CN1970070A - Oral administered formulation for reducing fat and expelling toxins, preparation process and quality control method thereof - Google Patents

Abstract

The invention relates to an oral pharmaceutical preparation for antihyperglycemic and toxin expelling, its preparing process and quality control method, wherein the preparation is made mainly from rhubarb horsetails, cassia seed, haw, oriental wormwood, cape jasmine, oriental water plantain rhizome, fleece-flower root, zedoary, thorowax root and right amount of adjuvant. The preparation can be effectively used for the treatment of hyperlipoidemia.

Description

Defatting and poison expelling oral formulations and preparation method thereof and method of quality control

Technical field: the present invention relates to a kind of defatting and poison expelling oral formulations and preparation method thereof and method of quality control, belong to technical field of traditional Chinese medicine pharmacy.

Background technology: hyperlipemia belongs to that traditional Chinese medical science expectorant is turbid more, the expectorant stasis of blood, qi depression to blood stasis category, be meant a kind of state that dyslipidemias increases in the blood, mostly occur at middle-aged and elderly people, obesity crowd and greasy food of long-term happiness edible oil or heavy drinker have the medical history person of hyperlipemia family easily to send out the crowd especially.Hyperlipemia can cause obesity, fatty liver, atherosclerosis and cardiovascular and cerebrovascular disease.Defatting and poison expelling capsule just was disclosed in during " national standard for traditional Chinese medicines compilation " internal medicine feels concerned about heat-clearing and toxic substances removing, blood stasis dispelling blood fat reducing as far back as in 2002.Be used for the treatment of turbid stasis of blood mutual resistance, hyperlipidemia is clinically received good effect.Form by Radix Et Rhizoma Rhei, Herba Artemisiae Scopariae, Rhizoma Alismatis, Radix Polygoni Multiflori, Semen Cassiae, Fructus Crataegi etc. in the side.Radix Et Rhizoma Rhei is a monarch drug in the side, and nature and flavor hardship, cold is returned spleen, stomach, large intestine, liver, pericardium channel, the function purging heat and dredging bowels, removing pathogenic heat from blood and toxic substance from the body, eliminating blood stasis and inducing menstruation, decorporation just, protect the liver, hemostasis, blood fat reducing, infection, raising immunologic function.Herba Artemisiae Scopariae property hardship, suffering are slightly cold, and return spleen, stomach, liver, gallbladder meridian, clearing away damp-heat, jaundice eliminating subcutaneous ulcer.Rhizoma Alismatis property is sweet, cold, returns kidney, urinary bladder channel, diuresis, clearing away damp-heat.Radix Polygoni Multiflori hardship, sweet, puckery, temperature is returned liver, the heart, kidney channel, detoxifcation, eliminating carbuncle, loosening bowel to relieve constipation.Semen Cassiae is sweet, bitter, salty, is slightly cold, and returns liver, large intestine channel, clearing away heat to improve acuity of vision, loosening bowel to relieve constipation.In calendar year 2001 the patent application of defatting and poison expelling capsule is just arranged, but original preparation formulation is single, can not satisfy market demand; And defatting and poison expelling preparation function cures mainly and is blood stasis dispelling blood fat reducing, the relieving constipation Cuo that disappears, and is used for the Simple Obesity due to the stagnation of turbidity and stasis, hyperlipemia, and acne, thereby a large amount of sugar should not arranged in the adjuvant.In addition, in the existing quality standard, the discrimination method feminine gender of Radix Et Rhizoma Rhei, Radix Polygoni Multiflori has interference, and the assay of jasminoidin becomes swarming to separate also incomplete with other, the quality of defatting and poison expelling preparation be can not effectively control, thereby production and the quality and the clinical efficacy thereof of product influenced.

Summary of the invention:

The objective of the invention is to: a kind of defatting and poison expelling oral formulations and preparation method thereof and method of quality control are provided, and this oral formulations comprises tablet and granule.The present invention is directed to the deficiencies in the prior art, adjuvant, preparation technology and the method for quality control of defatting and poison expelling oral formulations carried out research and preferred, satisfied requirement of different patients, and can effectively control the quality of said preparation, thereby guaranteed its clinical efficacy.

The present invention constitutes like this: calculate according to composition by weight: it is made by Radix Et Rhizoma Rhei 30-300 part, Semen Cassiae 100-500 part, Fructus Crataegi 100-500 part, Herba Artemisiae Scopariae 100-500 part, Fructus Gardeniae 50-200 part, Rhizoma Alismatis 100-400 part, Radix Polygoni Multiflori 100-400 part, Rhizoma Curcumae 100-400 part, Radix Bupleuri 50-300 part and appropriate amount of auxiliary materials.

Specifically, it is made by Radix Et Rhizoma Rhei 150g, Semen Cassiae 300g, Fructus Crataegi 300g, Herba Artemisiae Scopariae 300g, Fructus Gardeniae 100g, Rhizoma Alismatis 250g, Radix Polygoni Multiflori 250g, Rhizoma Curcumae 250g, Radix Bupleuri 150g and appropriate amount of auxiliary materials.

Described oral formulations is tablet or granule.

The preparation method of defatting and poison expelling oral formulations of the present invention is: get Radix Et Rhizoma Rhei, Semen Cassiae, Radix Polygoni Multiflori, Rhizoma Alismatis and add ethanol extraction, merge extractive liquid, leaves standstill, and filters, and filtrate is condensed into thick paste, and drying is ground into fine powder, and is standby; Fructus Gardeniae, Radix Bupleuri, Rhizoma Curcumae, Fructus Crataegi, Herba Artemisiae Scopariae decoct with water, and filter, and collecting decoction is got supernatant concentration and become thick paste, and drying is ground into fine powder, with above-mentioned fine powder mixing, adds appropriate amount of auxiliary materials then and makes different preparations.

Specifically, get Radix Et Rhizoma Rhei, Semen Cassiae, Radix Polygoni Multiflori, Rhizoma Alismatis and add 5～12 times of amount 30～85% ethanol extractions 1～5 time, 2～6 hours for the first time, 1～5 hour for the second time, 0.5～3 hour for the third time, fourth, fifth time each 0.5～2 hour.Merge extractive liquid, leaves standstill, and filters, and filtrate is condensed into thick paste, and drying is ground into fine powder, and is standby; Fructus Gardeniae, Radix Bupleuri, Rhizoma Curcumae, Fructus Crataegi, Herba Artemisiae Scopariae add 3～15 times of water gagings and decoct 1～5 time, and 1～4 hour for the first time, second and third time each 0.5～3 hour, fourth, fifth time each 0.5～2 hour, filter, collecting decoction is got supernatant concentration and is become thick paste, drying is ground into fine powder, with above-mentioned fine powder mixing; The pregelatinized Starch that adds medicated powder total amount 15～40%, mixing, dry pressing is granulated, granulate, it is an amount of to add 0.1～0.6% magnesium stearate and pregelatinized Starch again, and making gross weight is 280g, mix homogeneously, tabletting, the bag film-coat promptly gets tablet; Add dextrin in the mixed powder: mannitol=1: 2 is an amount of, mixing, and packing promptly gets granule.

More precisely, get Radix Et Rhizoma Rhei, Semen Cassiae, Radix Polygoni Multiflori, Rhizoma Alismatis and add 8 times of amount 65% ethanol extractions three times, 4 hours for the first time, 3 hours for the second time, 2 hours for the third time, merge extractive liquid, left standstill, and filtered, and filtrate is condensed into thick paste, and drying is ground into fine powder, and is standby; Fructus Gardeniae, Radix Bupleuri, Rhizoma Curcumae, Fructus Crataegi, Herba Artemisiae Scopariae add 10 times of water gagings and decoct three times, and 3 hours for the first time, second and third time each 2 hours filtered, and collecting decoction is got supernatant concentration and become thick paste, and drying is ground into fine powder, with above-mentioned fine powder mixing; The pregelatinized Starch that adds medicated powder total amount 26%, mixing, dry pressing is granulated, granulate, it is an amount of to add 0.3% magnesium stearate and pregelatinized Starch again, and making gross weight is 280g, mix homogeneously, tabletting, the bag film-coat promptly gets tablet; Add dextrin in the mixed powder: mannitol=1: 2 is an amount of, mixing, and packing promptly gets granule.

The method of quality control of defatting and poison expelling tablet of the present invention and granule is: described method of quality control mainly comprise in character, discriminating, inspection and the assay project partly or entirely; Wherein differentiate the thin layer chromatography discriminating that comprises Radix Et Rhizoma Rhei, Fructus Crataegi, Fructus Gardeniae and Rhizoma Alismatis in the preparation; Assay is that the contained jasminoidin of Fructus Gardeniae in the preparation is carried out assay.

The discrimination method of Radix Et Rhizoma Rhei is to be contrast with the Radix Et Rhizoma Rhei control medicinal material, is the thin layer chromatography of developing solvent with the upper solution of 30～60 ℃ petroleum ether-formic acid second fat-formic acid=5-25: 1-10: 0.1-2; The discrimination method of Fructus Crataegi is to be contrast with the ursolic acid reference substance, and with petroleum ether benzene glacial acetic acid ethyl acetate=5-15: 10-30: 0.1-1: 1-10 is the thin layer chromatography of developing solvent; The discrimination method of Fructus Gardeniae is to be contrast with the jasminoidin reference substance, is the thin layer chromatography of developing solvent with ethyl acetate-acetone-formic acid-water=5-15: 1-12: 0.5-5: 0.1-1; The discrimination method of Rhizoma Alismatis is to be contrast with the Rhizoma Alismatis control medicinal material, is the thin layer chromatography of developing solvent with toluene-ethyl acetate-formic acid=5-15: 0.5-5: 0.1-0.8.

Discrimination method comprises the part or all of of following project:

(1) get tablet or granule, fine ground, add methanol, close plug soaks, and filters, get the filtrate evaporate to dryness, residue is dissolved in water, and adds hydrochloric acid again, reflux, cooling immediately, extract with the ether jolting, divide and get ether solution, evaporate to dryness, residue add the chloroform dissolving, as need testing solution; Other gets the Radix Et Rhizoma Rhei control medicinal material, shines medical material solution in pairs with legal system; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw above-mentioned need testing solution and control medicinal material solution, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, upper solution with 30～60 ℃ petroleum ether-formic acid second fat-formic acid=5-25: 1-10: 0.1-2 is developing solvent, launch, take out, dry, put under the 200-500nm ultraviolet light and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence principal spot of same color;

(2) get tablet or granule, pulverize, add ether, reflux filters, and filtrate volatilizes, and residue adds ethanol, as need testing solution; Other gets the ursolic acid reference substance, adds ethanol and makes reference substance solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw above-mentioned need testing solution and reference substance solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether-benzene-glacial acetic acid-ethyl acetate=5-15: 10-30: 0.1-1: 1-10 is developing solvent, launches, and takes out, dry, spray is with sulphuric acid ethanol liquid, and it is clear to be heated to the speckle colour developing at 90～120 ℃, puts under the 200-500nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical fluorescence speckle;

(3) get tablet or granule, porphyrize, the jolting that adds diethyl ether discards ether solution, and residue volatilizes, and adds ethyl acetate, and reflux filters, and filtrate volatilizes, and residue adds ethanol makes dissolving, as need testing solution; Other gets the jasminoidin reference substance, adds ethanol and makes reference substance solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ethyl acetate-acetone-formic acid-water=5-15: 1-12: 0.5-5: 0.1-1 is developing solvent, launches, and takes out, dry, spray is with ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 110 ℃, inspects under the daylight; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;

(4) get tablet or granule, porphyrize is dissolved in water, and transferring PH with sodium hydroxide is 12～13, add ether and saturated aqueous common salt and fully vibrate, divide and get ether layer, water layer repeats once combined ether layer according to last method again, volatilize, residue adds ethyl acetate makes dissolving, as need testing solution; Other gets the Rhizoma Alismatis control medicinal material, adds water boil, filters, and filtrate concentrates, and transferring PH with sodium hydroxide is 12～13, adds diethyl ether and saturated aqueous common salt, shines medical material solution in pairs with legal system; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, drawing above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with toluene-ethyl acetate-formic acid=5-15: 0.5-5: 0.1-0.8, room temperature condition launches down, take out, dry, spray is with ethanol solution of sulfuric acid, it is clear that hot blast blows to the speckle colour developing, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.

Concrete discrimination method comprises the part or all of of following project:

(1) get 2～8 in tablet or granule 2～8g, fine ground, add methanol 10～40ml, close plug soaked 0.5～2 hour, filtered, get filtrate 2～8ml, evaporate to dryness, residue add water 5～20ml makes dissolving, add hydrochloric acid 0.5～2ml again, reflux 15～60 minutes, cooling immediately, divide 2 joltings to extract with ether, each 10～40ml merges ether solution, evaporate to dryness, residue add chloroform 0.5～3ml dissolving, as need testing solution; Other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, shines medical material solution in pairs with legal system; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw need testing solution 10 μ l, control medicinal material solution 5 μ l, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, upper solution with 30～60 ℃ petroleum ether-formic acid second fat-formic acid=5-25: 1-10: 0.1-2 is developing solvent, launches, and takes out, dry, put under the 365nm ultraviolet light and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence principal spot of same color;

(2) get 2～8 in tablet or granule 2～8g, pulverize, the 10～40ml that adds diethyl ether, reflux 0.5～2 hour filters, and filtrate volatilizes, and residue adds ethanol 0.5～5ml makes dissolving, as need testing solution; Other gets the ursolic acid reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw need testing solution 5 μ l, reference substance solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether-benzene-glacial acetic acid-ethyl acetate=5-15: 10-30: 0.1-1: 1-10 is developing solvent, launches, and takes out, dry, spray is with 10% sulphuric acid ethanol liquid, and it is clear to be heated to the speckle colour developing at 90～120 ℃, puts under the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical fluorescence speckle;

(3) get 2～8 in tablet or granule 2～8g, porphyrize, the 5～30ml that adds diethyl ether, jolting 5～20 minutes, discard ether solution, residue volatilizes, and adds ethyl acetate 5～30ml, reflux 0.5～2 hour, filter, filtrate volatilizes, and residue adds ethanol 0.5～2ml makes dissolving, as need testing solution; Other gets the jasminoidin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw each 2 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ethyl acetate-acetone-formic acid water=5-15: 1-12: 0.5-5: 0.1-1 is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 110 ℃, inspects under the daylight; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;

(4) get 10～40 in tablet or granule 10～50g, porphyrize, add water 20～60ml, it is 12～13 that the sodium hydroxide with 15% is transferred PH, adds ether 20～60ml and saturated aqueous common salt 2～6ml and fully vibrates, divide and get ether layer, water layer repeats once according to last method again, and combined ether layer volatilizes, residue adds ethyl acetate 0.2～2ml makes dissolving, as need testing solution; Other gets Rhizoma Alismatis control medicinal material 1～3g, adds water 20～90ml, boils 15～60min, filters, and filtrate is concentrated into about 30ml, and it is 12～13 that the sodium hydroxide with 15% is transferred PH, adds diethyl ether and saturated aqueous common salt, shines medical material solution in pairs with legal system; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, drawing each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with toluene-ethyl acetate-formic acid=5-15: 0.5-5: 0.1-0.8, room temperature condition launches down, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear that hot blast blows to the speckle colour developing, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.

The content assaying method of jasminoidin is to be contrast with the jasminoidin reference substance in the Fructus Gardeniae, is the high performance liquid chromatography of mobile phase with methanol-water=15-40: 50-100.

The content assaying method of jasminoidin is:

According to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring:

Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water=15-40: 50-100 is a mobile phase; The detection wavelength is 240nm; Number of theoretical plate must not calculate with the jasminoidin peak and is lower than 4000;

The preparation precision of reference substance solution takes by weighing the jasminoidin reference substance, adds dissolve with methanol, shakes up, promptly;

Tablet or the granule under the content uniformity item got in the preparation of need testing solution, accurate claims surely, and the accurate methanol that adds claims decide weight, and supersound extraction is put coldly, adds methanol and supplies weight, shakes up, and gets the supernatant filtration, promptly;

Accurate respectively reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly;

In this preparation, tablet contains Fructus Gardeniae with jasminoidin C ₁₇H ₂₄O ₁₀Meter must not be less than the 0.25mg/ sheet; Granule contains Fructus Gardeniae with jasminoidin C for every bag ₁₇H ₂₄O ₁₀Meter must not be less than 1.0mg.

Content assaying method is more specifically:

According to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring:

Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water=15-40: 50-100 is a mobile phase; The detection wavelength is 240nm; Number of theoretical plate must not calculate with the jasminoidin peak and is lower than 4000;

The preparation precision of reference substance solution takes by weighing the jasminoidin reference substance, adds methanol and makes the solution that every 1ml contains jasminoidin 60.0 μ g, shakes up, promptly;

Tablet or the granule 0.5-2g under the content uniformity item got in the preparation of need testing solution, the accurate title, decide, precision adds methanol 10-50ml, claim to decide weight, supersound extraction was put cold after 20～60 minutes under power 250W, frequency 50kHZ condition, add methanol and supply weight, shake up, get supernatant and filter, promptly with being less than or equal to 0.45 μ m microporous filter membrane;

Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly;

In this preparation, tablet contains Fructus Gardeniae with jasminoidin C ₁₇H ₂₄O ₁₀Meter must not be less than the 0.25mg/ sheet; Granule contains Fructus Gardeniae with jasminoidin C for every bag ₁₇H ₂₄O ₁₀Meter must not be less than 1.0mg.

Method of quality control of the present invention comprises:

Character: for tablet, product is a Film coated tablets, is pale brown color to sepia after removing film-coat; Bitter in the mouth;

For granule, product is that pale brown color is to brown granular; It is sweet to distinguish the flavor of;

Differentiate: (1) gets tablet or granule, and is fine ground, adds methanol, and close plug soaks, and filters, get the filtrate evaporate to dryness, residue is dissolved in water, and adds hydrochloric acid again, reflux, cooling immediately, extract with the ether jolting, divide and get ether solution, evaporate to dryness, residue add the chloroform dissolving, as need testing solution; Other gets the Radix Et Rhizoma Rhei control medicinal material, shines medical material solution in pairs with legal system; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw above-mentioned need testing solution and control medicinal material solution, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, upper solution with 30～60 ℃ petroleum ether-formic acid second fat-formic acid=5-25: 1-10: 0.1-2 is developing solvent, launch, take out, dry, put under the 200-500nm ultraviolet light and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence principal spot of same color;

(2) get tablet or granule, pulverize, add ether, reflux filters, and filtrate volatilizes, and residue adds ethanol, as need testing solution; Other gets the ursolic acid reference substance, adds ethanol and makes reference substance solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw above-mentioned need testing solution and reference substance solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether-benzene-glacial acetic acid-ethyl acetate=5-15: 10-30: 0.1-1: 1-10 is developing solvent, launches, and takes out, dry, spray is with sulphuric acid ethanol liquid, and it is clear to be heated to the speckle colour developing at 90～120 ℃, puts under the 200-500nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical fluorescence speckle;

(3) get tablet or granule, porphyrize, the jolting that adds diethyl ether discards ether solution, and residue volatilizes, and adds ethyl acetate, and reflux filters, and filtrate volatilizes, and residue adds ethanol makes dissolving, as need testing solution; Other gets the jasminoidin reference substance, adds ethanol and makes reference substance solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ethyl acetate-acetone-formic acid-water=5-15: 1-12: 0.5-5: 0.1-1 is developing solvent, launches, and takes out, dry, spray is with ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 110 ℃, inspects under the daylight; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;

(4) get tablet or granule, porphyrize is dissolved in water, and transferring PH with sodium hydroxide is 12～13, add ether and saturated aqueous common salt and fully vibrate, divide and get ether layer, water layer repeats once combined ether layer according to last method again, volatilize, residue adds ethyl acetate makes dissolving, as need testing solution; Other gets the Rhizoma Alismatis control medicinal material, adds water boil, filters, and filtrate concentrates, and transferring PH with sodium hydroxide is 12～13, adds diethyl ether and saturated aqueous common salt, shines medical material solution in pairs with legal system; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, drawing above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with toluene-ethyl acetate-formic acid=5-15: 0.5-5: 0.1-0.8, room temperature condition launches down, take out, dry, spray is with ethanol solution of sulfuric acid, it is clear that hot blast blows to the speckle colour developing, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;

Check: should meet relevant every regulation under Chinese Pharmacopoeia appendix tablet of version in 2005 or the granule item;

Assay: jasminoidin shines an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring:

Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water=15-40: 50-100 is a mobile phase; The detection wavelength is 240nm; Number of theoretical plate must not calculate with the jasminoidin peak and is lower than 4000;

The preparation precision of reference substance solution takes by weighing the jasminoidin reference substance, adds dissolve with methanol, shakes up, promptly;

Tablet or the granule under the content uniformity item got in the preparation of need testing solution, accurate claims surely, and the accurate methanol that adds claims decide weight, and supersound extraction is put coldly, adds methanol and supplies weight, shakes up, and gets the supernatant filtration, promptly;

Accurate respectively reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly;

In this preparation, tablet contains Fructus Gardeniae with jasminoidin C ₁₇H ₂₄O ₁₀Meter must not be less than the 0.25mg/ sheet; Granule contains Fructus Gardeniae with jasminoidin C for every bag ₁₇H ₂₄O ₁₀Meter must not be less than 1.0mg.

Through discovering of applicant, adopt the quality of following method of quality control with this defatting and poison expelling oral formulations of easier control, be more conducive to guarantee the clinical efficacy of said preparation.So described method of quality control also can comprise:

Character: for tablet, product is a Film coated tablets, is pale brown color to sepia after removing film-coat; Bitter in the mouth;

For granule, product is that pale brown color is to brown granular; It is sweet to distinguish the flavor of;

Differentiate: (1) gets 2～8 in tablet or granule 2～8g, and is fine ground, adds methanol 10～40ml, close plug soaked 0.5～2 hour, filtered, get filtrate 2～8ml, evaporate to dryness, residue add water 5～20ml makes dissolving, add hydrochloric acid 0.5～2ml again, reflux 15～60 minutes, cooling immediately, divide 2 joltings to extract with ether, each 10～40ml merges ether solution, evaporate to dryness, residue add chloroform 0.5～3ml dissolving, as need testing solution; Other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, shines medical material solution in pairs with legal system; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw need testing solution 10 μ l, control medicinal material solution 5 μ l, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, upper solution with 30～60 ℃ petroleum ether-formic acid second fat-formic acid=5-25: 1-10: 0.1-2 is developing solvent, launches, and takes out, dry, put under the 365nm ultraviolet light and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence principal spot of same color;

(2) get 2～8 in tablet or granule 2～8g, pulverize, the 10～40ml that adds diethyl ether, reflux 0.5～2 hour filters, and filtrate volatilizes, and residue adds ethanol 0.5～5ml makes dissolving, as need testing solution; Other gets the ursolic acid reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw need testing solution 5 μ l, reference substance solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether-benzene-glacial acetic acid-ethyl acetate=5-15: 10-30: 0.1-1: 1-10 is developing solvent, launches, and takes out, dry, spray is with 10% sulphuric acid ethanol liquid, and it is clear to be heated to the speckle colour developing at 90～120 ℃, puts under the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical fluorescence speckle;

(3) get 2～8 in tablet or granule 2～8g, porphyrize, the 5～30ml that adds diethyl ether, jolting 5～20 minutes, discard ether solution, residue volatilizes, and adds ethyl acetate 5～30ml, reflux 0.5～2 hour, filter, filtrate volatilizes, and residue adds ethanol 0.5～2ml makes dissolving, as need testing solution; Other gets the jasminoidin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw each 2 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ethyl acetate-acetone-formic acid water=5-15: 1-12: 0.5-5: 0.1-1 is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 110 ℃, inspects under the daylight; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;

(4) get 10～40 in tablet or granule 10～50g, porphyrize, add water 20～60ml, it is 12～13 that the sodium hydroxide with 15% is transferred PH, adds ether 20～60ml and saturated aqueous common salt 2～6ml and fully vibrates, divide and get ether layer, water layer repeats once according to last method again, and combined ether layer volatilizes, residue adds ethyl acetate 0.2～2ml makes dissolving, as need testing solution; Other gets Rhizoma Alismatis control medicinal material 1～3g, adds water 20～90ml, boils 15～60min, filters, and filtrate is concentrated into about 30ml, and it is 12～13 that the sodium hydroxide with 15% is transferred PH, adds diethyl ether and saturated aqueous common salt, shines medical material solution in pairs with legal system; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, drawing each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with toluene-ethyl acetate-formic acid=5-15: 0.5-5: 0.1-0.8, room temperature condition launches down, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear that hot blast blows to the speckle colour developing, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;

Check: should meet relevant every regulation under Chinese Pharmacopoeia appendix tablet of version in 2005 or the granule item;

Assay: jasminoidin shines an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring:

Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water=15-40: 50-100 is a mobile phase; The detection wavelength is 240nm; Number of theoretical plate must not calculate with the jasminoidin peak and is lower than 4000;

The preparation precision of reference substance solution takes by weighing the jasminoidin reference substance, adds methanol and makes the solution that every 1ml contains jasminoidin 60.0 μ g, shakes up, promptly;

Tablet or the granule 0.5-2g under the content uniformity item got in the preparation of need testing solution, the accurate title, decide, precision adds methanol 10-50ml, claim to decide weight, supersound extraction was put cold after 20～60 minutes under power 250W, frequency 50kHZ condition, add methanol and supply weight, shake up, get supernatant and filter, promptly with being less than or equal to 0.45 μ m microporous filter membrane;

Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly;

In this preparation, tablet contains Fructus Gardeniae with jasminoidin C ₁₇H ₂₄O ₁₀Meter must not be less than the 0.25mg/ sheet; Granule contains Fructus Gardeniae with jasminoidin C for every bag ₁₇H ₂₄O ₁₀Meter must not be less than 1.0mg.

The preparation method of preparation of the present invention and method of quality control are the preferred plan that obtains through a large amount of screenings, and following experimentation is a preferred process of the present invention.

Experiment 1: the screening of additive of tablet

Tablet is full extractum sheet, needs to add suitable filler, adhesive, and disintegrating agent and lubricant consider that the hygroscopicity of extract powder is strong, and is mobile poor, need make a certain size granule before the tabletting.

One, the screening of filler

Through data check, the filler of tablet has dextrin, sucrose, pregelatinized Starch etc.With disintegration time, hygroscopicity, compressibility is that index is screened filler, the results are shown in Table 1.

The screening of table 1 filler kind

Filler	Dextrin	Sucrose	Pregelatinized Starch
				Hygroscopicity	Slower	Comparatively fast	Slower
Disintegration time (min)	56	47	40
				Compressibility	Relatively poor	Better	Good

From table 1 result as seen, it is comparatively suitable to make filler with pregelatinized Starch.

Two, the selection of disintegrating agent

Pregelatinized Starch is a multi-functional auxiliary material, can make filler, has good flowability, compressibility, self-lubricity and dry adhesive, and disintegration is preferably arranged.

Aborning, the inside and outside addition of the general employing of disintegrating agent, can make the disintegrate of tablet not only occur in granule interior but also occur between the granule, thereby reach good disintegrate effect, usually add disintegrate dosage and account for 25%～50% of disintegrating agent total amount, in add disintegrate dosage and account for 75%～50% of disintegrating agent total amount, for the ratio that allows in the disintegrating agent, add more reasonable, with investigating its used ratio as index disintegration, the results are shown in Table 2.

The screening of the inside and outside additional proportion of table 2 disintegrating agent

The inside and outside addition ratio of disintegrating agent	5∶5	6∶4	7∶3	8∶2
					Disintegration time (min)	38	35	30	32

Evaluation of result: the amount of pregelatinized Starch 70% adds with interior addition, and it is best that addition adds effect beyond 30% the amount.

Three, the selection of method of granulating

Because of this preparation is full extractum sheet, the chance water viscosity is too big, so adopt the ethanol of high concentration to granulate and dry granulation as wetting agent, once makes particulate yield by investigation and selects granulating process, the results are shown in Table 3.

The selection result of table 3 concentration of alcohol

Method of granulating	Granule yield (%) in particle size range (grit number 20-60)
		85% ethanol	33
90% ethanol	47

95% ethanol	42
		Dry method	70

Interpretation of result: 90% following ethanol is made wetting agent, medicated powder conglomeration hardening, and color is profound, can not make soft material; 95% ethanol is made wetting agent and is granulated, and loose particles is inhomogeneous; Dry-pressing is granulated, granule is neat, of light color, because of the dry-pressing granulation need not add any wetting agent, granule just need not dried can be directly used in tabletting, can effectively keep contained heat-labile composition in the medicine, compare with wet processing, shortened process route, saved human and material resources and energy consumption, so preferred dry-pressing is granulated.

Four, the screening of lubricant

Lubricant can improve particulate flowability, is convenient to tabletting.Conventional lubricants has Pulvis Talci, magnesium stearate, micropowder silica gel etc., adds in the granule with same amount, surveys its angle of repose, investigates its influence to the tabletting process.The results are shown in Table 4.

The screening of table 4 lubricant kind

The lubricant kind	Pulvis Talci	Magnesium stearate	Micropowder silica gel
				Angle of repose	38.3°	35.7°	35.0°

The result is as seen: the lubricant effect of magnesium stearate and micropowder silica gel is suitable, and all good than Pulvis Talci, says from cost, selects magnesium stearate to be more suitable for.To further investigate its consumption below, the results are shown in Table 5.

The screening of table 5 magnesium stearate consumption

Consumption (%)	0.1	0.2	0.3	0.4	0.5
						Angle of repose	36.8°	36.3°	34.1°	33.4°	32.5°
Disintegration time (minute)	＜30	＜30	＜30	＞30	＞30
						Hardness (kg)	3.7	3.6	3.9	3.2	2.9

Therefore, determine the amount of the consumption of magnesium stearate for adding 0.3% in each prescription.

Experiment 2: the selection of granule adjuvant

Defatting and poison expelling preparation function cures mainly and is blood stasis dispelling blood fat reducing, the relieving constipation Cuo that disappears.Be used for the Simple Obesity due to the stagnation of turbidity and stasis, hyperlipemia, acne should not have a large amount of sugar in the adjuvant.Mix the back respectively with starch+mannitol, dextrin+mannitol by dried cream powder and survey the melting experiment, selected adjuvant is mainly dextrin+mannitol, as the examination index, selects the ratio between dextrin and the mannitol with flowability, melting, mouthfeel.The result is as follows:

Table 6 adjuvant is selected experimental result

Sample	Dried cream powder and ratio of adjuvant (0.2: 0.8)	Angle of repose (°)	Melting	Mouthfeel
					1	Dried cream powder+(dextrin+mannitol=1: 1)	28.2	Better	Better
2	Dried cream powder+(dextrin+mannitol=1: 2)	23.7	Good	Good
					3	Dried cream powder+(dextrin+mannitol=1: 3)	22.4	Good	Better

4	Dried cream powder+(dextrin+mannitol=2: 1)	30.5	Better	Poor slightly
					5	Dried cream powder+(dextrin+mannitol=3: 1)	32.1	Poor slightly	Difference

By above experiment, find that 2 and 3 result is more satisfactory, but the angle from reducing production costs determines that it is best that the dextrin and the ratio of mannitol are classified 1: 2 as.

Experiment 3: jasminoidin content assaying method research

1. need testing solution preparation method research

Method one: get this preparation 0.9g under the content uniformity item, the accurate title, decide, and places the 10ml measuring bottle, adds methanol and be diluted to scale, shakes up, and leaves standstill.Get supernatant with 0.45 μ m filtering with microporous membrane, accurately again draw subsequent filtrate 1ml and put in the 10ml measuring bottle, add methanol-water=be diluted to scale at 1: 1, shake up, as need testing solution.

Method two: get this preparation 0.9g under the content uniformity item, the accurate title, decide, precision adds methanol 25ml, claim to decide weight, supersound extraction was put cold after 45 minutes under power 250W, frequency 50kHZ condition, add methanol and supply weight, shake up, get supernatant and filter, promptly with being less than or equal to 0.45 μ m microporous filter membrane.

Method three: get this preparation 0.9g under the content uniformity item, put in the 100ml measuring bottle, adding distil water shakes up to scale, filters with being less than or equal to 0.45 μ m microporous filter membrane, gets subsequent filtrate, promptly.

Table 7

Sample	Method 1 (mg/g)	Method 2 (mg/g)	Method 3 (mg/g)
				1	0.658	0.831	0.622
2	0.700	0.852	0.654
				3	0.698	0.843	0.638

According to result of the test table 7 as can be known, adopt method two to prepare need testing solution, jasminoidin extracts more complete.

2. the selection of mobile phase

Mobile phase 1: methanol-water=27: 73 is a mobile phase

Mobile phase 2: acetonitrile-water=10: 90 is a mobile phase

Mobile phase 3: water-methanol-phosphoric acid=85: 15: 0.1

The result: with methanol-water=27: 73 was mobile phase, and defatting and poison expelling preparation good separation, jasminoidin separate fully (separating degree＞1.5) with close impurity peaks, so optimal flow is mutually: methanol-water=27: 73.

3. replica test

Get this preparation fine powder, the preparation method by test liquid under the assay item in the method for quality control of the present invention prepares 5 parts of test liquids respectively, and sample introduction is measured peak area, and the jasminoidin average content is 1.7027mg/g, and RSD is 0.59%.Show that repeatability is good, the results are shown in Table 8.

The replica test of jasminoidin in the table 8 preparation test sample

The sample introduction number of times	1	2	3	4	5	Meansigma methods	RSD(％)
								Peak area	1.7162	1.6956	1.7090	1.7012	1.6914	1.7027	0.59

4. stability test

Get this preparation fine powder, prepare test liquid by the preparation method of test liquid under the assay item in the method for quality control of the present invention, measure its jasminoidin peak area respectively at 0,2,4,6,8 hour, average peak area is 863144, and RSD is 0.27%.Show that jasminoidin is stable in 8 hours in the need testing solution, the results are shown in Table 9.

The stability test of jasminoidin in the table 9 preparation test sample

Time (hour)	0	2	4	6	8	Meansigma methods	RSD(％)
								Peak area	860904	864441	866394	861600	862380	863144	0.27

5. recovery test

Adopt the application of sample absorption method, each is an amount of for accurate this preparation of absorption (average content is 1.7027mg/g) respectively, put in the tool plug conical flask, (with methanol is solvent to accurate adding jasminoidin reference substance, make that to contain jasminoidin be 30.6 μ g/ml) solution 25ml, make test liquid by the preparation method of test liquid under the assay item in the method for quality control of the present invention.The accurate respectively 10 μ l of absorption inject chromatograph of liquid, and the record chromatograph is measured content, and calculate recovery rate sees Table 10.Average recovery rate is 99.07%, and RSD is 1.22%, proves that this method is feasible.

Jasminoidin is measured recovery test in table 10 need testing solution

Experiment number	Sample size (g)	Contain jasminoidin (mg)	Add jasminoidin (mg)	The amount of recording (mg)	The response rate (%)	Average recovery rate (%)	RSD (％)
								1	0.4438	0.7557	0.765	1.5025	97.62	99.07	1.22
2	0.4411	0.7511	1.5074	98.86
					3	0.4412	0.7512	1.5189	100.35
4	0.4413	0.7514	1.5185	100.27
					5	0.4470	0.7611	1.5128	98.26

6. method of quality control contrast experiment

The defatting and poison expelling granule: one hundred pharmaceutical Co. Ltd provides by the Guizhou benefit; The defatting and poison expelling sheet: one hundred pharmaceutical Co. Ltd provides by the Guizhou benefit.By the method for quality control and the method for quality control of the present invention of original standard product is differentiated and assay respectively.The results are shown in following table:

Table 11 method of quality control result contrast

	Former method defatting and poison expelling granule	Former method defatting and poison expelling tablet	Granule of the present invention	Tablet of the present invention
					Radix Et Rhizoma Rhei is differentiated	Feminine gender has interference	Feminine gender has interference	Negative noiseless, the speckle separating degree is good, and repeatability is good	Negative noiseless, the speckle separating degree is good, and repeatability is good
Fructus Crataegi is differentiated	Negative noiseless, repeatability is good	Negative noiseless, repeatability is good	Negative noiseless, repeatability is good	Negative noiseless, repeatability is good
					Radix Polygoni Multiflori is differentiated	Feminine gender has interference	Feminine gender has interference	Do not have	Do not have
Fructus Gardeniae is differentiated	Negative noiseless, repeatability is good	Negative noiseless, repeatability is good	Negative noiseless, repeatability is good	Negative noiseless, repeatability is good
					Rhizoma Alismatis is differentiated	Do not have	Do not have	The speckle separating degree is good, and negative noiseless, repeatability is good	The speckle separating degree is good, and negative noiseless, repeatability is good
Stability experiment RSD value (%)	0.58	0.62	0.27	0.26
					Response rate experiment RSD value (%)	1.60	1.55	1.22	1.21

The result shows that by method of quality control of the present invention, the quality of easier control product, stability is better, and accuracy is higher.

Compared with prior art, the adjuvant in the oral formulations provided by the present invention does not have and contains sugared composition, and preparation technology is reasonable, can more effectively treat hyperlipidemia, has satisfied requirement of different patients.Method of quality control accuracy height of the present invention, favorable reproducibility, good stability, response rate height has improved the quality control standard of defatting and poison expelling oral formulations, can effectively guarantee the clinical efficacy of said preparation.

The specific embodiment:

Embodiments of the invention 1: Radix Et Rhizoma Rhei 150g, Semen Cassiae 300g, Fructus Crataegi 300g, Herba Artemisiae Scopariae 300g, Fructus Gardeniae 100g, Rhizoma Alismatis 250g, Radix Polygoni Multiflori 250g, Rhizoma Curcumae 250g, Radix Bupleuri 150g

Get Radix Et Rhizoma Rhei, Semen Cassiae, Radix Polygoni Multiflori, Rhizoma Alismatis and add 8 times of amount 65% ethanol extractions three times, 4 hours for the first time, 3 hours for the second time, 2 hours for the third time, merge extractive liquid, left standstill, and filtered, and filtrate is condensed into thick paste, and drying is ground into fine powder, and is standby; Fructus Gardeniae, Radix Bupleuri, Rhizoma Curcumae, Fructus Crataegi, Herba Artemisiae Scopariae add 10 times of water gagings and decoct three times, and 3 hours for the first time, second and third time each 2 hours filtered, and collecting decoction is got supernatant concentration and become thick paste, and drying is ground into fine powder, with above-mentioned fine powder mixing; The pregelatinized Starch that adds medicated powder total amount 26%, mixing, dry pressing is granulated, granulate, it is an amount of to add 0.3% magnesium stearate and pregelatinized Starch again, and making gross weight is 280g, mix homogeneously, tabletting, the bag film-coat is made 1000 altogether, promptly gets tablet of the present invention.

Embodiments of the invention 2: Radix Et Rhizoma Rhei 30g, Semen Cassiae 100g, Fructus Crataegi 100g, Herba Artemisiae Scopariae 100g, Fructus Gardeniae 50g, Rhizoma Alismatis 100g, Radix Polygoni Multiflori 100g, Rhizoma Curcumae 100g, Radix Bupleuri 50g

Get Radix Et Rhizoma Rhei, Semen Cassiae, Radix Polygoni Multiflori, Rhizoma Alismatis and add 5 times of amount 30% ethanol extractions 6 hours, extracting solution leaves standstill, and filters, and filtrate is condensed into thick paste, and drying is ground into fine powder, and is standby; Fructus Gardeniae, Radix Bupleuri, Rhizoma Curcumae, Fructus Crataegi, Herba Artemisiae Scopariae add 3 times of water gagings and decocted 4 hours, filter, and collecting decoction is got supernatant concentration and become thick paste, and drying is ground into fine powder, with above-mentioned fine powder mixing; The pregelatinized Starch that adds medicated powder total amount 15%, mixing, dry pressing is granulated, granulate, it is an amount of to add 0.1% magnesium stearate and pregelatinized Starch again, and making gross weight is 280g, mix homogeneously, tabletting, the bag film-coat promptly gets tablet of the present invention.

Embodiments of the invention 3: Radix Et Rhizoma Rhei 300g, Semen Cassiae 500g, Fructus Crataegi 500g, Herba Artemisiae Scopariae 500g, Fructus Gardeniae 200g, Rhizoma Alismatis 400g, Radix Polygoni Multiflori 400g, Rhizoma Curcumae 400g, Radix Bupleuri 300g

Get Radix Et Rhizoma Rhei, Semen Cassiae, Radix Polygoni Multiflori, Rhizoma Alismatis and add 12 times of amount 85% ethanol extractions 5 times, 2 hours for the first time, 1 hour for the second time, third and fourth, five times each 0.5 hour, merge extractive liquid, leaves standstill, and filters, filtrate is condensed into thick paste, drying is ground into fine powder, and is standby; Fructus Gardeniae, Radix Bupleuri, Rhizoma Curcumae, Fructus Crataegi, Herba Artemisiae Scopariae add 15 times of water gagings and decoct 5 times, 1 hour for the first time, second and third, four, five times each 0.5 hour, filter, collecting decoction is got supernatant concentration and is become thick paste, drying is ground into fine powder, with above-mentioned fine powder mixing; The pregelatinized Starch that adds medicated powder total amount 40%, mixing, dry pressing is granulated, granulate, it is an amount of to add 0.6% magnesium stearate and pregelatinized Starch again, and making gross weight is 280g, mix homogeneously, tabletting, the bag film-coat promptly gets tablet of the present invention.

Embodiments of the invention 4: Radix Et Rhizoma Rhei 100g, Semen Cassiae 200g, Fructus Crataegi 200g, Herba Artemisiae Scopariae 200g, Fructus Gardeniae 80g, Rhizoma Alismatis 200g, Radix Polygoni Multiflori 200g, Rhizoma Curcumae 200g, Radix Bupleuri 100g

Get Radix Et Rhizoma Rhei, Semen Cassiae, Radix Polygoni Multiflori, Rhizoma Alismatis and add 10 times of amount 50% ethanol extractions twice, 6 hours for the first time, 5 hours for the second time, merge extractive liquid, left standstill, and filtered, and filtrate is condensed into thick paste, and drying is ground into fine powder, and is standby; Fructus Gardeniae, Radix Bupleuri, Rhizoma Curcumae, Fructus Crataegi, Herba Artemisiae Scopariae add 8 times of water gagings and decoct twice, and 4 hours for the first time, 3 hours for the second time, filter, collecting decoction is got supernatant concentration and is become thick paste, and drying is ground into fine powder, with above-mentioned fine powder mixing; Add dextrin: mannitol=1: 2 is an amount of, and mixing is made about 1000g, and packing promptly gets granule of the present invention.

Embodiments of the invention 5: the method for quality control of defatting and poison expelling tablet comprises:

Character: for tablet, product is a Film coated tablets, is pale brown color to sepia after removing film-coat; Bitter in the mouth.

Differentiate: (1) gets 4 in tablet, and is fine ground, adds methanol 20ml, close plug soaked 1 hour, filtered, get filtrate 5ml, evaporate to dryness, residue add water 10ml makes dissolving, add hydrochloric acid 1ml again, reflux 30 minutes, cooling immediately, divide 2 joltings to extract with ether, each 20ml merges ether solution, evaporate to dryness, residue add chloroform 1ml dissolving, as need testing solution.Other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, shines medical material solution in pairs with legal system.Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw need testing solution 10 μ l, control medicinal material solution 5 μ l, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, upper solution with 30～60 ℃ petroleum ether-formic acid second fat-formic acid=15: 5: 1 is developing solvent, launch, take out, dry, put under the ultraviolet light 365nm and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence principal spot of same color.

(2) get 4 in tablet, pulverize, the 30ml that adds diethyl ether, reflux 1 hour filters, and filtrate volatilizes, and residue adds ethanol 2ml makes dissolving, as need testing solution.Other gets the ursolic acid reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw need testing solution 5 μ l, reference substance solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether-benzene-glacial acetic acid-ethyl acetate=10: 20: 0.5: 5 was developing solvent, launches, and takes out, dry, spray is with 10% sulphuric acid ethanol liquid, and it is clear to be heated to the speckle colour developing at 110 ℃, puts under the 365nm ultra-violet lamp and inspects.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical fluorescence speckle.

(3) get 4 in tablet, porphyrize, the 15ml that adds diethyl ether, jolting 10 minutes discards ether solution, and residue volatilizes, and adds ethyl acetate 15ml, and reflux 1 hour filters, and filtrate volatilizes, and residue adds ethanol 1ml makes dissolving, as need testing solution.Other gets the jasminoidin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw each 2 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ethyl acetate-acetone-formic acid-water=10: 7: 2: 0.5 was developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 110 ℃, inspects under the daylight.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.

(4) get 24 in tablet, porphyrize, add water 40ml, it is 12～13 that the sodium hydroxide with 15% is transferred PH, adds ether 40ml and saturated aqueous common salt 4ml and fully vibrates, divide and get ether layer, water layer repeats once according to last method again, and combined ether layer volatilizes, residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Other gets Rhizoma Alismatis control medicinal material 2g, adds water 60ml, boils 30min, filters, and filtrate is concentrated into about 30ml, and it is 12～13 that the sodium hydroxide with 15% is transferred PH, adds diethyl ether and saturated aqueous common salt, shines medical material solution in pairs with legal system.Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, drawing each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with toluene-ethyl acetate-formic acid=10: 3: 0.3, room temperature condition launches down, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear that hot blast blows to the speckle colour developing, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.

Check: should meet relevant every regulation under an appendix tablet of Chinese Pharmacopoeia version in 2005 item.

Assay: jasminoidin shines an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring:

Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water=27: 73 is a mobile phase; The detection wavelength is 240nm.Number of theoretical plate must not calculate with the jasminoidin peak and is lower than 4000.

The preparation precision of reference substance solution takes by weighing the jasminoidin reference substance, adds methanol and makes the solution that every 1ml contains jasminoidin 60.0 μ g, shakes up, promptly.

The tablet 0.9g under the content uniformity item is got in the preparation of need testing solution, the accurate title, decide, precision adds methanol 25ml, claim to decide weight, supersound extraction was put cold after 45 minutes under power 250W, frequency 50kHZ condition, add methanol and supply weight, shake up, get supernatant with 0.45 μ m filtering with microporous membrane, promptly.

Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.

Every in this preparation contains Fructus Gardeniae with jasminoidin (C ₁₇H ₂₄O ₁₀) must not count and be less than 0.25mg.

Embodiments of the invention 6: the method for quality control of defatting and poison expelling granule comprises:

Character: for granule, product is that pale brown color is to brown granular; It is sweet to distinguish the flavor of.

Differentiate: (1) gets granule 2g, and is fine ground, adds methanol 10ml, close plug soaked 0.5 hour, filtered, get filtrate 2ml, evaporate to dryness, residue add water 5ml makes dissolving, add hydrochloric acid 0.5ml again, reflux 15 minutes, cooling immediately, divide 2 joltings to extract with ether, each 10ml merges ether solution, evaporate to dryness, residue add chloroform 0.5ml dissolving, as need testing solution.Other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, shines medical material solution in pairs with legal system.Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw need testing solution 10 μ l, control medicinal material solution 5 μ l, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, upper solution with 30～60 ℃ petroleum ether-formic acid second fat-formic acid=5: 10: 0.1 is developing solvent, launch, take out, dry, put under the 365nm ultraviolet light and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence principal spot of same color.

(2) get granule 2g, pulverize, the 10ml that adds diethyl ether, reflux 0.5 hour filters, and filtrate volatilizes, and residue adds ethanol 0.5ml makes dissolving, as need testing solution.Other gets the ursolic acid reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw need testing solution 5 μ l, reference substance solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether-benzene-glacial acetic acid-ethyl acetate=5: 30: 0.1: 10 was developing solvent, launches, and takes out, dry, spray is with 10% sulphuric acid ethanol liquid, and it is clear to be heated to the speckle colour developing at 90 ℃, puts under the 365nm ultra-violet lamp and inspects.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical fluorescence speckle.

(3) get granule 2g, porphyrize, the 5ml that adds diethyl ether, jolting 5 minutes discards ether solution, and residue volatilizes, and adds ethyl acetate 5ml, and reflux 0.5 hour filters, and filtrate volatilizes, and residue adds ethanol 0.5ml makes dissolving, as need testing solution.Other gets the jasminoidin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw each 2 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ethyl acetate-acetone-formic acid-water=5: 12: 0.5: 1 was developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 110 ℃, inspects under the daylight.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.

(4) get granule 10g, porphyrize, add water 20ml, it is 12～13 that the sodium hydroxide with 15% is transferred PH, adds ether 20ml and saturated aqueous common salt 2ml and fully vibrates, divide and get ether layer, water layer repeats once according to last method again, and combined ether layer volatilizes, residue adds ethyl acetate 0.2ml makes dissolving, as need testing solution.Other gets Rhizoma Alismatis control medicinal material 1g, adds water 20ml, boils 15min, filters, and filtrate is concentrated into about 30ml, and it is 12～13 that the sodium hydroxide with 15% is transferred PH, adds diethyl ether and saturated aqueous common salt, shines medical material solution in pairs with legal system.Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, drawing each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with toluene-ethyl acetate-formic acid=5: 5: 0.1, room temperature condition launches down, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear that hot blast blows to the speckle colour developing, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.

Check: should meet relevant every regulation under an appendix granule of Chinese Pharmacopoeia version in 2005 item.

Assay: jasminoidin shines an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring:

Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water=15: 100 is a mobile phase; The detection wavelength is 240nm; Number of theoretical plate must not calculate with the jasminoidin peak and is lower than 4000.

The preparation precision of reference substance solution takes by weighing the jasminoidin reference substance, adds methanol and makes the solution that every 1ml contains jasminoidin 60.0 μ g, shakes up, promptly.

The granule 0.5g under the content uniformity item is got in the preparation of need testing solution, the accurate title, decide, precision adds methanol 10ml, claim to decide weight, supersound extraction was put cold after 20 minutes under power 250W, frequency 50kHZ condition, add methanol and supply weight, shake up, get supernatant and filter, promptly with 0.30 μ m microporous filter membrane.

Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.

This granule contains Fructus Gardeniae with jasminoidin C for every bag ₁₇H ₂₄O ₁₀Meter must not be less than 1.0mg.

Embodiments of the invention 7: the method for quality control of defatting and poison expelling oral formulations of the present invention can comprise:

Character: for tablet, product is a Film coated tablets, is pale brown color to sepia after removing film-coat; Bitter in the mouth;

For granule, product is that pale brown color is to brown granular; It is sweet to distinguish the flavor of.

Differentiate: (1) gets 8 in tablet or granule 8g, and is fine ground, adds methanol 40ml, close plug soaked 2 hours, filtered, get filtrate 8ml, evaporate to dryness, residue add water 20ml makes dissolving, add hydrochloric acid 2ml again, reflux 60 minutes, cooling immediately, divide 2 joltings to extract with ether, each 40ml merges ether solution, evaporate to dryness, residue add chloroform 3ml dissolving, as need testing solution.Other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, shines medical material solution in pairs with legal system.Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw need testing solution 10 μ l, control medicinal material solution 5 μ l, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, upper solution with 30～60 ℃ petroleum ether-formic acid second fat-formic acid=25: 1: 2 is developing solvent, launch, take out, dry, put under the 365nm ultraviolet light and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence principal spot of same color.

(2) get 8 in tablet or granule 8g, porphyrize, the 30ml that adds diethyl ether, jolting 20 minutes discards ether solution, and residue volatilizes, and adds ethyl acetate 30ml, and reflux 2 hours filters, and filtrate volatilizes, and residue adds ethanol 2ml makes dissolving, as need testing solution.Other gets the jasminoidin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw each 2 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ethyl acetate-acetone-formic acid-water=15: 1: 5: 0.1 was developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 110 ℃, inspects under the daylight.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.

(3) get 40 in tablet or granule 50g, porphyrize, add water 60ml, it is 12～13 that the sodium hydroxide with 15% is transferred PH, adds ether 60ml and saturated aqueous common salt 6ml and fully vibrates, divide and get ether layer, water layer repeats once according to last method again, and combined ether layer volatilizes, residue adds ethyl acetate 2ml makes dissolving, as need testing solution.Other gets Rhizoma Alismatis control medicinal material 3g, adds water 90ml, boils 60min, filters, and filtrate is concentrated into about 30ml, and it is 12～13 that the sodium hydroxide with 15% is transferred PH, adds diethyl ether and saturated aqueous common salt, shines medical material solution in pairs with legal system.Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, drawing each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with toluene-ethyl acetate-formic acid=15: 0.5: 0.8, room temperature condition launches down, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear that hot blast blows to the speckle colour developing, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.

Check: should meet relevant every regulation under Chinese Pharmacopoeia appendix tablet of version in 2005 or the granule item.

Embodiments of the invention 8: the method for quality control of defatting and poison expelling oral formulations can comprise:

Character: for tablet, product is a Film coated tablets, is pale brown color to sepia after removing film-coat; Bitter in the mouth;

For granule, product is that pale brown color is to brown granular; It is sweet to distinguish the flavor of.

Differentiate: get 8 in tablet or granule 8g, pulverize, the 40ml that adds diethyl ether, reflux 2 hours filters, and filtrate volatilizes, and residue adds ethanol 5ml makes dissolving, as need testing solution.Other gets the ursolic acid reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw need testing solution 5 μ l, reference substance solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether-benzene-glacial acetic acid-ethyl acetate=15: 10: 1: 1 was developing solvent, launches, and takes out, dry, spray is with 10% sulphuric acid ethanol liquid, and it is clear to be heated to the speckle colour developing at 120 ℃, puts under the 365nm ultra-violet lamp and inspects.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical fluorescence speckle.

Assay: jasminoidin shines an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring:

Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water=40: 50 is a mobile phase; The detection wavelength is 240nm; Number of theoretical plate must not calculate with the jasminoidin peak and is lower than 4000.

The preparation precision of reference substance solution takes by weighing the jasminoidin reference substance, adds methanol and makes the solution that every 1ml contains jasminoidin 60.0 μ g, shakes up, promptly.

Tablet or the granule 2g under the content uniformity item got in the preparation of need testing solution, the accurate title, decide, precision adds methanol 50ml, claim to decide weight, supersound extraction was put cold after 60 minutes under power 250W, frequency 50kHZ condition, add methanol and supply weight, shake up, get supernatant and filter, promptly with 0.40 μ m microporous filter membrane.

Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.

In this preparation, tablet contains Fructus Gardeniae with jasminoidin C ₁₇H ₂₄O ₁₀Meter must not be less than the 0.25mg/ sheet; This granule contains Fructus Gardeniae with jasminoidin C for every bag ₁₇H ₂₄O ₁₀Meter must not be less than 1.0mg.

Claims (15)

1. defatting and poison expelling oral formulations, it is characterized in that: calculate according to composition by weight: it is made by Radix Et Rhizoma Rhei 30-300 part, Semen Cassiae 100-500 part, Fructus Crataegi 100-500 part, Herba Artemisiae Scopariae 100-500 part, Fructus Gardeniae 50-200 part, Rhizoma Alismatis 100-400 part, Radix Polygoni Multiflori 100-400 part, Rhizoma Curcumae 100-400 part, Radix Bupleuri 50-300 part and appropriate amount of auxiliary materials.

2. according to the described defatting and poison expelling oral formulations of claim 1, it is characterized in that: it is made by Radix Et Rhizoma Rhei 150g, Semen Cassiae 300g, Fructus Crataegi 300g, Herba Artemisiae Scopariae 300g, Fructus Gardeniae 100g, Rhizoma Alismatis 250g, Radix Polygoni Multiflori 250g, Rhizoma Curcumae 250g, Radix Bupleuri 150g and appropriate amount of auxiliary materials.

3. according to claim 1 or 2 described defatting and poison expelling oral formulations, it is characterized in that: described oral formulations is tablet or granule.

4. the preparation method of defatting and poison expelling oral formulations as claimed in claim 1 or 2 is characterized in that: get Radix Et Rhizoma Rhei, Semen Cassiae, Radix Polygoni Multiflori, Rhizoma Alismatis and add ethanol extraction, merge extractive liquid, leaves standstill, and filters, and filtrate is condensed into thick paste, and drying is ground into fine powder, and is standby; Fructus Gardeniae, Radix Bupleuri, Rhizoma Curcumae, Fructus Crataegi, Herba Artemisiae Scopariae decoct with water, and filter, and collecting decoction is got supernatant concentration and become thick paste, and drying is ground into fine powder, with above-mentioned fine powder mixing, adds appropriate amount of auxiliary materials then and makes different preparations.

5. according to the preparation method of the described defatting and poison expelling oral formulations of claim 4, it is characterized in that: get Radix Et Rhizoma Rhei, Semen Cassiae, Radix Polygoni Multiflori, Rhizoma Alismatis and add 5～12 times of amount 30～85% ethanol extractions 1～5 time, 2～6 hours for the first time, 1～5 hour for the second time, 0.5～3 hour for the third time, fourth, fifth time each 0.5～2 hour.Merge extractive liquid, leaves standstill, and filters, and filtrate is condensed into thick paste, and drying is ground into fine powder, and is standby; Fructus Gardeniae, Radix Bupleuri, Rhizoma Curcumae, Fructus Crataegi, Herba Artemisiae Scopariae add 3～15 times of water gagings and decoct 1～5 time, and 1～4 hour for the first time, second and third time each 0.5～3 hour, fourth, fifth time each 0.5～2 hour, filter, collecting decoction is got supernatant concentration and is become thick paste, drying is ground into fine powder, with above-mentioned fine powder mixing; The pregelatinized Starch that adds medicated powder total amount 15～40%, mixing, dry pressing is granulated, granulate, it is an amount of to add 0.1～0.6% magnesium stearate and pregelatinized Starch again, and making gross weight is 280g, mix homogeneously, tabletting, the bag film-coat promptly gets tablet; Add dextrin in the mixed powder: mannitol=1: 2 is an amount of, mixing, and packing promptly gets granule.

6. according to the preparation method of claim 4 or 5 described defatting and poison expelling oral formulations, it is characterized in that: get Radix Et Rhizoma Rhei, Semen Cassiae, Radix Polygoni Multiflori, Rhizoma Alismatis and add 8 times of amount 65% ethanol extractions three times, 4 hours for the first time, 3 hours for the second time, 2 hours for the third time, merge extractive liquid, leaves standstill, and filters, filtrate is condensed into thick paste, drying is ground into fine powder, and is standby; Fructus Gardeniae, Radix Bupleuri, Rhizoma Curcumae, Fructus Crataegi, Herba Artemisiae Scopariae add 10 times of water gagings and decoct three times, and 3 hours for the first time, second and third time each 2 hours filtered, and collecting decoction is got supernatant concentration and become thick paste, and drying is ground into fine powder, with above-mentioned fine powder mixing; The pregelatinized Starch that adds medicated powder total amount 26%, mixing, dry pressing is granulated, granulate, it is an amount of to add 0.3% magnesium stearate and pregelatinized Starch again, and making gross weight is 280g, mix homogeneously, tabletting, the bag film-coat promptly gets tablet; Add dextrin in the mixed powder: mannitol=1: 2 is an amount of, mixing, and packing promptly gets granule.

7. as the method for quality control of defatting and poison expelling oral formulations as described in each among the claim 1-6, described preparation comprises tablet and granule, it is characterized in that: described method of quality control mainly comprise in character, discriminating, inspection and the assay project partly or entirely; Wherein differentiate the thin layer chromatography discriminating that comprises Radix Et Rhizoma Rhei, Fructus Crataegi, Fructus Gardeniae and Rhizoma Alismatis in the preparation; Assay is that the contained jasminoidin of Fructus Gardeniae in the preparation is carried out assay.

8. according to the method for quality control of the described defatting and poison expelling oral formulations of claim 7, it is characterized in that: the discrimination method of Radix Et Rhizoma Rhei is to be contrast with the Radix Et Rhizoma Rhei control medicinal material, is the thin layer chromatography of developing solvent with the upper solution of 30～60 ℃ petroleum ether-formic acid second fat-formic acid=5-25: 1-10: 0.1-2; The discrimination method of Fructus Crataegi is to be contrast with the ursolic acid reference substance, is the thin layer chromatography of developing solvent with petroleum ether-benzene-glacial acetic acid-ethyl acetate=5-15: 10-30: 0.1-1: 1-10; The discrimination method of Fructus Gardeniae is to be contrast with the jasminoidin reference substance, is the thin layer chromatography of developing solvent with ethyl acetate-acetone-formic acid-water=5-15: 1-12: 0.5-5: 0.1-1; The discrimination method of Rhizoma Alismatis is to be contrast with the Rhizoma Alismatis control medicinal material, is the thin layer chromatography of developing solvent with toluene-ethyl acetate-formic acid=5-15: 0.5-5: 0.1-0.8.

9. according to the method for quality control of claim 7 or 8 described defatting and poison expelling oral formulations, it is characterized in that: discrimination method comprises the part or all of of following project:

(1) get tablet or granule, fine ground, add methanol, close plug soaks, and filters, get the filtrate evaporate to dryness, residue is dissolved in water, and adds hydrochloric acid again, reflux, cooling immediately, extract with the ether jolting, divide and get ether solution, evaporate to dryness, residue add the chloroform dissolving, as need testing solution; Other gets the Radix Et Rhizoma Rhei control medicinal material, shines medical material solution in pairs with legal system; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw above-mentioned need testing solution and control medicinal material solution, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, upper solution with 30～60 ℃ petroleum ether-formic acid second fat-formic acid=5-25: 1-10: 0.1-2 is developing solvent, launch, take out, dry, put under the 200-500nm ultraviolet light and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence principal spot of same color;

(2) get tablet or granule, pulverize, add ether, reflux filters, and filtrate volatilizes, and residue adds ethanol, as need testing solution; Other gets the ursolic acid reference substance, adds ethanol and makes reference substance solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw above-mentioned need testing solution and reference substance solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether-benzene-glacial acetic acid-ethyl acetate=5-15: 10-30: 0.1-1: 1-10 is developing solvent, launches, and takes out, dry, spray is with sulphuric acid ethanol liquid, and it is clear to be heated to the speckle colour developing at 90～120 ℃, puts under the 200-500nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical fluorescence speckle;

(3) get tablet or granule, porphyrize, the jolting that adds diethyl ether discards ether solution, and residue volatilizes, and adds ethyl acetate, and reflux filters, and filtrate volatilizes, and residue adds ethanol makes dissolving, as need testing solution; Other gets the jasminoidin reference substance, adds ethanol and makes reference substance solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ethyl acetate-acetone-formic acid-water=5-15: 1-12: 0.5-5: 0.1-1 is developing solvent, launches, and takes out, dry, spray is with ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 110 ℃, inspects under the daylight; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;

(4) get tablet or granule, porphyrize is dissolved in water, and transferring PH with sodium hydroxide is 12～13, add ether and saturated aqueous common salt and fully vibrate, divide and get ether layer, water layer repeats once combined ether layer according to last method again, volatilize, residue adds ethyl acetate makes dissolving, as need testing solution; Other gets the Rhizoma Alismatis control medicinal material, adds water boil, filters, and filtrate concentrates, and transferring PH with sodium hydroxide is 12～13, adds diethyl ether and saturated aqueous common salt, shines medical material solution in pairs with legal system; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, drawing above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with toluene-ethyl acetate-formic acid=5-15: 0.5-5: 0.1-0.8, room temperature condition launches down, take out, dry, spray is with ethanol solution of sulfuric acid, it is clear that hot blast blows to the speckle colour developing, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.

10. according to the method for quality control of the described defatting and poison expelling oral formulations of claim 9, it is characterized in that: concrete discrimination method comprises the part or all of of following project:

(1) get 2～8 in tablet or granule 2～8g, fine ground, add methanol 10～40ml, close plug soaked 0.5～2 hour, filtered, get filtrate 2～8ml, evaporate to dryness, residue add water 5～20ml makes dissolving, add hydrochloric acid 0.5～2ml again, reflux 15～60 minutes, cooling immediately, divide 2 joltings to extract with ether, each 10～40ml merges ether solution, evaporate to dryness, residue add chloroform 0.5～3ml dissolving, as need testing solution; Other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, shines medical material solution in pairs with legal system; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw need testing solution 10 μ l, control medicinal material solution 5 μ l, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, upper solution with 30～60 ℃ petroleum ether-formic acid second fat-formic acid=5-25: 1-10: 0.1-2 is developing solvent, launches, and takes out, dry, put under the 365nm ultraviolet light and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence principal spot of same color;

(2) get 2～8 in tablet or granule 2～8g, pulverize, the 10～40ml that adds diethyl ether, reflux 0.5～2 hour filters, and filtrate volatilizes, and residue adds ethanol 0.5～5ml makes dissolving, as need testing solution; Other gets the ursolic acid reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw need testing solution 5 μ l, reference substance solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether-benzene-glacial acetic acid-ethyl acetate=5-15: 10-30: 0.1-1: 1-10 is developing solvent, launches, and takes out, dry, spray is with 10% sulphuric acid ethanol liquid, and it is clear to be heated to the speckle colour developing at 90～120 ℃, puts under the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical fluorescence speckle;

(3) get 2～8 in tablet or granule 2～8g, porphyrize, the 5～30ml that adds diethyl ether, jolting 5～20 minutes, discard ether solution, residue volatilizes, and adds ethyl acetate 5～30ml, reflux 0.5～2 hour, filter, filtrate volatilizes, and residue adds ethanol 0.5～2ml makes dissolving, as need testing solution; Other gets the jasminoidin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw each 2 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ethyl acetate-acetone-formic acid-water=5-15: 1-12: 0.5-5: 0.1-1 is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 110 ℃, inspects under the daylight; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;

(4) get 10～40 in tablet or granule 10～50g, porphyrize, add water 20～60ml, it is 12～13 that the sodium hydroxide with 15% is transferred PH, adds ether 20～60ml and saturated aqueous common salt 2～6ml and fully vibrates, divide and get ether layer, water layer repeats once according to last method again, and combined ether layer volatilizes, residue adds ethyl acetate 0.2～2ml makes dissolving, as need testing solution; Other gets Rhizoma Alismatis control medicinal material 1～3g, adds water 20～90ml, boils 15～60min, filters, and filtrate is concentrated into about 30ml, and it is 12～13 that the sodium hydroxide with 15% is transferred PH, adds diethyl ether and saturated aqueous common salt, shines medical material solution in pairs with legal system; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, drawing each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with toluene-ethyl acetate-formic acid=5-15: 0.5-5: 0.1-0.8, room temperature condition launches down, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear that hot blast blows to the speckle colour developing, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.

11. method of quality control according to the described defatting and poison expelling oral formulations of claim 7, it is characterized in that: the content assaying method of jasminoidin is to be contrast with the jasminoidin reference substance in the Fructus Gardeniae, is the high performance liquid chromatography of mobile phase with methanol-water=15-40: 50-100.

12. the method for quality control according to claim 7 or 11 described defatting and poison expelling oral formulations is characterized in that: the content assaying method of jasminoidin is:

According to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring:

Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water=15-40: 50-100 is a mobile phase; The detection wavelength is 240nm; Number of theoretical plate must not calculate with the jasminoidin peak and is lower than 4000;

The preparation precision of reference substance solution takes by weighing the jasminoidin reference substance, adds dissolve with methanol, shakes up, promptly;

Tablet or the granule under the content uniformity item got in the preparation of need testing solution, accurate claims surely, and the accurate methanol that adds claims decide weight, and supersound extraction is put coldly, adds methanol and supplies weight, shakes up, and gets the supernatant filtration, promptly;

Accurate respectively reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly;

In this preparation, tablet contains Fructus Gardeniae in jasminoidin C17H24O10, must not be less than the 0.25mg/ sheet; Granule contains Fructus Gardeniae for every bag must not be less than 1.0mg in jasminoidin C17H24O10.

13. the method for quality control according to the described defatting and poison expelling oral formulations of claim 12 is characterized in that: content assaying method is more specifically:

According to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring:

Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water=15-40: 50-100 is a mobile phase; The detection wavelength is 240nm; Number of theoretical plate must not calculate with the jasminoidin peak and is lower than 4000;

The preparation precision of reference substance solution takes by weighing the jasminoidin reference substance, adds methanol and makes the solution that every 1ml contains jasminoidin 60.0 μ g, shakes up, promptly;

Tablet or the granule 0.5-2g under the content uniformity item got in the preparation of need testing solution, the accurate title, decide, precision adds methanol 10-50ml, claim to decide weight, supersound extraction was put cold after 20～60 minutes under power 250W, frequency 50kHZ condition, add methanol and supply weight, shake up, get supernatant and filter, promptly with being less than or equal to 0.45 μ m microporous filter membrane;

Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly;

In this preparation, tablet contains Fructus Gardeniae in jasminoidin C17H24O10, must not be less than the 0.25mg/ sheet; Granule contains Fructus Gardeniae for every bag must not be less than 1.0mg in jasminoidin C17H24O10.

14. the method for quality control according to the described defatting and poison expelling oral formulations of claim 7 is characterized in that: described method of quality control comprises:

Character: for tablet, product is a Film coated tablets, is pale brown color to sepia after removing film-coat; Bitter in the mouth;

For granule, product is that pale brown color is to brown granular; It is sweet to distinguish the flavor of;

Differentiate: (1) gets tablet or granule, and is fine ground, adds methanol, and close plug soaks, and filters, get the filtrate evaporate to dryness, residue is dissolved in water, and adds hydrochloric acid again, reflux, cooling immediately, extract with the ether jolting, divide and get ether solution, evaporate to dryness, residue add the chloroform dissolving, as need testing solution; Other gets the Radix Et Rhizoma Rhei control medicinal material, shines medical material solution in pairs with legal system; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw above-mentioned need testing solution and control medicinal material solution, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, upper solution with 30～60 ℃ petroleum ether-formic acid second fat-formic acid=5-25: 1-10: 0.1-2 is developing solvent, launch, take out, dry, put under the 200-500nm ultraviolet light and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence principal spot of same color;

(2) get tablet or granule, pulverize, add ether, reflux filters, and filtrate volatilizes, and residue adds ethanol, as need testing solution; Other gets the ursolic acid reference substance, adds ethanol and makes reference substance solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw above-mentioned need testing solution and reference substance solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether-benzene-glacial acetic acid-ethyl acetate=5-15: 10-30: 0.1-1: 1-10 is developing solvent, launches, and takes out, dry, spray is with sulphuric acid ethanol liquid, and it is clear to be heated to the speckle colour developing at 90～120 ℃, puts under the 200-500nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical fluorescence speckle;

(3) get tablet or granule, porphyrize, the jolting that adds diethyl ether discards ether solution, and residue volatilizes, and adds ethyl acetate, and reflux filters, and filtrate volatilizes, and residue adds ethanol makes dissolving, as need testing solution; Other gets the jasminoidin reference substance, adds ethanol and makes reference substance solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ethyl acetate-acetone-formic acid-water=5-15: 1-12: 0.5-5: 0.1-1 is developing solvent, launches, and takes out, dry, spray is with ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 110 ℃, inspects under the daylight; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;

(4) get tablet or granule, porphyrize is dissolved in water, and transferring PH with sodium hydroxide is 12～13, add ether and saturated aqueous common salt and fully vibrate, divide and get ether layer, water layer repeats once combined ether layer according to last method again, volatilize, residue adds ethyl acetate makes dissolving, as need testing solution; Other gets the Rhizoma Alismatis control medicinal material, adds water boil, filters, and filtrate concentrates, and transferring PH with sodium hydroxide is 12～13, adds diethyl ether and saturated aqueous common salt, shines medical material solution in pairs with legal system; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, drawing above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with toluene-ethyl acetate-formic acid=5-15: 0.5-5: 0.1-0.8, room temperature condition launches down, take out, dry, spray is with ethanol solution of sulfuric acid, it is clear that hot blast blows to the speckle colour developing, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;

Check: should meet relevant every regulation under Chinese Pharmacopoeia appendix tablet of version in 2005 or the granule item;

Assay: jasminoidin shines an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring:

Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water=15-40: 50-100 is a mobile phase; The detection wavelength is 240nm; Number of theoretical plate must not calculate with the jasminoidin peak and is lower than 4000;

The preparation precision of reference substance solution takes by weighing the jasminoidin reference substance, adds dissolve with methanol, shakes up, promptly;

Tablet or the granule under the content uniformity item got in the preparation of need testing solution, accurate claims surely, and the accurate methanol that adds claims decide weight, and supersound extraction is put coldly, adds methanol and supplies weight, shakes up, and gets the supernatant filtration, promptly;

Accurate respectively reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly;

In this preparation, tablet contains Fructus Gardeniae in jasminoidin C17H24O10, must not be less than the 0.25mg/ sheet; Granule contains Fructus Gardeniae for every bag must not be less than 1.0mg in jasminoidin C17H24O10.

15. the method for quality control according to the described defatting and poison expelling oral formulations of claim 14 is characterized in that: described method of quality control comprises:

Character: for tablet, product is a Film coated tablets, is pale brown color to sepia after removing film-coat; Bitter in the mouth;

For granule, product is that pale brown color is to brown granular; It is sweet to distinguish the flavor of;

Differentiate: (1) gets 2～8 in tablet or granule 2～8g, and is fine ground, adds methanol 10～40ml, close plug soaked 0.5～2 hour, filtered, get filtrate 2～8ml, evaporate to dryness, residue add water 5～20ml makes dissolving, add hydrochloric acid 0.5～2ml again, reflux 15～60 minutes, cooling immediately, divide 2 joltings to extract with ether, each 10～40ml merges ether solution, evaporate to dryness, residue add chloroform 0.5～3ml dissolving, as need testing solution; Other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, shines medical material solution in pairs with legal system; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw need testing solution 10 μ l, control medicinal material solution 5 μ l, put respectively in same be on the silica gel H lamellae of adhesive with the sodium carboxymethyl cellulose, upper solution with 30～60 ℃ petroleum ether-formic acid second fat-formic acid=5-25: 1-10: 0.1-2 is developing solvent, launches, and takes out, dry, put under the 365nm ultraviolet light and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence principal spot of same color;

(2) get 2～8 in tablet or granule 2～8g, pulverize, the 10～40ml that adds diethyl ether, reflux 0.5～2 hour filters, and filtrate volatilizes, and residue adds ethanol 0.5～5ml makes dissolving, as need testing solution; Other gets the ursolic acid reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw need testing solution 5 μ l, reference substance solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether-benzene-glacial acetic acid-ethyl acetate=5-15: 10-30: 0.1-1: 1-10 is developing solvent, launches, and takes out, dry, spray is with 10% sulphuric acid ethanol liquid, and it is clear to be heated to the speckle colour developing at 90～120 ℃, puts under the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical fluorescence speckle;

(3) get 2～8 in tablet or granule 2～8g, porphyrize, the 5～30ml that adds diethyl ether, jolting 5～20 minutes, discard ether solution, residue volatilizes, and adds ethyl acetate 5～30ml, reflux 0.5～2 hour, filter, filtrate volatilizes, and residue adds ethanol 0.5～2ml makes dissolving, as need testing solution; Other gets the jasminoidin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw each 2 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ethyl acetate-acetone-formic acid-water=5-15: 1-12: 0.5-5: 0.1-1 is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 110 ℃, inspects under the daylight; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;

(4) get 10～40 in tablet or granule 10～50g, porphyrize, add water 20～60ml, it is 12～13 that the sodium hydroxide with 15% is transferred PH, adds ether 20～60ml and saturated aqueous common salt 2～6ml and fully vibrates, divide and get ether layer, water layer repeats once according to last method again, and combined ether layer volatilizes, residue adds ethyl acetate 0.2～2ml makes dissolving, as need testing solution; Other gets Rhizoma Alismatis control medicinal material 1～3g, adds water 20～90ml, boils 15～60min, filters, and filtrate is concentrated into about 30ml, and it is 12～13 that the sodium hydroxide with 15% is transferred PH, adds diethyl ether and saturated aqueous common salt, shines medical material solution in pairs with legal system; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, drawing each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with toluene-ethyl acetate-formic acid=5-15: 0.5-5: 0.1-0.8, room temperature condition launches down, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear that hot blast blows to the speckle colour developing, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;

Check: should meet relevant every regulation under Chinese Pharmacopoeia appendix tablet of version in 2005 or the granule item;

Assay: jasminoidin shines an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring:

Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water=15-40: 50-100 is a mobile phase; The detection wavelength is 240nm; Number of theoretical plate must not calculate with the jasminoidin peak and is lower than 4000;

The preparation precision of reference substance solution takes by weighing the jasminoidin reference substance, adds methanol and makes the solution that every 1ml contains jasminoidin 60.0 μ g, shakes up, promptly;

Tablet or the granule 0.5-2g under the content uniformity item got in the preparation of need testing solution, the accurate title, decide, precision adds methanol 10-50ml, claim to decide weight, supersound extraction was put cold after 20～60 minutes under power 250W, frequency 50kHZ condition, add methanol and supply weight, shake up, get supernatant and filter, promptly with being less than or equal to 0.45 μ m microporous filter membrane;

Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly;

In this preparation, tablet contains Fructus Gardeniae in jasminoidin C17H24010, must not be less than the 0.25mg/ sheet; Granule contains Fructus Gardeniae for every bag must not be less than 1.0mg in jasminoidin C17H24O10.