CN1768854A

CN1768854A - Chinese medicinal capsule with spleen-supplementing, intestine-benefiting function

Info

Publication number: CN1768854A
Application number: CN 200510114587
Authority: CN
Inventors: 谭沛; 韩正洲; 刘志刚; 何健; 冉繁荣; 赵枫林
Original assignee: SANJIU PHARMACEUTICAL CO Ltd
Current assignee: China Resources Sanjiu Medical and Pharmaceutical Co Ltd
Priority date: 2005-10-26
Filing date: 2005-10-26
Publication date: 2006-05-10
Anticipated expiration: 2025-10-26
Also published as: CN1768854B

Abstract

The invention discloses a Chinese medicinal capsule with spleen-supplementing, intestine-benefiting functions, and the quality controlling method of the preparation, wherein the premix dissoluble portion of the raw material herbs includes astragalus root, pilose asiabell root, amomum fruit, root of herbaceous peony, Chinese angelica root, white atractylodes rhizome and Cinnamomum cassia, and the intestine dissoluble portion comprises corydalis tuber, lychee seed, dried ginger, licorice root, ledebouriella root, banksia rose, psoralea fruit and red halloysite.

Description

A kind of Chinese medicinal capsule preparation with functions of reinforcing spleen and benefiting intestine

Technical field

The present invention relates to a kind of Chinese medicinal capsule preparation, particularly relate to a kind of Chinese medicinal capsule preparation with functions of reinforcing spleen and benefiting intestine.

Background technology

Chronic non-specific ulcerative colitis is comparatively common clinically, the easily colonic mucosa of outbreak and the chronic inflammation enteropathy of Submucosa repeatedly, with lower abdominal pain, diarrhoea or defecate thin, mucus to be arranged or have blood in stool etc. be clinical characters; Because the course of disease is long, outbreak repeatedly is difficult to cure, and the possibility of potential malignant change is arranged, and therefore, the patient is very painful.Owing to be a kind of agnogenic autoimmune disease, therefore still there are not good Therapeutic Method and medicine both at home and abroad.

The doctor trained in Western medicine choice drug is adrenocortical hormone and thyroliberin, and the person of failing to respond to any medical treatment can add with azathioprine or Ismipur, and be no less than 3 months the course of treatment, generally should continue half a year to 2 year.Also can use treatments such as antibacterials prontosil pyridine, bactrim, neomycin, norfloxacin.Adopt the medicine retention enema can obtain certain effect, sleep every night preceding 1 time, 2-3 week is a course of treatment.Theory of Chinese medical science thinks that primary disease belongs to the category of " diarrhea due to hypofunction of the spleen ", adopts the method treatment of invigorating the spleen to arrest diarrhea can obtain certain therapeutic effect.The end of the seventies, the beginning of the eighties, domestic middle medical circles have just begun the clinical research at chronic non-specific ulcerative colitis, adopt the decoction for the treatment colitis of invigorating the spleen and benefiting QI to obtain effect preferably.According to the external treatment with Chinese medicine theory, adopt the medicine of convergence, relieving diarrhea with astringents to carry out colon clysis to control its mark subsequently, oral invigorating the spleen and benefiting QI Chinese medicine is with Zhi Qiben simultaneously, and inside and outside treating both the principal and the secondary aspects of a disease at the same time obtains promising result.But clysmata must just can be carried out in hospital, the several hrs of at every turn need on operating-table, lying on one's side, abdominal distention unbearably, the life-time service patient is difficult to accept.

Summary of the invention

Purpose of the present invention is to provide a kind of Chinese medicinal capsule preparation with functions of reinforcing spleen and benefiting intestine; Another object of the present invention is to provide a kind of preparation method with Chinese medicinal capsule agent of functions of reinforcing spleen and benefiting intestine, and the object of the invention also is to provide the method for quality control of this capsule preparations.

Technical scheme

Chinese medicinal capsule preparation with functions of reinforcing spleen and benefiting intestine of the present invention is made up of following raw material medicaments, proportioning following (by weight):

The said preparation crude drug divides two partly to form, wherein

The gastric solubleness part:

Radix Astragali 150-250 weight portion Radix Codonopsis (rice is fried) 100-200 weight portion

Fructus Amomi 40-80 weight portion Radix Paeoniae Alba 250-400 weight portion

Radix Angelicae Sinensis (parching with earth) the 30-70 weight portion Rhizoma Atractylodis Macrocephalae (parching with earth) 70-140 weight portion

Cortex Cinnamomi 20-40 weight portion.

The molten part of colon:

Rhizoma Corydalis (system) 70-140 weight portion Semen Litchi 70-140 weight portion

Rhizoma Zingiberis (big gun) 40-90 weight portion Radix Glycyrrhizae (processing) 70-140 weight portion

Radix Saposhnikoviae 70-140 weight portion Radix Aucklandiae 70-140 weight portion

Fructus Psoraleae (processed with salt) 70-140 weight portion Halloysitum Rubrum (forging) 250-350 weight portion

Gastric solubleness part, the molten part of colon prepare respectively, and wherein the capsule quantity partly made of gastric solubleness is 2 times of the molten part capsule of colon quantity.

Method for making:

Above gastric solubleness part seven flavors are got Fructus Amomi, Cortex Cinnamomi powder is broken into fine powder, sieves mixing; The five tastes such as all the other Radixs Astragali add water 8-12 doubly to be measured, and soaks after 20-40 minute, decocts 2-3 time, each 1-3 hour, collecting decoction filtered, filtrate decompression concentrates (below 60 ℃) to about 1.10 (60 ℃) of relative density, and room temperature to be chilled to adds ethanol and makes and contain the alcohol amount and be 50-70%, stir evenly, after leaving standstill, get supernatant and reclaim ethanol, concentrating under reduced pressure (below 60 ℃) to relative density is about 1.20 (60 ℃), vacuum drying (below 60 ℃) becomes dry extract, pulverizes; With above-mentioned Fructus Amomi, Cortex Cinnamomi fine powder mixing, to granulate, the Capsules of packing into is made gastric-dissolved capsule.

Molten part eight flavors of above colon are got Halloysitum Rubrum 4/5 amount, add water 8-12 and doubly measure, and decoct 1-2 hour, staticly settle, and get supernatant, and are standby; Remaining Halloysitum Rubrum is ground into fine powder, and is standby.Seven flavors such as all the other Rhizoma Corydalis add water 11-15 doubly to measure, and soak after 20-40 minute, decoct 2-4 time, each 1-2 hour, collecting decoction, filter, filtrate decompression concentrates (below 60 ℃) to about 1.10 (60 ℃) of relative density, room temperature to be chilled to, add ethanol and make the alcohol amount of containing be 50-70%, stir evenly, leave standstill, the supernatant of getting supernatant and above-mentioned Halloysitum Rubrum merges, and reclaims ethanol, and concentrating under reduced pressure (below 60 ℃) to relative density is about 1.20 (60 ℃), vacuum drying (below 60 ℃) becomes dry extract, pulverizes; With Halloysitum Rubrum powder mixing, to granulate, the colon soluble and intestine soluble hollow capsule of packing into is made the colon soluble and intestine soluble capsule.

Method of quality control of the present invention comprises following discriminating and/or content assaying method.

Discrimination method comprises to the discriminating of gastric-dissolved capsule with to the discriminating of the molten part enteric coated capsule of colon content:

Wherein the discrimination method of gastric-dissolved capsule comprises one or more in the following method:

A. the Radix Astragali: get gastric-dissolved capsule content 3g, porphyrize adds n-butyl alcohol 30ml, put in the water-bath reflux 2 hours, and filtered, filtrate is put in the separatory funnel, add 1% sodium hydroxide solution jolting, wash 3 times, each 15ml, discard alkali liquor, the reuse n-butyl alcohol is saturated is washed to neutrality, discards water layer, n-butyl alcohol liquid evaporate to dryness in water-bath, residue adds methanol 1ml makes dissolving, as need testing solution.Get Radix Astragali control medicinal material fine powder 3g,, make the medical material contrast solution according to the preparation method of need testing solution.Other gets the astragaloside reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.According to thin layer chromatography (" 2005 editions one appendix VI B of Chinese pharmacopoeia) test, draw need testing solution, medical material contrast solution, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with 12-15: 6-8: lower floor's solution that 1-3 chloroform-methanol-water is placed below 10 ℃ is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph, daylight shows down identical sepia speckle, the 365nm ultra-violet lamp shows identical orange-yellow fluorescence speckle down.

B. the Radix Paeoniae Alba: get gastric-dissolved capsule content 2g, porphyrize adds ethanol 10ml, and jolting 5 minutes filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution.Get Radix Paeoniae Alba control medicinal material fine powder 1g,, make the medical material contrast solution according to the preparation method of need testing solution.Other gets the peoniflorin reference substance, adds ethanol and makes every 1ml and contain 1mg solution, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with 35-45: 3-7: 8-12: 0.1-0.4 chloroform-ethyl acetate-methanol-formic acid is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing.In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show identical bluish violet speckle

C. Cortex Cinnamomi: get gastric-dissolved capsule content 1.5g, add ethanol 10ml, close plug, merceration 20 minutes, jolting constantly filters, and filtrate is as need testing solution.Get Cortex Cinnamomi control medicinal material fine powder 0.5g,, make control medicinal material solution according to the preparation method of need testing solution.Other gets the cinnamic aldehyde reference substance, adds ethanol and makes the reference substance solution that every 1ml contains 1 μ l.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 5 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with 15-19: 2-4 petroleum ether (60～90 ℃)-ethyl acetate is developing solvent, launch, take out, dry, spray is with dinitrophenylhydrazine ethanol test solution.In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph, show the speckle of same color;

D. Fructus Amomi: get gastric-dissolved capsule content 2g, porphyrize adds absolute ether 20ml, and merceration spends the night.Filter, filtrate volatilizes naturally, and residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution.Get Fructus Amomi control medicinal material fine powder 0.5g,, make the medical material contrast solution according to the preparation method of need testing solution.Get the bornyl acetate reference substance, add dehydrated alcohol and make the solution that every 1ml contains 10 μ l, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw above-mentioned three kinds of each 5ul of solution, respectively with same silica gel g thin-layer plate on, with 20-24: 1 cyclohexane extraction-ethyl acetate is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing.In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color.

Wherein the molten capsular discrimination method of colon comprises one or more in the following method:

E. Rhizoma Corydalis: get colon soluble and intestine soluble capsule 's content 4g, porphyrize adds ammonia solution 30ml dissolving, puts in the separatory funnel, and the 50ml jolting that adds diethyl ether is extracted, and divides and gets ether layer, reclaims solvent, and residue adds methanol 1ml makes dissolving, as need testing solution.Get Rhizoma Corydalis control medicinal material fine powder 1g, the saturated ether 30ml of ammonification soaked overnight filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.Get the tetrahydropalmatine reference substance, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 3 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with 6-8: 3-5: it is developing solvent that 1 normal hexane-chloroform-methanol adds 1 strong ammonia solution, launch, take out, dry, smoked clear with iodine vapor to the speckle colour developing.Inspect under the daylight, in the test sample chromatograph, with reference substance, the corresponding position of control medicinal material chromatograph on, show the speckle of same color; After in air, waving the iodine that adsorbs on the most plate, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with reference substance, the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.

F. Fructus Psoraleae: get colon soluble and intestine soluble capsule 's content 1g, add water 20ml dissolving, aqueous solution adds ethyl acetate 30ml extraction, divides and gets ethyl acetate liquid evaporate to dryness, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Get Fructus Psoraleae control medicinal material fine powder 0.5g, add ethyl acetate 20ml, ultrasonic 30 minutes, filter, filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as the medical material contrast solution.Get psoralen, isopsoralen reference substance, add ethyl acetate and make the mixed solution that every 1ml contains 2mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 4 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, with 3-5: 1-2 normal hexane-ethyl acetate is developing solvent, launch, take out, dry, spray is put under the ultra-violet lamp (365nm) and is inspected with 10% potassium hydroxide methanol solution.In the test sample chromatograph, with reference substance, the corresponding position of control medicinal material chromatograph on, show two identical fluorescence speckles.

G. Radix Glycyrrhizae: get colon soluble and intestine soluble capsule 's content 5g, porphyrize adds chloroform 40ml, supersound process 15-30 minute, filter, discard filtrate, filtering residue adds methanol 50ml, supersound process 15-30 minute, filters, filtrate is concentrated into about 5ml, is added on the neutral alumina post (100～200 orders, the 15g that have handled well, on the internal diameter 10～15mm),, collect eluent with 40% methanol 150ml eluting, evaporate to dryness, residue adds water 30ml makes dissolving, with water saturated n-butanol extraction 2-3 time, and each 25ml, merge n-butyl alcohol liquid, with ammonia scrubbing 2-4 time, each 20ml, n-butyl alcohol liquid is put evaporate to dryness in the water-bath, residue adds the 1ml dissolve with methanol, as need testing solution.Extracting liquorice control medicinal material fine powder 2g according to the preparation method of need testing solution, makes control medicinal material solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw above-mentioned two kinds of each 8ul of solution, put respectively on same silica gel g thin-layer plate, with 13-17: 38-45: 20-25: lower floor's solution that 8-12 chloroform-ethyl acetate-methanol-water is placed below 10 ℃ is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃.Inspect under the daylight, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color; Put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.

H. the thin layer chromatography identification experiment of Radix Saposhnikoviae: get colon soluble and intestine soluble capsule 's content 1g, porphyrize adds acetone 20ml, and supersound process 15-25 minute, filter, filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution.Get Radix Saposhnikoviae control medicinal material fine powder 1g,, make control medicinal material solution according to the preparation method of need testing solution.According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 15 μ l of above-mentioned solution, put in same silica gel G F respectively ₂₅₄On the lamellae, with 7-9: 1 chloroform-methanol is developing solvent, launches, and takes out, and dries, and puts under the uviol lamp (254nm) and inspects.In the test sample chromatograph, with the corresponding position of control medicinal material on, show the speckle of same color.

Content assaying method comprises to be measured and to the molten part psoralen of colon assay the content of paeoniflorin of gastric-dissolved capsule:

Content of paeoniflorin is surveyed:

The selection of chromatographic column: adopt the octadecylsilane chemically bonded silica chromatographic column.

The selection of mobile phase: the ratio of acetonitrile-water is 15-19: 75-88

The detection wavelength is 230nm, flow velocity 1.0ml/min.

Number of theoretical plate calculates by the peoniflorin peak should be not less than 1500.

The preparation of need testing solution: get gastric-dissolved capsule content 0.3g, the accurate title, decide, and puts in the 25ml measuring bottle, add the about 20ml of methanol, supersound process, power, 150-300W, frequency, 40-70KHz, 20-40 minute, put coldly, add methanol to scale, shake up, leave standstill, get supernatant, filter with microporous filter membrane (0.45 μ m), get filtrate, promptly.

The assay of psoralen

Instrument and reagent:

Chromatographic column: octadecyl silane chromatographic column; The methanol of mobile phase: 45-55: 45-55-1% glacial acetic acid or methanol-acetonitrile-water or methanol-water; The detection wavelength is 245nm; Flow velocity 0.8ml/min; Column temperature 25-40 ℃.Number of theoretical plate calculates by the psoralen peak should be not less than 2000.

The preparation of need testing solution: get colon soluble and intestine soluble capsule 's content 0.4g, put in the 25ml measuring bottle, add the about 20ml of methanol, supersound process power, 150-300W, frequency, 40-70KHz 20-40 minute, is put cold, add methanol to scale, shake up, leave standstill, get supernatant, filter with microporous filter membrane (0.45 μ m), get filtrate, promptly.

Beneficial effect

Preparation of the present invention has great pharmacological effects and therapeutic effect, taking dose is little simultaneously, quality stability is good, the discriminating medical material of selecting and as the composition of assay, can reach effective control to the quality of product, and, make method precision, sensitivity, stability all higher by to each method screening.We make branch colloidal sol capsule preparation with gastric solubleness and the molten part of colon, and layer segment has promoted effective ingredient the absorbing of specific part in colonic location dissolving in can making, and gives full play to the advantage of traditional Chinese medical science treating both the principal and secondary aspects of a disease, obviously improves the curative effect of medicine.The tradition pill, have some inevitable shortcomings: wayward as each position dissolving of gastrointestinal, local curative effect is undesirable, taking dose big (once taking 6g) and make the patient be difficult to swallow, the medicated powder of making a living entirely is used as medicine and makes health examination very difficult up to specification, molten in vivo diffusing absorption slowly and bioavailability is low, dissolve scattered time limit is difficult for reaching shortcomings such as requirement.

Following experiment and embodiment are used to further specify but are not limited to the present invention.

Experimental example 1 reinforcing spleen and benefiting intestine capsule is to the influence of 2,4 dinitrochlorobenzene type colitis

After rat modeling success, press 20ml/kg, the qd gastric infusion, continuous 14 days, normal group and model control group gavaged the distilled water of equivalent.12 hours eye socket veins are got blood behind the last medicine, by content and myeloperoxidase (MPO) (MPO) activity of biotinylation kit requirement with 721 spectrophotometric determination serum lactate dehydrogenase (SLD)s (LDH), serum amylase (AMS).Put to death rat then and get colon (anus is to ileocecus), observe general form and change, press the scoring of table 1 standard.Get colon 5cm long (apart from anus 3cm) simultaneously and claim weight in wet base, 10% formaldehyde fixed, the routine paraffin wax embedding, HE dyeing tissues observed form changes, and presses the scoring of table 2 standard.

Table 1 general form damage standards of grading

	The general form performance	Scoring
	The general form performance	Scoring	Adhesion ulcer and inflammation	Do not have slight (colon and its hetero-organization are peeled off transaction) severe and do not have contrafluxion; NIP 1 place's ulcer is not accompanied hyperemia or ulcer companion inflammation (hyperemia or intestines wall thickening)＞2 place's ulcer and/or inflammation＞1cm ulcer and/or the inflammation＞2cm of ulcer companion inflammation (hyperemia or intestines wall thickening)＞2 place of intestines wall thickening 1 place; The every increase of extent of disease 1cm, score adds 1	0 1 2 0 1 2 3 4 5 6～8

Table 2 Histological injury standards of grading

	Histology's performance	Scoring
	Histology's performance	Scoring	Ulcer	Big ulcer＞the 3mm of no aphtha＜3mm	0 1 2
Inflammation	There is not slight (inflammatory cell infiltration is few, goblet cell reduce light) severe (inflammatory cell infiltration is many, goblet cell reduce obvious)	0 1 2	Ulcer	Big ulcer＞the 3mm of no aphtha＜3mm	0 1 2
Inflammation		0 1 2	Granuloma	Nothing has	0 1
The pathological changes degree of depth	No tela submucosa flesh layer placenta percreta	0 1 2 3	Granuloma	Nothing has	0 1
The pathological changes degree of depth	No tela submucosa flesh layer placenta percreta	0 1 2 3	Fibrosis	There is not slight severe	0 1 2

Table 3 pair 2,4 dinitrochlorobenzene type colitis rats

The influence of colon general form, Histological injury (n=10 x ± SD)

Group	Dosage (g/kg)	The anatomical lesion score	Histological injury's score
Group	Dosage (g/kg)	The anatomical lesion score	Histological injury's score	Normal group model+distilled water model+reinforcing spleen and benefiting intestine capsule model+reinforcing spleen and benefiting intestine capsule model+reinforcing spleen and benefiting intestine capsule model+pill for strengthening spleen and intestines model+SASP	- - 6.60 3.30 1.65 3.30 0.55	0±0 6.60±0.97## 3.00±0.97 2.90±1.07 4.90±1.20 4.00±1.25 3.30±1.34**	0.30±0.48 8.10±1.10## 1.90±1.66 2.40±2.07 4.60±1.71 4.80±1.93 3.60±1.35**

# refers to P and normal group relatively; * refer to that P and model group are relatively;

# or * P＜0.05; ## or * * P＜0.01, down together

Table 4 pair 2,4 dinitrochlorobenzene type colitis

The influence of rat blood serum biochemical indicator (n=10 x ± SD)

Group	Dosage (g/kg)	MPO(U/L)	LDH (u/dl)	AMS(u/dL)
Group	Dosage (g/kg)	MPO(U/L)	LDH (u/dl)	AMS(u/dL)	Normal group model+distilled water model+reinforcing spleen and benefiting intestine capsule model+reinforcing spleen and benefiting intestine capsule model+reinforcing spleen and benefiting intestine capsule model+pill for strengthening spleen and intestines model+SASP	- - 6.60 3.30 1.65 3.30 0.55	43.85±3.38 57.91±8.75## 39.43±3.58 40.98±5.01 52.90±5.01 47.49±4.97 43.56±4.89	4243.20±1705.31 11840.80±3869.17## 2750.60±1347.21 3780.40±1245.69 5167.40±2055.52 5050.80±1413.70 4160.20±1347.28**	766.90±7.09 720.60±22.74## 765.20±7.11 763.50±7.82 763.30±9.42 756.40±7.75 764.80±8.48**

Table 5 pair 2,4 dinitrochlorobenzene type colitis

The influence of rat body weight and colon weight (n=10 x ± SD)

Group	Dosage (g/kg)	Colon weight in wet base (g)	Administration forebody-afterbody method of double differences value (g)
Group	Dosage (g/kg)	Colon weight in wet base (g)		Normal group model+distilled water model+reinforcing spleen and benefiting intestine capsule model+reinforcing spleen and benefiting intestine capsule model+reinforcing spleen and benefiting intestine capsule model+pill for strengthening spleen and intestines model+SASP	- - 6.60 3.30 1.65 3.30 0.55	0.493±0.042 1.423±0.449## 0.796±0.168 0.824±0.198 1.076±0.796 1.018±0.305 0.981±0.196	↑42.60±17.68 ↓8.60±2.95## ↓4.40±1.71** ↓5.00±1.64* ↓5.80±2.10 ↓6.70±2.83* ↓5.80±2.20**

↑ to represent to increase, ↓ expression reduces, down together

The result shows (table 3, table 4, table 5): the reinforcing spleen and benefiting intestine capsule of high, medium and low dosage all can significantly reduce 2, general form, Histological injury's degree of 4 dinitrochlorobenzene type colitis rat colons, alleviate colon weight and reduction Serum LDH content and MPO activity, increase the content of serum AMS, the degree that loses weight when reducing colitis, compare P＜0.05～0.01 with model group, show that the reinforcing spleen and benefiting intestine capsule has certain therapeutical effect to ulcerative colitis.This effect is better than the Spleen Invigorating and Intestine Tonifying Pill group and the sulfasalazine group of dose,equivalent, P＜0.01.

Experimental example 2 reinforcing spleen and benefiting intestine capsules are to the influence of acetic acid type colitis

After rat modeling success, press 20ml/kg, the qd gastric infusion, continuous 14 days, normal group and model control group gavaged the distilled water of equivalent.12 hours execution rats are got colon (anus is to ileocecus) behind the last medicine, the observation general form changes, get colon 5cm long (apart from anus 3cm) simultaneously and claim weight in wet base, 10% formaldehyde fixed, the routine paraffin wax embedding, HE dyeing tissues observed form changes, and presses table 1, table 2 criterion calculation colitis general form and tissue morphology degree of injury.

Table 6 pair acetic acid type colitis rat

The influence of colon general form, Histological injury (n=10 x ± SD)

Group	Dosage (g/kg)	The anatomical lesion score	Histological injury's score
Group	Dosage (g/kg)	The anatomical lesion score	Histological injury's score	Normal group model+distilled water model+reinforcing spleen and benefiting intestine capsule model+reinforcing spleen and benefiting intestine capsule model+reinforcing spleen and benefiting intestine capsule model+pill for strengthening spleen and intestines model+SASP	- - 6.60 3.30 1.65 3.30 0.55	0.00±0.00 5.30±1.06## 2.30±1.25 2.80±1.32 3.30±1.77** 3.70±2.11* 3.70±1.64*	0.10±0.32 8.10±0.57## 2.60±1.26 3.30±0.67 4.20±1.55 4.60±1.51 3.80±1.48**

The influence of table 7 pair acetic acid type colitis rat body weight and colon weight (n=10 x ± SD)

Group	Dosage (g/kg)	Colon weight in wet base (g)	Administration forebody-afterbody method of double differences value (g)
Group	Dosage (g/kg)	Colon weight in wet base (g)		Normal group model+distilled water model+reinforcing spleen and benefiting intestine capsule model+reinforcing spleen and benefiting intestine capsule model+reinforcing spleen and benefiting intestine capsule model+pill for strengthening spleen and intestines model+SASP	- - 6.60 3.30 1.65 3.30 0.55	0.643±0.124 1.066±0.172## 0.837±0.099** 0.876±0.145* 0.855±0.200* 0.865±0.144* 0.815±0.144**	↑36.10±11.45 ↓7.50±1.90## ↓3.00±1.33** ↓4.20±1.75* ↓6.30±2.11 ↓5.60±1.07 ↓5.20±1.40

The result shows (table 6, table 7): the reinforcing spleen and benefiting intestine capsule of high, medium and low dosage can reduce significantly all that acetic acid type colitis rat body weight alleviates and the degree of the general form of colon, tissue morphology damage, and significantly alleviate colon weight, compare P＜0.05～0.01 with model group, show that the reinforcing spleen and benefiting intestine capsule has certain therapeutical effect to ulcerative colitis.This effect is better than the Spleen Invigorating and Intestine Tonifying Pill group and the sulfasalazine group of dose,equivalent, P＜0.05.

Experimental example 3 reinforcing spleen and benefiting intestine capsules are to the influence of capillary permeability

After the mice random packet, press 20ml/kg, the qd gastric infusion, continuous 4 days, matched group gavaged the distilled water of equivalent.Behind the last medicine 1 hour by the capillary permeability laboratory method, the quantitative 0.5% azovan blue normal saline of intravenous injection, the quantitative acetic acid of while lumbar injection, put to death mice behind the 15min, open the abdominal cavity, with the normal saline flushing abdominal cavity and collect flushing liquor, with the content of 721 spectrophotometric determination mouse peritoneal eluate (10ml) azovan blue.

The influence of table 8 pair capillary permeability (n=11, x ± SD)

Group	Dosage (g/kg)	The seepage discharge of azovan blue (OD value)
Group	Dosage (g/kg)	The seepage discharge of azovan blue (OD value)	Distilled water reinforcing spleen and benefiting intestine capsule reinforcing spleen and benefiting intestine capsule reinforcing spleen and benefiting intestine capsule Spleen Invigorating and Intestine Tonifying Pill indometacin	- 9.60 4.80 2.40 4.80 0.02	0.208±0.123 0.077±0.032## 0.088±0.061 ^## 0.095±0.061# 0.091±0.045## 0.028±0.011##

The result shows (table 8): the seepage discharge of azovan blue when the reinforcing spleen and benefiting intestine capsule of high, medium and low dosage all can significantly reduce acetic acid and causes the mouse peritoneal capillary permeability and increase, compare with matched group, P＜0.05～0.01, show that the reinforcing spleen and benefiting intestine capsule can reduce the permeability of blood capillary, has certain antiinflammatory action.This effect does not relatively have significant difference, P＞0.05 with Spleen Invigorating and Intestine Tonifying Pill.

Experimental example 4 reinforcing spleen and benefiting intestine capsule xylol cause the influence of mouse ear inflammatory reaction

With mice group and administration, with experimental example 1, dripped equivalent caused by dimethylbenzene xylene inflammation by the mice ear method to each group mice left side ear in 1 hour behind the last medicine, take off cervical vertebra in 15 minutes and put to death mice, along auricle baseline clip two ears, and lay auricle with card punch in same position, and weigh, be inflammation swelling degree with two ear weight differences.

Table 9 xylol causes influence (n=11, the x ± SD) of mouse ear inflammatory reaction

Group	Dosage (g/kg)	Ear inflammation swelling degree difference (mg)
Group	Dosage (g/kg)	Ear inflammation swelling degree difference (mg)	Distilled water reinforcing spleen and benefiting intestine capsule reinforcing spleen and benefiting intestine capsule reinforcing spleen and benefiting intestine capsule Spleen Invigorating and Intestine Tonifying Pill indometacin	- 9.60 4.80 2.40 4.80 0.02	3.70±2.06 1.70±0.78## 2.18±1.25# 2.66±2.02 3.00±1.98 1.04±0.35##

The result shows (table 9): high dose and middle dosage reinforcing spleen and benefiting intestine capsule can significantly alleviate the swelling degree of mice caused by dimethylbenzene xylene ear inflammatory reaction, compare P＜0.05 with matched group, show that the reinforcing spleen and benefiting intestine capsule has certain antiinflammatory action.This effect does not relatively have significant difference, P＞0.05 with Spleen Invigorating and Intestine Tonifying Pill.

Experimental example 5 reinforcing spleen and benefiting intestine capsules are to the influence of gastrointestinal function

1, to the influence of mouse small intestine charcoal end propelling rate

The mice medication is with experimental example 1, allow by small intestinal charcoal end propulsion trial method behind the last medicine and respectively organized the mice fasting 24 hours, gavage the medicinal liquid 20ml/kg that contains 5% carbon powder then, put to death mice after 15 minutes, press small intestinal carbon powder propulsion trial method and calculate mouse small intestine carbon powder propelling rate.

The influence of table 10 pair mouse small intestine charcoal end propelling rate (n=12, x ± SD)

Group	Dosage (g/kg)	Small intestinal total length (cm)	Advance length (cm)	Carbon powder propelling rate (%)
Group	Dosage (g/kg)	Small intestinal total length (cm)	Advance length (cm)	Carbon powder propelling rate (%)	Distilled water reinforcing spleen and benefiting intestine capsule reinforcing spleen and benefiting intestine capsule reinforcing spleen and benefiting intestine capsule Spleen Invigorating and Intestine Tonifying Pill atropine	- 9.60 4.80 2.40 4.80 0.48mg	52.50±3.23 52.75±2.99 53.50±2.07 53.33±3.42 52.67±3.65 54.17±3.16	20.92±5.35 17.17±2.52 17.50±3.45 20.50±3.29 18.17±3.69 13.75±1.76	39.71±9.19 34.96±4.83# 32.69±6.22# 38.46±5.84 34.35±5.95 25.53±4.01##

The result shows (table 10): the reinforcing spleen and benefiting intestine capsule of high dose and middle dosage can significantly suppress mouse small intestine carbon powder propelling rate, compares P＜0.05 with matched group, shows that the reinforcing spleen and benefiting intestine capsule has the effect that suppresses the mice gastrointestinal peristalsis.The Spleen Invigorating and Intestine Tonifying Pill of this effect and dose,equivalent does not relatively have significant difference, P＞0.05.

2, to Radix Et Rhizoma Rhei type mice with spleen deficiency defecation time, just and the influence of body weight

Mice is pressed the modeling in continuous 8 days of the insufficiency of the spleen molding of Radix Et Rhizoma Rhei type, and the medicine group is in first day while of modeling gastric infusion, and once a day, continuous 7 days, normal control group and model control group gavaged the distilled water of equivalent.Allow mice fasting 24 hours by charcoal end efflux time and feces color dot algoscopy behind the last medicine, gavage the medicinal liquid 20ml/kg that contains 5% charcoal end then, what each mice of opening entry was arranged row's melena in time and 2 hours of melena first behind the medicine counts (do not have row's melena person in 2 hours, then calculated by 2 hours).

Table 11 pair Radix Et Rhizoma Rhei type mice with spleen deficiency defecation time and influence just (n=13, x ± SD)

Group	Dosage (g/kg)	Defecation rate (%)	Begin to arrange the melena time (min)	Row's melena number (point/2h)
Group	Dosage (g/kg)	Defecation rate (%)	Begin to arrange the melena time (min)	Row's melena number (point/2h)	Normal control group model+distilled water model+reinforcing spleen and benefiting intestine capsule model+reinforcing spleen and benefiting intestine capsule model+reinforcing spleen and benefiting intestine capsule model+Spleen Invigorating and Intestine Tonifying Pill	- - 9.60 4.80 2.40 4.80	31％ 100％## 31.00％ 54.00％ 69.00％* 69.00％*	112.31±11.36 23.92±23.02## 90.54±46.26 79.62±46.54 54.54.00±52.67 59.77±52.48*	0.62±1.04 3.31±1.80## 0.62±1.12 1.31±1.60 1.77±1.74* 2.31±2.06

The influence of table 12 pair Radix Et Rhizoma Rhei type mice with spleen deficiency body weight (n=13, x ± SD)

Group	Dosage (g/kg)	Body weight (g) before the medicine	Body weight behind the medicine (g)	Difference (g)
Group	Dosage (g/kg)	Body weight (g) before the medicine	Body weight behind the medicine (g)	Difference (g)	Normal control group model+distilled water model+reinforcing spleen and benefiting intestine capsule model+reinforcing spleen and benefiting intestine capsule model+reinforcing spleen and benefiting intestine capsule model+Spleen Invigorating and Intestine Tonifying Pill	- - 9.60 4.80 2.40 4.80	20.85±1.63 20.62±1.50 20.69±1.32 20.92±1.38 20.08±1.26 20.46±1.13	23.92±0.95 18.62±1.61 22.69±2.39 22.31±2.14 20.15±1.77 20.38±1.19	↑3.08±1.26 ↓2.00±1.15## ↑2.00±1.41 ↑1.38±1.04 ↑0.08±2.10 ↓0.08±0.86

The result shows (table 11, table 12): but the defecation time of the equal significant prolongation Radix Et Rhizoma Rhei type model of spleen deficiency mice of the reinforcing spleen and benefiting intestine capsule of high, medium and low dosage, the interior row of minimizing 2h melena is counted and is arranged the melena rate, reduce the degree that the model of spleen deficiency mice loses weight, compare P＜0.05～0.01 with model control group.Show that the reinforcing spleen and benefiting intestine capsule has some improvement to Radix Et Rhizoma Rhei type mice with spleen deficiency symptom, this may be relevant with its anti-diarrhea effect.The Spleen Invigorating and Intestine Tonifying Pill of this effect and dose,equivalent does not relatively have significant difference, P＞0.05.

3, to the influence of blood stasis model hemorheology of rat

After the rat random packet, 20ml/kg, the qd gastric infusion, continuous 15 days, normal control group and model control group gavaged the distilled water of equivalent.Pressed depression of liver-QI and cold-condensing type syndrome of blood stasis modelling subcutaneous injection epinephrine on the 13rd day in administration, every day 2 times, and between 2 injections, soak frozen water once, modeling in continuous 2 days.12 hours socket of the eye veins are got blood behind the last medicine, take into account LBY-Nn Trace Blood slurry viscosity instrumentation with the rotary blood viscosity of LBY-N6A type and decide whole blood viscosity (low cut, height cut), whole blood reduced viscosity (low cut, height cut), plasma viscosity, RBC hematocrit, RBC aggregate index, RBC deformation index etc.

The influence of table 13 pair Blood stasis hemorheology of rat (n=10, x ± SD)

Group	Dosage (g/kg)	Whole blood viscosity (low cutting) (mPa.s)	Whole blood viscosity (height is cut) (mPa.s)
Group	Dosage (g/kg)	Whole blood viscosity (low cutting) (mPa.s)	Whole blood viscosity (height is cut) (mPa.s)	Normal group model control group reinforcing spleen and benefiting intestine capsule reinforcing spleen and benefiting intestine capsule reinforcing spleen and benefiting intestine capsule pill for strengthening spleen and intestines Fufang Danshen Pian	- - 6.60 3.30 1.65 3.30 0.55	12.799±4.150 19.375±3.964 ^## 15.396±2.299* 18.053±4.263 16.460±3.966 17.441±3.911 13.757±1.896**	4.913±0.772 6.439±0.699 ^## 5.586±0.708* 6.028±0.841 5.897±0.977 6.016±0.729 5.105±0.531**

The influence of table 14 pair syndrome of blood stasis hemorheology of rat (n=10, x ± SD)

Group	Dosage (g/kg)	Plasma viscosity (mPa.s)	RBC hematocrit (%)
Group	Dosage (g/kg)	Plasma viscosity (mPa.s)	RBC hematocrit (%)	Normal group model control group reinforcing spleen and benefiting intestine capsule reinforcing spleen and benefiting intestine capsule reinforcing spleen and benefiting intestine capsule pill for strengthening spleen and intestines Fufang Danshen Pian	- - 6.60 3.30 1.65 3.30 0.55	1.389±0.104 1.618±0.208 ^## 1.439±0.080* 1.490±0.122 1.424±0.094* 1.596±0.122 1.375±0.061**	45.500±6.587 49.00±3.432 46.800±2.573 48.100±4.202 47.400±3.098 48.900±2.644 47.800±2.658

The influence of table 15 pair syndrome of blood stasis hemorheology of rat (n=10, x ± SD)

Group	Dosage (g/kg)	Whole blood reduced viscosity (low cutting) (mPa.s)	Whole blood reduced viscosity (height is cut) (mPa.s)
Group	Dosage (g/kg)	Whole blood reduced viscosity (low cutting) (mPa.s)	Whole blood reduced viscosity (height is cut) (mPa.s)	Normal group model control group reinforcing spleen and benefiting intestine capsule reinforcing spleen and benefiting intestine capsule reinforcing spleen and benefiting intestine capsule pill for strengthening spleen and intestines Fufang Danshen Pian	- - 6.60 3.30 1.65 3.30 0.55	24.437±5.895 36.010±5.803 ^## 29.964±5.383* 34.085±6.632 31.563±6.587 33.096±5.724 25.870±3.459**	7.712±0.805 9.848±1.029 ^## 8.916±1.689 9.422±1.384 9.426±1.634 9.285±1.097 7.821±1.136**

The influence of table 16 pair syndrome of blood stasis hemorheology of rat (n=10, x ± SD)

Group	Dosage (g/kg)	The RBC aggregate index	The RBC deformation index
Group	Dosage (g/kg)	The RBC aggregate index	The RBC deformation index	Normal group model control group reinforcing spleen and benefiting intestine capsule reinforcing spleen and benefiting intestine capsule reinforcing spleen and benefiting intestine capsule pill for strengthening spleen and intestines Fufang Danshen Pian	- - 6.60 3.30 1.65 3.30 0.55	2.544±0.454 2.987±0.349* 2.755±0.186 2.963±0.365 2.772±0.235 3.112±0.527 2.687±0.179*	0.874±0.090 0.869±0.074 0.894±0.091 0.890±0.072 0.912±0.063 0.890±0.105 0.862±0.068

The result shows (table 13, table 14, table 15, table 16): the reinforcing spleen and benefiting intestine capsule of high dose group can significantly reduce stasis syndrome disease rat whole blood viscosity (low cutting with height cut), whole blood reduced viscosity (low cutting) and plasma viscosity; Low dose group also can reduce plasma viscosity, compares P＜0.05 with model group.Little to RBC hematocrit, deformation index and aggregate index influence, compare P＞0.05 with model group.Prompting: the reinforcing spleen and benefiting intestine capsule has some improvement to the hemorheological property of stasis syndrome disease.Relatively there is not significant difference, P＞0.05 with the Spleen Invigorating and Intestine Tonifying Pill of dose,equivalent.

The experiment of experimental example 6 assays

(1). the paeoniflorin content determination experiment

1, method:

Instrument and reagent:

High performance liquid chromatograph: the P680 of Dai An company pump, PDA-100 diode array detector, ASI-100 automatic sampler

Acetonitrile: chromatographically pure, water: ultra-pure water, other reagent are analytical pure, the peoniflorin reference substance that assay is used is provided by Nat'l Pharmaceutical ﹠ Biological Products Control Institute.

The selection of chromatographic column: adopt the octadecylsilane chemically bonded silica chromatographic column,, can reach the purpose of separation determination through test.Experiment chromatographic column adopting: Dalian Yi Lite ODS-AP 200*4.6mm, 5 μ m;

The selection of mobile phase: acetonitrile-water (17: 83).

The detection wavelength is 230nm, flow velocity 1.0ml/min.

The preparation of need testing solution: get gastric-dissolved capsule content 0.3g, the accurate title, decide, and puts in the 25ml measuring bottle, add the about 20ml of methanol, supersound process (power 200W, frequency 59KHz) 30 minutes, put cold, add methanol to scale, shake up, leave standstill, get supernatant, filter with microporous filter membrane (0.45 μ m), get filtrate, promptly.Every of gastric-dissolved capsule contains the Radix Paeoniae Alba with peoniflorin (C ₂₃H ₂₈O ₁₁) meter, must not be less than 3.00mg

2, method is investigated

The linear preparation precision of investigating reference substance solution takes by weighing 36 hours peoniflorin reference substance 18.5mg of drying in the phosphorus pentoxide vacuum drying apparatus, puts in the 100ml measuring bottle, adds dissolve with methanol and is settled to scale, promptly.

Accurate reference substance solution 4,6,8,16, the 24 μ l that draw of regression equation calculation, inject chromatograph of liquid, measure chromatographic peak area and be respectively 7.8627,15.8282,23.6600,52.6845,81.4952, with the peoniflorin sample size is abscissa, with the chromatographic peak area is vertical coordinate, and the drawing standard curve returns through linearity, get regression equation: Y=19.814X-6.2152, r=0.9999.The result shows: the sample size of peoniflorin is good linear relationship with its peak area in 0.74-4.44 μ g scope.

Stability experiment is got need testing solution, respectively at preparation 0,4,8,12, measures after 24 hours, and peak area is respectively 22.7272,22.8541,23.1243,22.3584,22.2145 RSD=1.46% as a result.Show that sample solution kept stable in 24 hours.

The precision test: get the peoniflorin reference substance solution, repeat sample introduction 5 times, each 10 μ l measure peak area and are respectively 32.2631,32.9048,32.2549,32.5810,32.2941, RSD=0.78%.By The effects such as linearity, stability, precision, illustrate that this content assaying method precision, sensitivity, stability are all higher.

(2) assay of psoralen

1, method:

Instrument and reagent:

Methanol: chromatographically pure, water: ultra-pure water, other reagent are analytical pure, the psoralen reference substance that assay is used is provided by Nat'l Pharmaceutical ﹠ Biological Products Control Institute.

Chromatographic column: octadecyl silane chromatographic column; Mobile phase: methanol-water (50: 50); The detection wavelength is 245nm; Flow velocity 0.8ml/min; 25 ℃ of column temperatures.Number of theoretical plate calculates by the psoralen peak should be not less than 2000.

The selection of mobile phase: methanol-1% glacial acetic acid, methanol-acetonitrile-water, methanol-water all can be used as the flow phase system of assay, chromatographic column adopts reversed-phase column (250*4.6mm more, 5 μ m), detect wavelength and be 245nm, column temperature generally is controlled at 25,35,40 ℃.

The preparation of need testing solution: get the content under the colon soluble and intestine soluble capsule content uniformity item, porphyrize is got 0.4g, the accurate title, decide, and puts in the 25ml measuring bottle, adds the about 20ml of methanol, supersound process (power 200W, frequency 59KHz) 30 minutes is put cold, add methanol to scale, shake up, leave standstill, get supernatant, filter with microporous filter membrane (0.45 μ m), get filtrate, promptly.Every of colon soluble and intestine soluble capsule contains Fructus Psoraleae with psoralen (C ₁₁H ₆O ₃) meter, must not be less than 0.35mg.

2, method is investigated

The linear preparation precision of investigating reference substance solution takes by weighing psoralen reference substance 2.5mg, puts in the 100ml measuring bottle, adds dissolve with methanol, and is fixed molten to scale, promptly.

Accurate psoralen reference substance solution 1,4,8,16, the 24 μ l that draw of the calculating of regression equation, inject chromatograph of liquid, measure chromatographic peak area, peak area is respectively 4.0056,16.6624,35.6612,72.3456,111.5657, with the psoralen sample size is abscissa, is vertical coordinate with the chromatographic peak area, returns through linearity, get regression equation: Y=187.30X-1.5866, r=0.9998.The result shows: the sample size of psoralen is good linear relationship with its peak area in 0.025～0.600 μ g scope.

Stability test is got need testing solution, respectively at preparation 0,4,8,12, measures after 24 hours, and peak area is respectively 28.3669,28.2147,28.6585,27.8294,27.9516, RSD=1.17%.Show that sample solution kept stable in 24 hours.

The psoralen reference substance solution is got in the precision test, repeats sample introduction 5 times, and each 10 μ l measure peak area and are respectively 45.2279,45.4865,46.0248,45.9824,45.1978, RSD=0.78%.By The effects such as linearity, stability, precision, illustrate that this content assaying method precision, sensitivity, stability are all very high.

Following embodiment all can realize the effect of above-mentioned experimental example.

Embodiment 1:Capsule

Place ten thousand

The gastric solubleness part:

Radix Astragali 200g Radix Codonopsis (rice is fried) 150g Fructus Amomi 60g

Radix Paeoniae Alba 300g Radix Angelicae Sinensis (parching with earth) the 50g Rhizoma Atractylodis Macrocephalae (parching with earth) 100g

Cortex Cinnamomi 30g

The molten part of colon:

Rhizoma Corydalis (system) 100g Semen Litchi 100g Rhizoma Zingiberis (big gun) 60g

Radix Glycyrrhizae (processing) 100g Radix Saposhnikoviae 120g Radix Aucklandiae 100g

Fructus Psoraleae (processed with salt) 100g Halloysitum Rubrum (forging) 300g

Method for making

Above gastric solubleness part seven flavors are got Fructus Amomi, Cortex Cinnamomi powder is broken into fine powder, sieves mixing; The five tastes such as all the other Radixs Astragali add 10 times of amounts of water, soak after 30 minutes, decoct secondary, each 2 hours, collecting decoction filtered, filtrate decompression concentrates (below 60 ℃) to about 1.10 (60 ℃) of relative density, and room temperature to be chilled to adds ethanol and makes that to contain the alcohol amount be 60%, stir evenly, after leaving standstill 24 hours, get supernatant and reclaim ethanol, concentrating under reduced pressure (below 60 ℃) to relative density is about 1.20 (60 ℃), vacuum drying (below 60 ℃) becomes dry extract, pulverizes; With above-mentioned Fructus Amomi, Cortex Cinnamomi fine powder mixing, to granulate, the Capsules of packing into is made gastric-dissolved capsule.

Molten part eight flavors of above colon are got Halloysitum Rubrum 4/5 amount, add 10 times of amounts of water, decoct 1 hour, staticly settle, and get supernatant, and are standby; Remaining Halloysitum Rubrum is ground into fine powder, and is standby.Seven flavors such as all the other Rhizoma Corydalis add 13 times of amounts of water, soak after 30 minutes, decoct three times, each 1.5 hours, collecting decoction, filter, filtrate decompression concentrates (below 60 ℃) to about 1.10 (60 ℃) of relative density, room temperature to be chilled to, add ethanol and make that to contain alcohol amount be 60%, stir evenly, left standstill 24 hours, the supernatant of getting supernatant and above-mentioned Halloysitum Rubrum merges, and reclaims ethanol, and concentrating under reduced pressure (below 60 ℃) to relative density is about 1.20 (60 ℃), vacuum drying (below 60 ℃) becomes dry extract, pulverizes; With Halloysitum Rubrum powder mixing, to granulate, the colon soluble and intestine soluble hollow capsule of packing into is made the colon soluble and intestine soluble capsule.

Make 1000 of capsules (wherein gastric solubleness is partly made 667 of gastric-dissolved capsules, and enteric is partly made 333 of colon soluble and intestine soluble capsules).

Usage and dosage: oral, 3 (2 of gastric-dissolved capsules, 1 of colon soluble and intestine soluble capsule) on the one, 3 times on the one; The child is cut down according to the circumstance; Serious symptom dosage or follow the doctor's advice.30 days is a course of treatment, generally serve on 2-3 the course of treatment.

Embodiment 2: capsule

Prescription

The gastric solubleness part:

Radix Astragali 220g Radix Codonopsis (rice is fried) 160g Fructus Amomi 50g

Radix Paeoniae Alba 320g Radix Angelicae Sinensis (parching with earth) the 40g Rhizoma Atractylodis Macrocephalae (parching with earth) 90g

Cortex Cinnamomi 30g

The molten part of colon:

Rhizoma Corydalis (system) 110g Semen Litchi 120g Rhizoma Zingiberis (big gun) 70g

Radix Glycyrrhizae (processing) 110g Radix Saposhnikoviae 100g Radix Aucklandiae 80g

Fructus Psoraleae (processed with salt) 90g Halloysitum Rubrum (forging) 280g

Method for making

Embodiment 3: the capsule discrimination method

Used capsular method for making such as embodiment 1 or 2.

Discrimination method comprises to the discriminating of gastric-dissolved capsule with to the molten part of colon to be differentiated:

Wherein the discrimination method of gastric-dissolved capsule comprises following:

The Radix Astragali: get gastric-dissolved capsule content 3g, porphyrize adds n-butyl alcohol 30ml, put in the water-bath reflux 2 hours, and filtered, filtrate is put in the separatory funnel, add 1% sodium hydroxide solution jolting, wash 3 times, each 15ml, discard alkali liquor, the reuse n-butyl alcohol is saturated is washed to neutrality, discards water layer, n-butyl alcohol liquid evaporate to dryness in water-bath, residue adds methanol 1ml makes dissolving, as need testing solution.Get Radix Astragali control medicinal material fine powder 3g,, make the medical material contrast solution according to the preparation method of need testing solution.Other get in gastric solubleness partly the prescription ratio make the negative control sample 3g that lacks the Radix Astragali, prepare negative control solution according to the preparation method of need testing solution.Other gets the astragaloside reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution, medical material contrast solution, negative control solution each 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, lower floor's solution of placing below 10 ℃ with chloroform-methanol-water (13: 7: 2) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph, daylight shows down identical sepia speckle, ultra-violet lamp (365nm) shows identical orange-yellow fluorescence speckle down.Negative control is noiseless.

The Radix Paeoniae Alba: get gastric-dissolved capsule content 2g, porphyrize adds ethanol 10ml, and jolting 5 minutes filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution.Get Radix Paeoniae Alba control medicinal material fine powder 1g,, make the medical material contrast solution according to the preparation method of need testing solution.Get in gastric solubleness partly the prescription ratio make the negative control sample 2g that lacks the Radix Paeoniae Alba, prepare negative control solution according to the preparation method of need testing solution.Other gets the peoniflorin reference substance, adds ethanol and makes every 1ml and contain 1mg solution, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ l of above-mentioned four kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-formic acid (40: 5: 10: 0.2) be developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing.In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show identical bluish violet speckle

Wherein the molten capsular discrimination method of colon comprises following:

Rhizoma Corydalis: get colon soluble and intestine soluble capsule 's content 4g, porphyrize adds ammonia solution 30ml dissolving, puts in the separatory funnel, and the 50ml jolting that adds diethyl ether is extracted, and divides and gets ether layer, reclaims solvent, and residue adds methanol 1ml makes dissolving, as need testing solution.Get Rhizoma Corydalis control medicinal material fine powder 1g, the saturated ether 30ml of ammonification soaked overnight filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.Other get in enteric partly the prescription ratio make the negative control sample 4g that lacks Rhizoma Corydalis, prepare negative control solution according to the preparation method of need testing solution.Get the tetrahydropalmatine reference substance, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 3 μ l of above-mentioned four kinds of solution, put respectively on same silica gel g thin-layer plate, adding 1 strong ammonia solution with normal hexane-chloroform-methanol (7.5: 4: 1) is developing solvent, launch, take out, dry, smoked clear with iodine vapor to the speckle colour developing.Inspect under the daylight, in the test sample chromatograph, with reference substance, the corresponding position of control medicinal material chromatograph on, show the speckle of same color; After in air, waving the iodine that adsorbs on the most plate, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with reference substance, the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.

Fructus Psoraleae: get colon soluble and intestine soluble capsule 's content 1g, add water 20ml dissolving, aqueous solution adds ethyl acetate 30ml extraction, divides and gets ethyl acetate liquid evaporate to dryness, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Get Fructus Psoraleae control medicinal material fine powder 0.5g, add ethyl acetate 20ml, ultrasonic 30 minutes, filter, filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as the medical material contrast solution.Other get in enteric partly the prescription ratio make the negative control sample 1g that lacks Fructus Psoraleae, prepare negative control solution according to the preparation method of need testing solution.Get psoralen, isopsoralen reference substance, add ethyl acetate and make the mixed solution that every 1ml contains 2mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 4 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate (4: 1) is developing solvent, launch, take out, dry, spray is put under the ultra-violet lamp (365nm) and is inspected with 10% potassium hydroxide methanol solution.In the test sample chromatograph, with reference substance, the corresponding position of control medicinal material chromatograph on, show two identical fluorescence speckles.

Embodiment 4:The capsule content assaying method

Used capsule such as embodiment 1 or 2.

Content of paeoniflorin is surveyed:

Instrument and reagent:

The selection of mobile phase: acetonitrile-water (17: 83).

The detection wavelength is 230nm, flow velocity 1.0ml/min.

The assay of psoralen

Instrument and reagent:

Chromatographic column: octadecylsilane chemically bonded silica chromatographic column; Mobile phase: methanol-water (50: 50); The detection wavelength is 245nm; Flow velocity 0.8ml/min; 25 ℃ of column temperatures.Number of theoretical plate calculates by the psoralen peak should be not less than 2000.

Embodiment 5: the capsule method of quality control

Used capsular method for making such as embodiment 1 or 2.

Wherein the discrimination method of gastric-dissolved capsule comprises following method:

The Radix Astragali: get gastric-dissolved capsule content 3g, porphyrize adds n-butyl alcohol 30ml, put in the water-bath reflux 2 hours, and filtered, filtrate is put in the separatory funnel, add 1% sodium hydroxide solution jolting, wash 3 times, each 15ml, discard alkali liquor, the reuse n-butyl alcohol is saturated is washed to neutrality, discards water layer, n-butyl alcohol liquid evaporate to dryness in water-bath, residue adds methanol 1ml makes dissolving, as need testing solution.Get Radix Astragali control medicinal material fine powder 3g,, make the medical material contrast solution according to the preparation method of need testing solution.Other get in gastric solubleness partly the prescription ratio make the negative control sample 3g that lacks the Radix Astragali, prepare negative control solution according to the preparation method of need testing solution.Other gets the astragaloside reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution, medical material contrast solution, negative control solution each 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, lower floor's solution of placing below 10 ℃ with chloroform-methanol-water (13: 7: 2) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph, daylight shows down identical sepia speckle, ultra-violet lamp (365nm) shows identical orange-yellow fluorescence speckle down ^[4]Negative control is noiseless.

Cortex Cinnamomi: get gastric-dissolved capsule content 1.5g, add ethanol 10ml, close plug, merceration 20 minutes, jolting constantly filters, and filtrate is as need testing solution.Get Cortex Cinnamomi control medicinal material fine powder 0.5g,, make control medicinal material solution according to the preparation method of need testing solution.Get in gastric solubleness partly the prescription ratio make and lack cinnamomic negative control sample 1.5g, prepare negative control solution according to the preparation method of need testing solution.Other gets the cinnamic aldehyde reference substance, adds ethanol and makes the reference substance solution that every 1ml contains 1 μ l.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 5 μ l of above-mentioned four kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (60～90 ℃)-ethyl acetate (17: 3) is developing solvent, launch, take out, dry, spray is with dinitrophenylhydrazine ethanol test solution.In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph, show the speckle of same color;

Fructus Amomi: get gastric-dissolved capsule content 2g, porphyrize adds absolute ether 20ml, and merceration spends the night.Filter, filtrate volatilizes naturally, and residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution.Get Fructus Amomi control medicinal material fine powder 0.5g,, make the medical material contrast solution according to the preparation method of need testing solution.Other get in gastric solubleness partly the prescription ratio make the negative control sample 2g that lacks Fructus Amomi, prepare negative control solution according to the preparation method of need testing solution.Get the bornyl acetate reference substance, add dehydrated alcohol and make the solution that every 1ml contains 10 μ l, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw above-mentioned four kinds of each 5ul of solution, respectively with same silica gel g thin-layer plate on, with cyclohexane extraction-ethyl acetate (22: 1) is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing.In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color.Negative control is noiseless.

Wherein the capsular discrimination method of colon soluble and intestine soluble comprises following:

Fructus Psoraleae: get colon soluble and intestine soluble capsule 's content 1g, add water 20ml dissolving, aqueous solution adds ethyl acetate 30ml extraction, divides and gets ethyl acetate liquid evaporate to dryness, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Get Fructus Psoraleae control medicinal material fine powder 0.5g, add ethyl acetate 20ml, ultrasonic 30 minutes, filter, filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as the medical material contrast solution.Other get in enteric partly the prescription ratio make the negative control sample 1g that lacks Fructus Psoraleae, prepare negative control solution according to the preparation method of need testing solution.Get psoralen, isopsoralen reference substance, add ethyl acetate and make the mixed solution that every 1ml contains 2mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 4 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate (4: 1) is developing solvent, launch, take out, dry, spray is put under the ultra-violet lamp (365nm) and is inspected with 10% potassium hydroxide methanol solution.In the test sample chromatograph, with reference substance, the corresponding position of control medicinal material chromatograph on, show two identical fluorescence speckles ^[12]

Radix Glycyrrhizae: get colon soluble and intestine soluble capsule 's content 5g, porphyrize adds chloroform 40ml, supersound process 20 minutes filters, and discards filtrate, filtering residue adds methanol 50ml, and supersound process 20 minutes filters, filtrate is concentrated into about 5ml, is added on the neutral alumina post (100～200 orders, the 15g that have handled well, on the internal diameter 10～15mm),, collect eluent with 40% methanol 150ml eluting, evaporate to dryness, residue adds water 30ml makes dissolving, with water saturated n-butanol extraction 2 times, and each 25ml, merge n-butyl alcohol liquid, with ammonia scrubbing 3 times, each 20ml, n-butyl alcohol liquid is put evaporate to dryness in the water-bath, residue adds the 1ml dissolve with methanol, as need testing solution.Extracting liquorice control medicinal material fine powder 2g according to the preparation method of need testing solution, makes control medicinal material solution.Other get in enteric partly the prescription ratio make the negative control sample 5g that lacks Radix Glycyrrhizae, prepare negative control solution according to the preparation method of need testing solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw above-mentioned three kinds of each 8ul of solution, put respectively on same silica gel g thin-layer plate, (15: 40: 22: 10) lower floor's solution of placing below 10 ℃ was developing solvent with chloroform-ethyl acetate-methanol-water, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃.Inspect under the daylight, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color; Put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.

Radix Saposhnikoviae: get colon soluble and intestine soluble capsule 's content 1g, porphyrize adds acetone 20ml, and supersound process 20 minutes filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution.Get Radix Saposhnikoviae control medicinal material fine powder 1g,, make control medicinal material solution according to the preparation method of need testing solution.Other get in enteric partly the prescription ratio make the negative control sample 1g that lacks Radix Saposhnikoviae, prepare negative control solution according to the preparation method of need testing solution.According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 15 μ l of above-mentioned three kinds of solution, put in same silica gel G F respectively ₂₅₄On the lamellae, be developing solvent, launch, take out, dry, put under the uviol lamp (254nm) and inspect with chloroform-methanol (8: 1).In the test sample chromatograph, with the corresponding position of control medicinal material on, show the speckle of same color.

Content of paeoniflorin is surveyed:

Instrument and reagent:

The selection of mobile phase: acetonitrile-water (17: 83).

The detection wavelength is 230nm, flow velocity 1.0ml/min.

The assay of psoralen

Instrument and reagent:

Chromatographic column: octadecylsilane bonded chromatographic post; Mobile phase: methanol-water (50: 50); The detection wavelength is 245nm; Flow velocity 0.8ml/min; 25 ℃ of column temperatures.Number of theoretical plate calculates by the psoralen peak should be not less than 2000.

The preparation of need testing solution: get the colon soluble and intestine soluble capsule 's content, porphyrize is got 0.4g, the accurate title, decide, and puts in the 25ml measuring bottle, adds the about 20ml of methanol, supersound process (power 200W, frequency 59KHz) 30 minutes is put cold, add methanol to scale, shake up, leave standstill, get supernatant, filter with microporous filter membrane (0.45 μ m), get filtrate, promptly.Fructus Psoraleae is with psoralen (C ₁₁H ₆O ₃) meter, must not be less than 0.35mg.

Claims

1, a kind of Chinese medicinal capsule preparation with functions of reinforcing spleen and benefiting intestine is characterized in that the said preparation crude drug partly is made up of gastric solubleness part, the molten part two of colon, wherein the gastric solubleness part:

Radix Astragali 150-250 weight portion Radix Codonopsis 100-200 weight portion Fructus Amomi 40-80 weight portion

Radix Paeoniae Alba 250-400 weight portion Radix Angelicae Sinensis 30-70 weight portion Rhizoma Atractylodis Macrocephalae 70-140 weight portion

Cortex Cinnamomi 20-40 weight portion, wherein Radix Codonopsis is that rice is fried, Radix Angelicae Sinensis, the Rhizoma Atractylodis Macrocephalae are parching with earth;

The molten part of colon wherein:

Rhizoma Corydalis (processed) 70-140 weight portion Semen Litchi 70-140 weight portion

Gun ginger 40-90 weight portion Radix Glycyrrhizae Preparata 70-140 weight portion

Processed with salt Fructus Psoraleae 70-140 weight portion Halloysitum Rubrum(calcined) 250-350 weight portion;

Wherein gastric solubleness part, the molten part of colon prepare respectively, and the capsule quantity that gastric solubleness is partly made is 2 times that the molten part of colon is made capsule quantity.

2, Chinese medicinal capsule preparation as claimed in claim 1 is characterized in that the said preparation crude drug is made up of following raw material medicaments:

The gastric solubleness part:

The Radix Astragali 220 weight portion Radix Codonopsis 160 weight portion Fructus Amomis 50 weight portions

The Radix Paeoniae Alba 320 weight portion Radix Angelicae Sinensis 40 weight portion Rhizoma Atractylodis Macrocephalaes 90 weight portions

Cortex Cinnamomi 30 weight portions;

The molten part of colon:

Rhizoma Corydalis 110 weight portion Semen Litchis 120 weight portion Rhizoma Zingiberiss 70 weight portions

The Radix Glycyrrhizae 110 weight portion Radix Saposhnikoviaes 100 weight portion Radix Aucklandiae 80 weight portions

Fructus Psoraleae 90 weight portion Halloysitum Rubrums 280 weight portions.

3, Chinese medicinal capsule preparation as claimed in claim 1 or 2 is characterized in that the said preparation preparation method is: gastric solubleness part seven flavor, get Fructus Amomi, Cortex Cinnamomi powder is broken into fine powder, sieves mixing; The five tastes such as all the other Radixs Astragali add water 8-12 doubly to be measured, and soaks after 20-40 minute, decocts 2-3 time, each 1-3 hour, collecting decoction filtered, filtrate decompression is concentrated into relative density 1.10, and room temperature to be chilled to adds ethanol and makes the alcohol amount of containing be 50-70%, stir evenly, after leaving standstill, get supernatant and reclaim ethanol, being evaporated to relative density is 1.20, vacuum drying becomes dry extract, pulverizes; With above-mentioned Fructus Amomi, Cortex Cinnamomi fine powder mixing, to granulate, the Capsules of packing into is made gastric-dissolved capsule;

Molten part eight flavors of colon are got Halloysitum Rubrum 4/5 amount, add water 8-12 and doubly measure, and decoct 1-2 hour, staticly settle, and get supernatant, and are standby; Remaining Halloysitum Rubrum is ground into fine powder, and is standby; Seven flavors such as all the other Rhizoma Corydalis add water 11-15 doubly to measure, and soak after 20-40 minute, decoct 2-4 time, each 1-2 hour, collecting decoction, filter, filtrate decompression is concentrated into relative density 1.10, room temperature to be chilled to, add ethanol and make the alcohol amount of containing be 50-70%, stir evenly, leave standstill, the supernatant of getting supernatant and above-mentioned Halloysitum Rubrum merges, and reclaims ethanol, is evaporated to relative density 1.20, vacuum drying becomes dry extract, pulverizes; With Halloysitum Rubrum powder mixing, to granulate, the colon soluble and intestine soluble hollow capsule of packing into is made the colon soluble and intestine soluble capsule.

4, Chinese medicinal capsule preparation as claimed in claim 3 is characterized in that the said preparation preparation method is: gastric solubleness part seven flavor, get Fructus Amomi, Cortex Cinnamomi powder is broken into fine powder, sieves mixing; The five tastes such as all the other Radixs Astragali add 10 times of amounts of water, soak after 30 minutes, decoct secondary, each 2 hours, collecting decoction filtered, filtrate is evaporated to 60 ℃ of relative densities below 60 ℃ about 1.10, and room temperature to be chilled to adds ethanol and makes that to contain the alcohol amount be 60%, stir evenly, after leaving standstill 24 hours, get supernatant and reclaim ethanol, being evaporated to relative density below 60 ℃ is 1.20 for about 60 ℃, vacuum drying becomes dry extract below 60 ℃, pulverizes; With above-mentioned Fructus Amomi, Cortex Cinnamomi fine powder mixing, to granulate, the Capsules of packing into is made gastric-dissolved capsule;

Molten part eight flavors of colon are got Halloysitum Rubrum 4/5 amount, add 10 times of amounts of water, decoct 1 hour, staticly settle, and get supernatant, and are standby; Remaining Halloysitum Rubrum is ground into fine powder, and is standby; Seven flavors such as all the other Rhizoma Corydalis add 13 times of amounts of water, soak after 30 minutes, decoct three times, each 1.5 hours, collecting decoction, filtrate is evaporated to 60 ℃ of relative densities below 60 ℃ about 1.10, and room temperature to be chilled to adds ethanol and makes that to contain the alcohol amount be 60%, stir evenly, left standstill 24 hours, the supernatant of getting supernatant and above-mentioned Halloysitum Rubrum merges, reclaim ethanol, being evaporated to 60 ℃ of relative densities below 60 ℃ is that vacuum drying becomes dry extract below 1.20,60 ℃, pulverizes; With Halloysitum Rubrum powder mixing, to granulate, the colon soluble and intestine soluble hollow capsule of packing into is made the colon soluble and intestine soluble capsule.

5, Chinese medicinal capsule preparation as claimed in claim 1 or 2 is characterized in that the discriminating of said preparation comprises following method, and wherein the discriminating of gastric-dissolved capsule comprises one or more in the following method:

A. the Radix Astragali: get gastric-dissolved capsule content 3g, porphyrize adds n-butyl alcohol 30ml, put in the water-bath reflux 2 hours, and filtered, filtrate is put in the separatory funnel, add 1% sodium hydroxide solution jolting, wash 3 times, each 15ml, discard alkali liquor, the reuse n-butyl alcohol is saturated is washed to neutrality, discards water layer, n-butyl alcohol liquid evaporate to dryness in water-bath, residue adds methanol 1ml makes dissolving, as need testing solution; Get Radix Astragali control medicinal material fine powder 3g,, make the medical material contrast solution according to the preparation method of need testing solution; Other gets the astragaloside reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw need testing solution, medical material contrast solution, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with 12-15: 6-8: lower floor's solution that 1-3 chloroform-methanol-water is placed below 10 ℃ is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph, daylight shows down identical sepia speckle, the 365nm ultra-violet lamp shows identical orange-yellow fluorescence speckle down;

B. the Radix Paeoniae Alba: get gastric-dissolved capsule content 2g, porphyrize adds ethanol 10ml, and jolting 5 minutes filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Get Radix Paeoniae Alba control medicinal material fine powder 1g,, make the medical material contrast solution according to the preparation method of need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes every 1ml and contain 1mg solution, in contrast product solution; According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw each 10 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with 35-45: 3-7: 8-12: 0.1-0.4 chloroform-ethyl acetate-methanol-formic acid is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show identical bluish violet speckle;

C. Cortex Cinnamomi: get gastric-dissolved capsule content 1.5g, add ethanol 10ml, close plug, merceration 20 minutes, jolting constantly filters, and filtrate is as need testing solution; Get Cortex Cinnamomi control medicinal material fine powder 0.5g,, make control medicinal material solution according to the preparation method of need testing solution; Other gets the cinnamic aldehyde reference substance, adds ethanol and makes the reference substance solution that every 1ml contains 1 μ l; According to thin layer chromatography test, draw each 5 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with 15-19: 60～90 ℃-ethyl acetate of 2-4 petroleum ether is developing solvent, launches, and takes out, and dries, and spray is with dinitrophenylhydrazine ethanol test solution; In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph, show the speckle of same color;

D. Fructus Amomi: get gastric-dissolved capsule content 2g, porphyrize adds absolute ether 20ml, and merceration spends the night; Filter, filtrate volatilizes naturally, and residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution; Get Fructus Amomi control medicinal material fine powder 0.5g,, make the medical material contrast solution according to the preparation method of need testing solution; Get the bornyl acetate reference substance, add dehydrated alcohol and make the solution that every 1ml contains 10 μ l, in contrast product solution; According to thin layer chromatography test, draw above-mentioned three kinds of each 5ul of solution, respectively with same silica gel g thin-layer plate on, with 20-24: 1 cyclohexane extraction-ethyl acetate is developing solvent, launches, and takes out, and dries, spray is with 5% vanillin sulfuric acid solution, be heated to speckle develop the color clear; In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color;

Wherein the molten capsular discriminating of colon comprises one or more in the following method:

E. Rhizoma Corydalis: get colon soluble and intestine soluble capsule 's content 4g, porphyrize adds ammonia solution 30ml dissolving, puts in the separatory funnel, and the 50ml jolting that adds diethyl ether is extracted, and divides and gets ether layer, reclaims solvent, and residue adds methanol 1ml makes dissolving, as need testing solution; Get Rhizoma Corydalis control medicinal material fine powder 1g, the saturated ether 30ml of ammonification soaked overnight filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution; Get the tetrahydropalmatine reference substance, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution; According to thin layer chromatography test, draw each 3 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with 6-8: 3-5: it is developing solvent that 1 normal hexane-chloroform-methanol adds 1 strong ammonia solution, launches, and takes out, and dries, smoked clear to the speckle colour developing with iodine vapor; Inspect under the daylight, in the test sample chromatograph, with reference substance, the corresponding position of control medicinal material chromatograph on, show the speckle of same color; After in air, waving the iodine that adsorbs on the most plate, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with reference substance, the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;

F. Fructus Psoraleae: get colon soluble and intestine soluble capsule 's content 1g, add water 20ml dissolving, aqueous solution adds ethyl acetate 30ml extraction, divides and gets ethyl acetate liquid evaporate to dryness, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Get Fructus Psoraleae control medicinal material fine powder 0.5g, add ethyl acetate 20ml, ultrasonic 30 minutes, filter, filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as the medical material contrast solution; Get psoralen, isopsoralen reference substance, add ethyl acetate and make the mixed solution that every 1ml contains 2mg, in contrast product solution; According to thin layer chromatography test, draw each 4 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, with 3-5: 1-2 normal hexane-ethyl acetate is developing solvent, launches, and takes out, and dries, and spray is put under the ultra-violet lamp 365nm and inspected with 10% potassium hydroxide methanol solution; In the test sample chromatograph, with reference substance, the corresponding position of control medicinal material chromatograph on, show two identical fluorescence speckles;

G. Radix Glycyrrhizae: get colon soluble and intestine soluble capsule 's content 5g, porphyrize adds chloroform 40ml, supersound process 15-30 minute, filter, discard filtrate, filtering residue adds methanol 50ml, supersound process 15-30 minute, filters, filtrate is concentrated into about 5ml, is added on neutral alumina post 100～200 orders of having handled well, 15g, on internal diameter 10～15mm,, collect eluent with 40% methanol 150ml eluting, evaporate to dryness, residue adds water 30ml makes dissolving, with water saturated n-butanol extraction 2-3 time, and each 25ml, merge n-butyl alcohol liquid, with ammonia scrubbing 2-4 time, each 20ml, n-butyl alcohol liquid is put evaporate to dryness in the water-bath, residue adds the 1ml dissolve with methanol, as need testing solution; Extracting liquorice control medicinal material fine powder 2g according to the preparation method of need testing solution, makes control medicinal material solution; Test according to thin layer chromatography, draw above-mentioned two kinds of each 8ul of solution, put respectively on same silica gel g thin-layer plate, with 13-17: 38-45: 20-25: lower floor's solution that 8-12 chloroform-ethyl acetate-methanol-water is placed below 10 ℃ is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; Inspect under the daylight, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color; Put under the ultra-violet lamp 365nm and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;

H. the thin layer chromatography identification experiment of Radix Saposhnikoviae: get colon soluble and intestine soluble capsule 's content 1g, porphyrize adds acetone 20ml, and supersound process 15-25 minute, filter, filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution; Get Radix Saposhnikoviae control medicinal material fine powder 1g,, make control medicinal material solution according to the preparation method of need testing solution; According to the thin layer chromatography test, draw each 15 μ l of above-mentioned two kinds of solution, put in same silica gel G F respectively ₂₅₄On the lamellae, with 7-9: 1 chloroform-methanol is developing solvent, launches, and takes out, and dries, and puts under the uviol lamp 254nm and inspects; In the test sample chromatograph, with the corresponding position of control medicinal material on, show the speckle of same color.

6, Chinese medicinal capsule preparation as claimed in claim 1 or 2 is characterized in that the determination in the method for quality control of said preparation comprises following method:

A. content of paeoniflorin is measured:

The selection of chromatographic column: adopt the octadecylsilane chemically bonded silica chromatographic column;

The selection of mobile phase: the ratio of acetonitrile-water is 15-19: 75-88

The detection wavelength is 230nm, flow velocity 1.0ml/min;

Number of theoretical plate calculates by the peoniflorin peak should be not less than 1500;

The preparation of need testing solution: get gastric-dissolved capsule content 0.3g, the accurate title, decide, and puts in the 25ml measuring bottle, add the about 20ml of methanol, supersound process, power, 150-300W, frequency, 40-70KHz, 20-40 minute, put coldly, add methanol to scale, shake up, leave standstill, get supernatant, filter with 0.45 μ m microporous filter membrane, get filtrate, promptly;

B. the assay of psoralen:

Chromatographic column: octadecylsilane chemically bonded silica chromatographic column; The methanol of mobile phase: 45-55: 45-55-1% glacial acetic acid or methanol-acetonitrile-water or methanol-water; The detection wavelength is 245nm; Flow velocity 0.8ml/min; Column temperature 25-40 ℃; Number of theoretical plate calculates by the psoralen peak should be not less than 2000;

The preparation of need testing solution: get colon soluble and intestine soluble capsule 's content 0.4g, put in the 25ml measuring bottle, add the about 20ml of methanol, supersound process power, 150-300W, frequency, 40-70KHz 20-40 minute, is put cold, add methanol to scale, shake up, leave standstill, get supernatant, filter with 0.45 μ m microporous filter membrane, get filtrate, promptly.

7, Chinese medicinal capsule preparation as claimed in claim 6 is characterized in that the determination in the method for quality control of said preparation comprises following method:

Content of paeoniflorin is surveyed:

The selection of chromatographic column: octadecylsilane chemically bonded silica chromatographic column

The selection of mobile phase: 17: 83 acetonitrile-water;

The detection wavelength is 230nm, flow velocity 1.0ml/min;

The preparation of need testing solution: get gastric-dissolved capsule content 0.3g, the accurate title, decide, and puts in the 25ml measuring bottle, add the about 20ml of methanol, supersound process, power 200W, frequency 59KHz 30 minutes, is put cold, add methanol to scale, shake up, leave standstill, get supernatant, filter with 0.45 μ m microporous filter membrane, get filtrate, promptly;

The assay of psoralen:

Chromatographic column: octadecylsilane chemically bonded silica chromatographic column; Mobile phase: 50: 50 methanol-water; The detection wavelength is 245nm; Flow velocity 0.8ml/min; 25 ℃ of column temperatures; Number of theoretical plate calculates by the psoralen peak should be not less than 2000;

The preparation of need testing solution: get the content under the colon soluble and intestine soluble capsule content uniformity item, porphyrize is got 0.4g, the accurate title, decide, and puts in the 25ml measuring bottle, adds the about 20ml of methanol, supersound process, power 200W, frequency 59KHz, 30 minutes, put coldly, add methanol to scale, shake up, leave standstill, get supernatant, filter with 0.45 μ m microporous filter membrane, get filtrate, promptly.