) after the last administration, etherization, open the abdominal cavity, the ligation pylorus injects above-mentioned various medicine 1.8ml (0.9g) through duodenum, then sew up the abdominal cavity, fasting was prohibited water 5 hours.Use etherization after 5 hours again, open the abdominal cavity, the ligation orifice of the stomach takes off stomach, filter gastric juice with two layers of cloth respectively, to the scale test tube, with the centrifugal 15min of 3000r/min, record supernatant liquid measure is gastric juice, uses respectively acidometer xylometric measurement, the special capillary test method of wheat, measures free acidity.Total acidity and pepsin activity the results are shown in following table:
Impact on rat gastric juice secreting function
Figure BSA00000389789700101
Figure BSA00000389789700111
Annotate: *P＜0.01
The result shows: invention medicine group I and medicine group II of the present invention all can promote to improve free acidity and total acidity discharge rate in mouse gastric secretion, compare with the physiological saline control group, pepsin activity is not made significant difference, and the effect of invention medicine group I same dose group is better than medicine group II of the present invention.
Experimental example 2 is on the impact of mouse small intestine ahead running
70 of mouse, be divided at random 7 groups, first, second, third group is gavage invention medicine group I suspension 4.0,6.0,8.0g/kg respectively, fourth, penta, own group gavage embodiment 7 suspension 6.0g/kg, organize gavage heptan with volume physiological saline, successive administration 7 days, fasting 24 hours (can't help water) after the last administration, the above-mentioned medicine of gavage is made into physiological water and contains carbon powder and each suspension 0.2ml/10g body weight of 10% of Arabic gum respectively, with the cervical vertebra dislocation method mouse is put to death after 15 minutes, cut the abdominal cavity open, take out intestines and stomach.Cut off the mesenterium that is attached on the intestinal tube, intestinal tube is not added traction ground be tiled in lightly (a little salt solution on the glass plate) on the glass plate.Take pylorus as starting point, measure the displacement of charcoal end in intestinal tube and the total length of small intestine (from pylorus to ileocecus), the displacement of calculating every mouse charcoal end accounts for small intestine total length percent, and namely little alvine pushing rate the results are shown in Table:
Group Dosage (g/kg) Little alvine pushing rate (%)
N.S 60.54±5.21
Invention medicine group I 4.0 81.18±4.73 **
Invention medicine group I 6.0 82.27±5.48 **
Invention medicine group I 8.0 84.23±4.15 **
Medicine group II of the present invention 4.0 72.23±4.29 *
Medicine group II of the present invention 6.0 73.87±5.09 *
Medicine group II of the present invention 8.0 76.47±4.89 *
Annotate: *P＜0.01; *P＜0.05
The result shows: invention medicine group I can promote the motion of mouse small intestine, with the physiological saline control group significant difference P＜0.01 is arranged relatively, and medicine group II of the present invention also has the mouse small intestine of promotion motion effect, but invention medicine group I effect is not strong.
The impact of experimental example 3 Dichlorodiphenyl Acetate type gastric ulcer
70 of rats, be divided at random 7 groups, then fasting is 24 hours, can't help water, under etherization, cut abdomen open by sterile working and draw stomach, behind the 2 dipping glacial acetic acid of the Lu scraps of paper with diameter 5mm, be posted on the 30Second of serous coat place, greater curvature both sides, remove rapidly the Lu scraps of paper, and dry with rayon balls, the reduction body of stomach is sewed up stomach wall.Postoperative begins feed and gastric infusion next day, grouping, dosage, through medicine with experiment 1, fasting is 24 hours after the last administration, dislocation is put to death, cut open the belly immediately and get stomach and fixing with 1% formalin, the interior pathology situation of record stomach, with ulcer length summation (mm) as UI, carry out statistical procedures, the results are shown in Table:
The impact of Dichlorodiphenyl Acetate type gastric ulcer
Group Dosage (g/kg) UI (mm)
N.S 140±2.83
Invention medicine group I 2.0 5.6±0.12 ***
Invention medicine group I 3.0 2.9±0.10 ***
Invention medicine group I 4.0 3.2±0.11 ***
Medicine group II of the present invention 2.0 5.4±0.12 ***
Medicine group II of the present invention 3.0 3.0±0.13 ***
Medicine group II of the present invention 4.0 3.9±0.13 ***
Annotate: * *P＜0.001
The result shows: medicine group of the present invention has obvious inhibiting effect to rat acetic acid type gastric ulcer, with the physiological saline control group significant differences P＜0.001 is arranged relatively, and it does in order to the invention medicine group I effect of 3.0g/kg best.
Experimental example 4 is differentiated screening experiment
We get the different preparations of medicine of the present invention, carry out respectively micro-discriminating, prove that this discrimination method is stable, and the thin layer that is applicable to all preparations under this its preparation process is differentiated.
The thin-layer identification method of 1 banksia rose:
1) different need testing solution preparation methods' selection:
Need testing solution one: get pharmaceutical preparation 5g of the present invention, porphyrize adds water 20ml, chloroform 20ml, hydrochloric acid 3ml, adds hot reflux 1 hour, divides and gets chloroform layer, washes with water to neutrality, volatilizes, and residue adds absolute ethyl alcohol 1ml makes dissolving, as need testing solution;
Need testing solution two: get pharmaceutical preparation 15g of the present invention, porphyrize adds 60-90 ℃ of sherwood oil 50ml, floods 25-35 minute, and ultrasonic processing 25-35 minute filters, and filtrate volatilizes, and residue adds absolute ethyl alcohol 1ml makes dissolving, as need testing solution.
2) different developping agents and ratio:
Developping agent one: sherwood oil (60-90 ℃)-benzene-ethyl acetate-glacial acetic acid (10: 20: 7: 0.5); Developping agent two: cyclohexane-acetone (10: 1).
3) selection of different contrast solutions
Contrast solution one: the dehydro-α-curcumene reference substance adds absolute ethyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution;
Contrast solution two: banksia rose control medicinal material 0.5g, add ethyl acetate 10ml, ultrasonic processing 25-35 minute, filter, filtrate is medicinal material solution in contrast.
According to the thin-layered chromatography test, put respectively above-mentioned two kinds of need testing solutions, two kinds of each 5 μ l of contrast solution at two silica gel g thin-layer plates, with above-mentioned two kinds of different developping agents, launch, take out, to dry, spray is with 1% vanillic aldehyde ethanol solution of sulfuric acid, and hot blast blows to clear spot.Compare the color developing effect of the need testing solution of two kinds of extracting method preparations, the results are shown in following table:
Figure BSA00000389789700131
As can be seen from the above table, adopt the color developing effect of need testing solution one, developping agent one good, the Pass Test requirement.And reference substance solution is good than control medicinal material solution color developing effect, so two kinds of methods are all feasible.
2) developping agent proportioning preferred in the discrimination method of the above-mentioned banksia rose: draw the as stated above need testing solution 10 μ l of preparation, reference substance solution one, two each 5 μ l, put respectively on same silica gel g thin-layer plate, take sherwood oil (60-90 ℃)-toluene-ethyl acetate-glacial acetic acid proportioning as (5: 30: 2: 0.5) (5: 25: 7: 0.5) (10: 20: 7: 0.5) (15: 15: 7: 0.5) as developping agent, launch, take out, dry, spray is with 1% vanillic aldehyde ethanol solution of sulfuric acid, it is clear that hot blast blows to the spot colour developing, puts respectively under daylight and the ultraviolet lamp (365nm) and inspect.Observe the effect that test sample launches on each thin layer plate, the results are shown in following table:
The developping agent proportioning 5∶30∶2∶0.5 5∶25∶7∶0.5 10∶20∶7∶0.5 15∶15∶7∶0.5
The Rf value 0.38 0.40 0.45 0.78
The developping agent proportioning is 10: 20: 7 as can be seen from the above table: 0.5 o'clock, it is best that need testing solution launches effect, and appearance hangover, spot separate the phenomenons such as bad.
3) mensuration of dehydro-α-curcumene detectability in the discrimination method of the above-mentioned banksia rose contains 0.03mg, 0.05mg, 0.1mg, 0.2mg in every 1ml reference substance solution.Reference substance solution one, two each 1 μ l, put respectively on same silica gel g thin-layer plate, take sherwood oil (60-90 ℃)-toluene-ethyl acetate-glacial acetic acid (10: 20: 7: 0.5) as developping agent, launch, take out, dry, spray is with 1% vanillic aldehyde ethanol solution of sulfuric acid, it is clear that hot blast blows to the spot colour developing, puts respectively under daylight and the ultraviolet lamp (365nm) and inspect.Observe the effect of test sample principal spot colour developing on the thin layer plate, the results are shown in following table:
Figure BSA00000389789700141
Test sample concentration is when 0.1mg/ml as can be seen from the above table, and it is clear to develop the color at thin layer plate, is fit to testing requirements.So with 10 -6G is decided to be the detectability of dehydro-α-curcumene.
4) sample solution concentration preferred in the discrimination method of the above-mentioned banksia rose contains this product 1g, 3g, 0.5g, 0.7g in every 1ml need testing solution.Reference substance solution one, two each 1 μ l need testing solution, 3 μ l, put respectively on same silica gel g thin-layer plate, take sherwood oil (60-90 ℃)-toluene-ethyl acetate-glacial acetic acid (27: 53: 19: 1) as developping agent, launch, take out, dry, spray is with 1% vanillic aldehyde ethanol solution of sulfuric acid, it is clear that hot blast blows to the spot colour developing, puts respectively under daylight and the ultraviolet lamp (365nm) and inspect.Observe the effect of test sample principal spot colour developing on the thin layer plate, the results are shown in following table:
Figure BSA00000389789700151
Test sample concentration is when 0.5g/ml as can be seen from the above table, and it is clear to develop the color at thin layer plate, is fit to testing requirements.So 5g/ml is decided to be the test sample concentration of dehydro-α-curcumene.
4) negative control test
Get the negative sample that lacks the banksia rose, prepare negative control solution according to need testing solution preparation method in the above-mentioned discrimination method (2), on reference substance solution one corresponding position, corresponding spot do not occur after launching, illustrate that selected identification experiment specificity is strong.And at reference substance solution two correspondence positions corresponding light spot is arranged, illustrate that selected identification experiment does not have specificity, so get rid of contrast two.
2, the thin-layer identification method of Poria cocos:
1) different need testing solution preparation methods' selection:
Need testing solution one: get pharmaceutical preparation 15g of the present invention, porphyrize, add water 50ml dissolving, add diethyl ether and three times (25ml that at every turn adds diethyl ether, saturated nacl aqueous solution 1ml) of saturated nacl aqueous solution extraction, divide and get ether solution, room temperature volatilizes, and residue adds normal hexane 0.5ml makes dissolving, as need testing solution;
Need testing solution two: get pharmaceutical preparation 5-15g of the present invention, the 40-60ml that adds diethyl ether, refluxing extraction 20-40 minute, filter, filtrate volatilizes, and residue adds the 0.5-2ml normal hexane makes dissolving, as need testing solution.
Need testing solution three: get pharmaceutical preparation 5-15g of the present invention, the 25-75ml that adds diethyl ether, refluxing extraction 15-45 minute, filter, filtrate volatilizes, and residue adds the 0.5-1.5ml normal hexane makes dissolving, as need testing solution.
2) selection of different contrast solutions
Contrast solution one: the Poria cocos control medicinal material, the 50ml that adds diethyl ether added hot reflux 1 hour, considered, and the filtrate room temperature volatilizes, and residue adds normal hexane 0.5ml makes dissolving, in contrast medicinal material solution;
Contrast solution two: the Poria cocos control medicinal material, the 40-60ml that adds diethyl ether adds hot reflux 20-40 minute, filters, and filtrate volatilizes, and residue adds normal hexane 0.5-2ml makes dissolving, in contrast medicinal material solution.
Contrast solution three: the Poria cocos control medicinal material, the 25-75ml that adds diethyl ether adds hot reflux 15-45 minute, filters, and filtrate volatilizes, and residue adds normal hexane 0.5-1.5ml makes dissolving, in contrast medicinal material solution.
Test according to thin-layered chromatography, put respectively above-mentioned two kinds of need testing solutions, two kinds of each 5 μ l of contrast solution at two silica gel g thin-layer plates, take sherwood oil (30-60 ℃)-acetone and ethyl acetate (84: 15: 1) as developping agent, presaturation 15 minutes, launch, take out, dry, put and observe (365nm) under the uviol lamp.Compare the color developing effect of the need testing solution of two kinds of extracting method preparations, the results are shown in following table:
Figure BSA00000389789700161
As can be seen from the above table, adopt the color developing effect of need testing solution one, developping agent one good, the Pass Test requirement.
2) the middle developping agent proportioning of above-mentioned discrimination method (2) is preferred: draw above-mentioned need testing solution one and reference substance solution one each 5 μ l, put respectively on same silica gel g thin-layer plate, take sherwood oil (30-60 ℃)-acetone and ethyl acetate (84: 15: 1) as developping agent, presaturation 15 minutes, launch, take out, dry, put and observe (365nm) under the uviol lamp.Observe the effect that test sample launches on each thin layer plate, the results are shown in following table:
The developping agent proportioning 84∶15∶1 60∶5∶0.5 70∶5∶0.5 100∶30∶20
Launch effect Good Better Better Poor
The developping agent proportioning is 84: 15: 1 o'clock as can be seen from the above table, and it is best that need testing solution launches effect, and appearance hangover, spot separate the phenomenons such as bad, unintelligible.
3) the middle sample solution point sample amount of above-mentioned discrimination method (2) is preferred, get need testing solution 1 μ l, 2 μ l, 3 μ l, 5 μ l, control medicinal material solution one 5 μ l, put respectively on same silica gel g thin-layer plate, take sherwood oil (30-60 ℃)-acetone and ethyl acetate (84: 15: 1) as developping agent, presaturation 15 minutes, launch, take out, dry, put and observe (365nm) under the uviol lamp.Observe the effect of test sample principal spot colour developing on the thin layer plate, the results are shown in following table:
Figure BSA00000389789700171
Test sample point sample amount is when 5 μ l as can be seen from the above table, and color developing effect is good on thin layer plate, is fit to testing requirements.
4) negative control test
Get the negative sample that lacks Poria cocos, prepare negative control solution according to above-mentioned need testing solution preparation method, on control medicinal material solution correspondence position, corresponding spot do not occur after launching, illustrate that selected identification experiment specificity is strong.
3, the thin-layer identification method of the bark of official magnolia:
Different need testing solution preparation methods' selection:
Method one: get pharmaceutical preparation 5g of the present invention, 30ml adds diethyl ether; Added hot reflux 0.5 hour, and took out, let cool, filter, filtrate evaporate to dryness, residue add ethyl acetate 2ml makes dissolving, as need testing solution.
Method two: get pharmaceutical preparation 5g of the present invention, add methyl alcohol 50ml, close plug, jolting 30 minutes filters, and filtrate is as need testing solution.
Draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, take toluene one methyl alcohol (96.5: 3.5) as developping agent, launch, take out, dry, spray is with 1% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to the spot colour developing at 100 ℃.Compare the color developing effect of the need testing solution of two kinds of extracting method preparations, the results are shown in following table:
Extracting method Method one Method two
Color developing effect Color developing effect is good It is clear to develop the color, and interference is arranged.
As can be seen from the above table, the color developing effect of two method need testing solutions is all good, but the method two negative test has interference, so method one Pass Test requirement.
Experimental example 5 assay shaker tests
1. test apparatus
Detecting instrument (room temperature detection): Agilent 1100 type high performance liquid chromatographs;
Octadecylsilane chemically bonded silica (4.6 * 150mm, 5 μ m)
Producer: Agilent Technologies Anjelen Sci. ﹠ Tech. Inc (China)
Mobile phase: methanol-water (13: 7)
Detect wavelength: 225nm
Flow velocity: 1.0ml/min
Column temperature: room temperature
The reference substance source: costunolide is purchased from Nat'l Pharmaceutical ﹠ Biological Products Control Institute's lot number: 1512-200001
Assay method: the preparation method who gets by the lower need testing solution of [assay] item prepares sample liquid; And by [method for making] lower blank sample that lacks the banksia rose for preparing, preparation negative controls.Filter with miillpore filter (0.45 μ m).Precision is drawn each 10 μ l of negative controls, reference substance liquid and need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
2. the investigation of test sample condition determination:
(1) investigation of extraction solvent amount:
By method under the assay item need testing solution is detected.Take by weighing three parts of every part of 5g of this product by the method precision under the preparation of need testing solution, put respectively in the tool plug conical flask, respectively accurate chloroform 15ml, 50ml, the 100ml of adding.
The content of costunolide is determined to add the chloroform amount as index in every gram medicine, and measurement result sees the following form:
Add the chloroform test findings
Figure BSA00000389789700191
Above result shows: add chloroform 50ml, the every gram medicine of 100ml gained content determination of costunolide is basic identical, select according to needs of production to add chloroform 50ml.
(2) ultrasonic time is investigated:
By method under the assay item need testing solution is detected.Need testing solution prepares 3 parts, and ultrasonic processing is 10 minutes, 30 minutes, 50 minutes respectively.
The content of costunolide is determined ultrasonic time as index in every gram medicine.Measurement result sees the following form:
The ultrasonic time test findings
Above result shows: 30 minutes, the 50 minutes every gram medicines of gained of ultrasonic time content determination of costunolide is basic identical, selects 30 minutes according to needs of production.
3. content assaying method is investigated:
(1) linear relationship is investigated and to be got reference substance solution (0.044mg/ml) and shake up, accurate 2,4,6,8,10, the 12 μ l of absorption inject high performance liquid chromatograph respectively, measure peak area, the results are shown in following table, and drawing standard curve, show that costunolide is linear between 0.088ug-0.528ug, its regression equation is:
Area＝1998.55256*Amt-0.2697686(r＝0.99958)
Figure BSA00000389789700193
(2) stability test reference substance solution respectively at rear 0,2,4,6,12,24 hour of preparation, is measured in accordance with the law, and the result shows that it is basicly stable in 24 hours, the results are shown in following table
Figure BSA00000389789700201
(3) the accurate need testing solution of drawing of precision test, (lot number: 02070903) 10 μ l, repeat sample introduction 5 times, try to achieve relative standard deviation＜2%, the results are shown in following table
Figure BSA00000389789700202
(4) the text method is pressed in the reappearance test, and (lot number: 02070903) sample is 5 parts, measures respectively, tries to achieve relative standard deviation＜2%, the results are shown in following table to get same lot number
(5) the recovery test precision take by weighing known content same lot number (lot number: sample 5g 02070601) more respectively precision take by weighing costunolide reference substance 0.35mg, press preparation method's operation of text need testing solution, measure its content, and calculate its recovery, measurement result sees the following form:
Figure BSA00000389789700204
Figure BSA00000389789700211
4. measurement result:
Figure BSA00000389789700212
Every bag contains the banksia rose with costunolide (C in this product 15H 20O 2), meter must not be less than 0.10mg.
The present composition is the preparation of embodiment 7 described in above-mentioned discriminating, the assay experiment, but following embodiment all can realize the described effect of above-mentioned experimental example
Embodiment
Embodiment 1: granule
Banksia rose 70g Divine Comedy (Jiao) 200g bighead atractylodes rhizome 100g
The dried orange peel 110g Poria cocos 110g tuber of pinellia (system) 110g
Rhizoma cyperi (vinegar system) the 60g dried immature fruit of citron orange (stir-fry) 60g cardamom (shelling) 60g
The bark of official magnolia (ginger system) 60g pawpaw 60g;
More than ten simply, Divine Comedy is ground into 100 purpose powder; The tuber of pinellia and ginger 33g make solvent according to the percolation under liquid extract and the extract item with 70% ethanol of 6 times of amounts of medicinal material, flood after 24 hours, and with the speed of per minute 1～3ml, diacolation slowly, the liquid of filtering is for subsequent use; The banksia rose, the bighead atractylodes rhizome, dried orange peel, the dried immature fruit of citron orange, cardamom, the bark of official magnolia are extracted volatile oil with the way of distillation, and the aqueous solution after the distillation in addition device is collected; The dregs of a decoction and Poria cocos, rhizoma cyperi, pawpaw and date 55g, boiling secondary, each 1.5 hours, collecting decoction filters, and filtrate and above-mentioned aqueous solution merge, concentrated relative density 1.10 (50～55 ℃), let cool, add equivalent ethanol, left standstill 24 hours, incline and get supernatant, filter, filtrate and above-mentioned filtrate merge, Recycled ethanol, being concentrated into relative density is the clear cream of 1.33～1.36 (50～55 ℃), 1 part of qinghuo reagent, 1.5 parts of cane sugar powders, 2 parts in dextrin, and above-mentioned powder, appropriate amount of ethanol, granulation, drying, add above-mentioned volatile oil, mixing is made 500g, and get final product.
Embodiment 2: soft capsule
Banksia rose 35g fructus amomi 45g bighead atractylodes rhizome 120g
The dried orange peel 120g Poria cocos 120g tuber of pinellia (system) 120g
Rhizoma cyperi (vinegar system) the 60g dried immature fruit of citron orange (stir-fry) 60g cardamom (shelling) 60g
The bark of official magnolia (ginger system) 60g Pogostemon cablin 60g Radix Glycyrrhizae 90g;
More than 12 flavors, the tuber of pinellia and ginger 36g make solvent according to the percolation under liquid extract and the extract item with 7 0% ethanol of 6 times of amounts of medicinal material, flood after 24 hours, with the speed of per minute 1～3ml, diacolation slowly, the liquid of filtering is for subsequent use; The banksia rose, fructus amomi, the bighead atractylodes rhizome, dried orange peel, the dried immature fruit of citron orange, cardamom, the bark of official magnolia, Pogostemon cablin extract volatile oil with the way of distillation, and the aqueous solution after the distillation in addition device is collected; Three flavor and the date 60g such as the dregs of a decoction and all the other Poria cocos, boiling secondary, each 1.5 hours, collecting decoction, filter, filtrate and above-mentioned aqueous solution merge, concentrated relative density 1.10 (50～55 ℃), let cool, add equivalent ethanol, left standstill 24 hours, incline and get supernatant, filter, filtrate and above-mentioned filtrate merge, Recycled ethanol, and being concentrated into relative density is the clear cream of 1.33～1.36 (50～55 ℃), drying under reduced pressure, be ground into fine powder, add vegetable oil and above-mentioned volatile oil, mixing, make 430, and get final product.
Embodiment 3: effervescent agent
Banksia rose 50g fructus amomi 30g bighead atractylodes rhizome 190g
The dried orange peel 200g Poria cocos 200g tuber of pinellia (system) 200g
Rhizoma cyperi (vinegar system) the 30g dried immature fruit of citron orange (stir-fry) 30g cardamom (shelling) 50g
The bark of official magnolia (ginger system) 60g Pogostemon cablin 50g Radix Glycyrrhizae 70g;
More than 12 flavors, the tuber of pinellia and ginger 60g make solvent according to the percolation under liquid extract and the extract item with 70% ethanol of 6 times of amounts of medicinal material, flood after 24 hours, with the speed of per minute 1～3ml, diacolation slowly, the liquid of filtering is for subsequent use; The banksia rose, fructus amomi, the bighead atractylodes rhizome, dried orange peel, the dried immature fruit of citron orange, cardamom, the bark of official magnolia, Pogostemon cablin extract volatile oil with the way of distillation, and the aqueous solution after the distillation in addition device is collected; Three flavor and the date 100g such as the dregs of a decoction and all the other Poria cocos, boiling secondary, each 1.5 hours, collecting decoction filters, and filtrate and above-mentioned aqueous solution merge, concentrated relative density 1.10 (50～55 ℃) lets cool, and adds equivalent ethanol, left standstill 24 hours, and inclined and get supernatant, filter, filtrate and above-mentioned filtrate merge, Recycled ethanol, being concentrated into relative density is the clear cream of 1.33～1.36 (50～55 ℃), drying under reduced pressure becomes dried cream, be ground into fine powder, add an amount of effervescent agent and auxiliary material, granulation, drying, add above-mentioned volatile oil, mixing is made 460g, and get final product.
Embodiment 4: capsule
Banksia rose 35g fructus amomi 45g bighead atractylodes rhizome 120g
The dried orange peel 120g Poria cocos 150g tuber of pinellia (system) 160g
Rhizoma cyperi (vinegar system) the 70g dried immature fruit of citron orange (stir-fry) 60g cardamom (shelling) 60g
The bark of official magnolia (ginger system) 60g Pogostemon cablin 60g Radix Glycyrrhizae 90g;
More than 12 flavors, the tuber of pinellia and ginger 48g make solvent according to the percolation under liquid extract and the extract item with 70% ethanol of 6 times of amounts of medicinal material, flood after 24 hours, with the speed of per minute 1～3ml, diacolation slowly, the liquid of filtering is for subsequent use; The banksia rose, fructus amomi, the bighead atractylodes rhizome, dried orange peel, the dried immature fruit of citron orange, cardamom, the bark of official magnolia, Pogostemon cablin extract volatile oil with the way of distillation, and the aqueous solution after the distillation in addition device is collected; Three flavor and the date 75g such as the dregs of a decoction and all the other Poria cocos, boiling secondary, each 1.5 hours, collecting decoction filters, and filtrate and above-mentioned aqueous solution merge, concentrated relative density 1.10 (50～55 ℃), let cool, add equivalent ethanol, left standstill 24 hours, incline and get supernatant, filter, filtrate and above-mentioned filtrate merge, Recycled ethanol, being concentrated into relative density is the clear cream of 1.33～1.36 (50～55 ℃), 1 part of qinghuo reagent, 1.5 parts of cane sugar powders, 2 parts in dextrin, appropriate amount of ethanol, granulation, drying, add above-mentioned volatile oil, mixing is made 515g, and get final product.
Embodiment 5: granule
Banksia rose 70g fructus amomi 70g bighead atractylodes rhizome 100g
The dried orange peel 130g Poria cocos 130g tuber of pinellia (system) 130g
Rhizoma cyperi (vinegar system) the 80g dried immature fruit of citron orange (stir-fry) 50g cardamom (shelling) 70g
The bark of official magnolia (ginger system) 50g Pogostemon cablin 50g Radix Glycyrrhizae 30g;
More than 12 flavors, the tuber of pinellia and ginger 39g make solvent according to the percolation under liquid extract and the extract item with 70% ethanol of 6 times of amounts of medicinal material, flood after 24 hours, with the speed of per minute 1～3ml, diacolation slowly, the liquid of filtering is for subsequent use; The banksia rose, fructus amomi, the bighead atractylodes rhizome, dried orange peel, the dried immature fruit of citron orange, cardamom, the bark of official magnolia, Pogostemon cablin extract volatile oil with the way of distillation, and the aqueous solution after the distillation in addition device is collected; Three flavor and the date 65g such as the dregs of a decoction and all the other Poria cocos, boiling secondary, each 1.5 hours, collecting decoction filters, and filtrate and above-mentioned aqueous solution merge, concentrated relative density 1.10 (50～55 ℃), let cool, add equivalent ethanol, left standstill 24 hours, incline and get supernatant, filter, filtrate and above-mentioned filtrate merge, Recycled ethanol, being concentrated into relative density is the clear cream of 1.33～1.36 (50～55 ℃), 1 part of qinghuo reagent, 1.5 parts of cane sugar powders, 2 parts in dextrin, appropriate amount of ethanol, granulation, drying, add above-mentioned volatile oil, mixing is made 480g, and get final product.
Embodiment 6: granule
Banksia rose 500g Divine Comedy (Jiao) 200g bighead atractylodes rhizome 200g
The dried orange peel 100g Poria cocos 100g tuber of pinellia (system) 100g
Rhizoma cyperi (vinegar system) the 50g dried immature fruit of citron orange (stir-fry) 70g cardamom (shelling) 60g
The bark of official magnolia (ginger system) 50g pawpaw 80g;
More than ten simply, Divine Comedy is ground into 100 purpose powder; The tuber of pinellia and ginger 30g make solvent according to the percolation under liquid extract and the extract item with 70% ethanol of 6 times of amounts of medicinal material, flood after 24 hours, and with the speed of per minute 1～3ml, diacolation slowly, the liquid of filtering is for subsequent use; The banksia rose, the bighead atractylodes rhizome, dried orange peel, the dried immature fruit of citron orange, cardamom, the bark of official magnolia are extracted volatile oil with the way of distillation, and the aqueous solution after the distillation in addition device is collected; The dregs of a decoction and Poria cocos, rhizoma cyperi, pawpaw and date 50g, boiling secondary, each 1.5 hours, collecting decoction filters, and filtrate and above-mentioned aqueous solution merge, concentrated relative density 1.10 (50～55 ℃), let cool, add equivalent ethanol, left standstill 24 hours, incline and get supernatant, filter, filtrate and above-mentioned filtrate merge, Recycled ethanol, being concentrated into relative density is the clear cream of 1.33～1.36 (50～55 ℃), 1 part of qinghuo reagent, 1.5 parts of cane sugar powders, 2 parts in dextrin, and above-mentioned powder, appropriate amount of ethanol, granulation, drying, add above-mentioned volatile oil, mixing is made 755g, and get final product.
Embodiment 7: granule
Banksia rose 70g fructus amomi 70g bighead atractylodes rhizome 100g
The dried orange peel 100g Poria cocos 100g tuber of pinellia (system) 100g
Rhizoma cyperi (vinegar system) the 70g dried immature fruit of citron orange (stir-fry) 70g cardamom (shelling) 70g
The bark of official magnolia (ginger system) 70g Pogostemon cablin 70g Radix Glycyrrhizae 30g;
More than 12 flavors, the tuber of pinellia and ginger 30g make solvent with 70% ethanol of 6 times of amounts of medicinal material, flood after 24 hours, with the speed of per minute 1～3ml, diacolation slowly, the liquid of filtering is for subsequent use; The banksia rose, fructus amomi, the bighead atractylodes rhizome, dried orange peel, the dried immature fruit of citron orange, cardamom, the bark of official magnolia, Pogostemon cablin extract volatile oil with the way of distillation, and the aqueous solution after the distillation in addition device is collected; Three flavor and the date 50g such as the dregs of a decoction and all the other Poria cocos, boiling secondary, each 1.5 hours, collecting decoction filters, and filtrate and above-mentioned aqueous solution merge, concentrated relative density 1.10 (50～55 ℃), let cool, add equivalent ethanol, left standstill 24 hours, incline and get supernatant, filter, filtrate and above-mentioned filtrate merge, Recycled ethanol, being concentrated into relative density is the clear cream of 1.33～1.36 (50～55 ℃), 1 part of qinghuo reagent, 1.5 parts of cane sugar powders, 2 parts in dextrin, appropriate amount of ethanol, granulation, drying, add above-mentioned volatile oil, mixing is made 460g, and get final product.
Differentiate
(1) get this product 15g, add ethanol-strong ammonia solution (1: 1) 5ml, wetting, placed 20 minutes, add chloroform 20ml, ultrasonic processing 20 minutes filters, and filtrate evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution; Other gets the synephrine reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin-layered chromatography, draw need testing solution 20 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, take toluene-ethyl acetate-methyl alcohol-isopropyl alcohol-strong ammonia solution (12: 6: 3: 3: 1) as developping agent, put in the chromatography cylinder of ammonia saturated with vapor, launch, take out, dry, spray is with 0.5% ethanol solution of ninhydrin, about 5 minutes of 105 ℃ of bakings; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious identical purple dot;
(2) get this product 5g, porphyrize adds water 20ml, chloroform 20ml, hydrochloric acid 3ml, adds hot reflux 1 hour, divides and gets chloroform layer, washes with water to neutrality, volatilizes, and residue adds absolute ethyl alcohol 1ml makes dissolving, as need testing solution; Other removes hydrogen constuslactone reference substance, adds absolute ethyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin-layered chromatography, draw control medicinal material solution 1 μ l, sample solution 2～4 μ l, put respectively on same silica gel g thin-layer plate, take sherwood oil (60～90 ℃)-toluene-ethyl acetate-glacial acetic acid (10: 20: 7: 0.5) as developping agent, launch, take out, dry, spray is with 1% vanillic aldehyde ethanol solution of sulfuric acid, and hot blast blows to clear spot; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
(3) get this product 15g, porphyrize adds water 50ml dissolving, add diethyl ether and three times (25ml that at every turn adds diethyl ether, saturated nacl aqueous solution 10ml) of saturated nacl aqueous solution extraction, divide and get ether solution, room temperature volatilizes, residue adds normal hexane 0.5ml dissolving, as need testing solution; Other gets Poria cocos control medicinal material 4g, and the 50ml that adds diethyl ether added hot reflux 1 hour, filters, and the filtrate room temperature volatilizes, and residue adds normal hexane 0.5ml dissolving, in contrast medicinal material solution; Test according to thin-layered chromatography, draw control medicinal material solution 2 μ l, sample solution 8 μ l, put respectively on same silica gel g thin-layer plate, take sherwood oil (30～60 ℃)-acetone and ethyl acetate (84: 15: 1) as developping agent, presaturation 15 minutes launches, and takes out, dry, observe under the uviol lamp (365nm); In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color;
(4) get this product 5g, porphyrize, the 30ml that adds diethyl ether added hot reflux 30 minutes, let cool, and filtered, and filtrate volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Other gets magnolol, honokiol reference substance, adds respectively methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to the thin-layered chromatography test, draw the about 10 μ l of need testing solution, reference substance solution 8 μ l, put respectively on same silica gel g thin-layer plate, take toluene-methyl alcohol (27: 1) as developping agent, launch, take out, dry, spray is with 1% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to the spot colour developing at 100 ℃; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
Assay:
(1) according to high effective liquid chromatography for measuring,
Chromatographic condition and system suitability: be filling agent (4.6 * 150mm, 5 μ m) with octadecylsilane chemically bonded silica; Methanol-water (13: 7) is mobile phase; The detection wavelength is 225nm, and theoretical cam curve is calculated by costunolide should be not less than 3000;
The accurately weighed costunolide reference substance of the preparation of reference substance solution 1mg puts in the 25ml measuring bottle, adds the ethyl acetate dissolving, and is diluted to scale, shakes up, and filters with miillpore filter (0.45 μ m), and get final product; (containing costunolide 0.04mg among every 1ml);
It is an amount of that particle is got under this product content uniformity in the preparation of need testing solution, porphyrize, and precision takes by weighing about 10g, puts in the tool plug Erlenmeyer flask, the accurate chloroform 100ml that adds, close plug shakes up, weighed weight, placement is spent the night, ultrasonic processing (power 250W, frequency 40KH Z) 30 minutes, take out, let cool, close plug, weighed weight is supplied the weight that subtracts mistake with chloroform again, shake up, filter, precision is measured subsequent filtrate 20ml, put in the evaporating dish, volatilize, residue adds an amount of methyl alcohol, low-grade fever makes dissolving, is transferred in the 5ml measuring bottle, and is diluted to scale, shake up, filter with miillpore filter (0.45 μ m), and get final product;
Determination method is accurate reference substance liquid, each 10 μ l injection liquid chromatography of test sample liquid drawn respectively, measures, and get final product; Every bag contains the banksia rose with costunolide (C in this product 15H 20O 2), meter must not be less than 0.25mg.
(2) according to high effective liquid chromatography for measuring
Chromatographic condition and system suitability are take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile-water-phosphoric acid (18: 82: 0.1) as mobile phase; The detection wavelength is 283nm, and number of theoretical plate is pressed aurantiin and calculated not the end in 2500.
It is an amount of, accurately weighed that the preparation of reference substance solution is taken at 110 ℃ of aurantiin reference substances that are dried to constant weight, adds methyl alcohol and make the solution that every 1ml contains 80 μ g, and get final product.
This product under the content uniformity item is got in the preparation of need testing solution, and porphyrize is got 5g, and is accurately weighed, put in the tool plug conical flask accurate methyl alcohol 50ml, close plug, the weighed weight of adding, ultrasonic processing (power 250W, frequency 40kHz) 45 minutes lets cool, more weighed weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, precision is measured subsequent filtrate 5ml, put in the 10ml measuring bottle, add methyl alcohol and be diluted to scale, shake up, filter with miillpore filter (0.45 μ m), get subsequent filtrate, and get final product.
Determination method: precision is drawn reference substance solution and need testing solution 10 a μ l respectively, and the injection liquid chromatography is measured, and be get final product.Every bag of this product contains dried orange peel with aurantiin (C 27H 32O 14) meter, must not be less than 4.0mg.
Function with cure mainly: warming middle-JIAO for easing the stomach.Be used for do not feel like eating, acid regurgitation, gastral cavilty is full vexed, the four limbs burnout.
Usage and consumption: boiling water is taken after mixing it with water, a 5g, 2 times on the one.
Specification: every packed 5g.

Claims (5)

1. the detection method with pharmaceutical composition of warming middle-JIAO for easing the stomach effect is characterized in that the method comprises the steps:
The bulk drug of described pharmaceutical composition consists of:
Figure FSB00000829945700011
This detection method comprises following discrimination method and content assaying method:
Differentiate:
(1) get the preparation of quite described composition material medicine 28-32g, add 1-2: 1-2 ethanol-strong ammonia solution 5ml, wetting, placed 15-30 minute, add chloroform 18-25ml, ultrasonic processing 15-30 minute, filter, filtrate evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution; Other gets the synephrine reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin-layered chromatography, draw need testing solution 20 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, take 10-15: 4-9: 2-6: 2-5: 1 toluene-ethyl acetate-methyl alcohol-isopropyl alcohol-strong ammonia solution is put in the chromatography cylinder of ammonia saturated with vapor as developping agent, launches, take out, dry, spray is with the 0.4-0.7% ethanol solution of ninhydrin, 105 ℃ of bakings about 4-7 minute; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious identical purple dot;
(2) get the preparation of quite described composition material medicine 10g, porphyrize adds water 20ml, chloroform 20ml, hydrochloric acid 3ml, adds hot reflux 1-2 hour, minute gets chloroform layer, washes with water to neutrality, volatilizes, and residue adds absolute ethyl alcohol 1ml makes dissolving, as need testing solution; Other removes hydrogen constuslactone reference substance, adds absolute ethyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin-layered chromatography, draw reference substance solution 1 μ l, need testing solution 2～4 μ l, put respectively on same silica gel g thin-layer plate, take the boiling range of 8-12: 18-22: 5-8: 0.4-0.7 as 60～90 ℃ of sherwood oil-toluene-ethyl acetate-glacial acetic acid as developping agent, launch, take out, dry, spray is with 1% vanillic aldehyde ethanol solution of sulfuric acid, and hot blast blows to clear spot; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
(3) get the preparation of quite described composition material medicine 28-32g, porphyrize, add water 50ml dissolving, add diethyl ether and saturated nacl aqueous solution extracts 2-4 time, add diethyl ether 20-30ml, saturated nacl aqueous solution 5-15ml minute get ether solution at every turn, and room temperature volatilizes, residue adds normal hexane 0.5ml dissolving, as need testing solution; Other gets Poria cocos control medicinal material 4g, and the 50ml that adds diethyl ether adds hot reflux 1-2 hour, filters, and the filtrate room temperature volatilizes, and residue adds normal hexane 0.5ml dissolving, in contrast medicinal material solution; Test according to thin-layered chromatography, draw control medicinal material solution 2 μ l, need testing solution 8 μ l, put respectively on same silica gel g thin-layer plate, take 80-90: 12-18: 1 boiling range as 30-60 ℃ of sherwood oil-acetone and ethyl acetate as developping agent, presaturation 10-20 minute, launch, take out, dry, observe under the 365nm uviol lamp; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color;
(4) get the preparation of quite described composition material medicine 10g, porphyrize, the 30ml that adds diethyl ether adds hot reflux 25-35 minute, lets cool, and filters, and filtrate volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Other gets magnolol, honokiol reference substance, adds respectively methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to the thin-layered chromatography test, draw the about 10 μ l of need testing solution, reference substance solution 8 μ l, put respectively on same silica gel g thin-layer plate, take 25-30: 1 toluene-methyl alcohol launches as developping agent, takes out, dry, spray is with 1% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to the spot colour developing at 100 ℃; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
Assay:
According to high effective liquid chromatography for measuring: chromatographic condition and system suitability are filling agent with octadecylsilane chemically bonded silica, 4.6 * 150mm, 5 μ m; 10-16: the 6-9 methanol-water is mobile phase; The detection wavelength is 225nm, and theoretical cam curve is calculated by costunolide should be not less than 3000; The preparation of reference substance solution: accurately weighed costunolide reference substance 1mg, put in the 25ml measuring bottle, add the ethyl acetate dissolving, and be diluted to scale, shake up, filter with miillpore filter, and get final product; The preparation of need testing solution: get the preparation of quite described composition material medicine 20g, put in the tool plug Erlenmeyer flask, the accurate chloroform 100ml that adds, close plug shakes up, weighed weight, placement is spent the night, ultrasonic processing 20-40 minute, power 200-400W, frequency 40KHz takes out, and lets cool, close plug, weighed weight is supplied the weight that subtracts mistake with chloroform again, shake up, filter, precision is measured subsequent filtrate 20ml, put in the evaporating dish, volatilize, residue adds an amount of methyl alcohol, low-grade fever makes dissolving, be transferred in the 5ml measuring bottle, and be diluted to scale, shake up, filter with miillpore filter, and get final product; Determination method: precision is drawn reference substance liquid, each 10 μ l injection liquid chromatography of test sample liquid respectively, measures, and get final product.
2. drug regimen object detecting method as claimed in claim 1 is characterized in that the bulk drug in this pharmaceutical composition consists of:
3. the detection method with pharmaceutical composition of warming middle-JIAO for easing the stomach effect is characterized in that the method comprises the steps:
The bulk drug of described pharmaceutical composition consists of:
Figure FSB00000829945700041
This detection method comprises following discrimination method and content assaying method:
Differentiate:
(1) get the preparation of quite described composition material medicine 28-32g, add 1-2: 1-2 ethanol-strong ammonia solution 5ml, wetting, placed 15-30 minute, add chloroform 18-25ml, ultrasonic processing 15-30 minute, filter, filtrate evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution; Other gets the synephrine reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin-layered chromatography, draw need testing solution 20 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, take 10-15: 4-9: 2-6: 2-5: 1 toluene-ethyl acetate-methyl alcohol-isopropyl alcohol-strong ammonia solution is put in the chromatography cylinder of ammonia saturated with vapor as developping agent, launches, take out, dry, spray is with the 0.4-0.7% ethanol solution of ninhydrin, 105 ℃ of bakings about 4-7 minute; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious identical purple dot;
(2) get the preparation of quite described composition material medicine 10g, porphyrize adds water 20ml, chloroform 20ml, hydrochloric acid 3ml, adds hot reflux 1-2 hour, minute gets chloroform layer, washes with water to neutrality, volatilizes, and residue adds absolute ethyl alcohol 1ml makes dissolving, as need testing solution; Other removes hydrogen constuslactone reference substance, adds absolute ethyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin-layered chromatography, draw reference substance solution 1 μ l, need testing solution 2～4 μ l, put respectively on same silica gel g thin-layer plate, take the boiling range of 8-12: 18-22: 5-8: 0.4-0.7 as 60～90 ℃ of sherwood oil-toluene-ethyl acetate-glacial acetic acid as developping agent, launch, take out, dry, spray is with 1% vanillic aldehyde ethanol solution of sulfuric acid, and hot blast blows to clear spot; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
(3) get the preparation of quite described composition material medicine 28-32g, porphyrize, add water 50ml dissolving, add diethyl ether and saturated nacl aqueous solution extracts 2-4 time, add diethyl ether 20-30ml, saturated nacl aqueous solution 5-15ml minute get ether solution at every turn, and room temperature volatilizes, residue adds normal hexane 0.5ml dissolving, as need testing solution; Other gets Poria cocos control medicinal material 4g, and the 50ml that adds diethyl ether adds hot reflux 1-2 hour, filters, and the filtrate room temperature volatilizes, and residue adds normal hexane 0.5ml dissolving, in contrast medicinal material solution; Test according to thin-layered chromatography, draw control medicinal material solution 2 μ l, need testing solution 8 μ l, put respectively on same silica gel g thin-layer plate, take 80-90: 12-18: 1 boiling range as 30-60 ℃ of sherwood oil-acetone and ethyl acetate as developping agent, presaturation 10-20 minute, launch, take out, dry, observe under the 365nm uviol lamp; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color;
(4) get the preparation of quite described composition material medicine 10g, porphyrize, the 30ml that adds diethyl ether adds hot reflux 25-35 minute, lets cool, and filters, and filtrate volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Other gets magnolol, honokiol reference substance, adds respectively methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to the thin-layered chromatography test, draw the about 10 μ l of need testing solution, reference substance solution 8 μ l, put respectively on same silica gel g thin-layer plate, take 25-30: 1 toluene-methyl alcohol launches as developping agent, takes out, dry, spray is with 1% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to the spot colour developing at 100 ℃; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
Assay:
According to high effective liquid chromatography for measuring: chromatographic condition and system suitability are filling agent with octadecylsilane chemically bonded silica, 4.6 * 150mm, 5 μ m; 10-16: the 6-9 methanol-water is mobile phase; The detection wavelength is 225nm, and theoretical cam curve is calculated by costunolide should be not less than 3000; The preparation of reference substance solution: accurately weighed costunolide reference substance 1mg, put in the 25ml measuring bottle, add the ethyl acetate dissolving, and be diluted to scale, shake up, filter with miillpore filter, and get final product; The preparation of need testing solution: get the preparation of quite described composition material medicine 20g, put in the tool plug Erlenmeyer flask, the accurate chloroform 100ml that adds, close plug shakes up, weighed weight, placement is spent the night, ultrasonic processing 20-40 minute, power 200-400W, frequency 40KHz takes out, and lets cool, close plug, weighed weight is supplied the weight that subtracts mistake with chloroform again, shake up, filter, precision is measured subsequent filtrate 20ml, put in the evaporating dish, volatilize, residue adds an amount of methyl alcohol, low-grade fever makes dissolving, be transferred in the 5ml measuring bottle, and be diluted to scale, shake up, filter with miillpore filter, and get final product; Determination method: precision is drawn reference substance liquid, each 10 μ l injection liquid chromatography of test sample liquid respectively, measures, and get final product.
4. drug regimen object detecting method as claimed in claim 3 is characterized in that the bulk drug of this pharmaceutical composition consists of:
5. such as claim 3 or 4 described drug regimen object detecting methods, it is characterized in that the preparation method of described pharmaceutical composition is:
The tuber of pinellia processed and ginger are made solvent with the 60-80% ethanol that medicinal material 5-7 doubly measures, and flood after 20-30 hour, and with the speed diacolation of per minute 1～6ml, the liquid of filtering is for subsequent use; The banksia rose, fructus amomi, the bighead atractylodes rhizome, dried orange peel, the stir-fry dried immature fruit of citron orange, the cardamom that shells, the ginger bark of official magnolia processed, Pogostemon cablin extract volatile oil with the way of distillation, and the aqueous solution after the distillation in addition device is collected; Three flavor and the dates such as the dregs of a decoction and all the other Poria cocos, boiling 2-3 time, each 1-2.5 hour, collecting decoction, filter, filtrate and above-mentioned aqueous solution merge, and being concentrated into 50～55 ℃ of survey relative densities is 1.10, let cool, add equivalent ethanol, left standstill 20-30 hour, incline and get supernatant, filter, filtrate and the above-mentioned liquid of filtering merge, Recycled ethanol, and being concentrated into 50～55 ℃, to survey relative densities be 1.33～1.36 clear cream, 1 part of qinghuo reagent, cane sugar powder 1-3 part, dextrin 1-3 part, appropriate amount of ethanol, granulation, drying adds above-mentioned volatile oil, mixing, and get final product.
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