CN1283304C - Composite Chinese medicine for treating bloat and its prepn process and quality control method - Google Patents
Composite Chinese medicine for treating bloat and its prepn process and quality control method Download PDFInfo
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- CN1283304C CN1283304C CN 03109399 CN03109399A CN1283304C CN 1283304 C CN1283304 C CN 1283304C CN 03109399 CN03109399 CN 03109399 CN 03109399 A CN03109399 A CN 03109399A CN 1283304 C CN1283304 C CN 1283304C
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- Medicinal Preparation (AREA)
Abstract
The present invention discloses a Chinese medicinal composition for treating drum belly symptoms, a preparation method thereof and a quality control method thereof. The composition is composed of the following five medicinal materials: melanterite, euphorbia kansui, Chinese date, aucklandia root and wheat. The Chinese medicinal composition is prepared through the following steps: pulverizing the medicinal materials into fine powder, sieving and uniformly mixing; pilling by mixing the mixture with hot water; drying the pills at below 60 DEG C to 70 DEG C; finally, preparing clinically acceptable preparation formulations directly through conventional process steps or by adding pharmacologically acceptable excipient. Simultaneously, the present invention also provides a quality control method for identifying the components of the composition. In treating drum belly symptoms, the composition has better effect on diuresis promotion for removing edema, moisture elimination and spleen strengthening.
Description
Invention field
The present invention relates to a kind of Chinese medicine composition, particularly treat the Chinese medicine composition of hoove, relate to the preparation method and the method for quality control of said composition simultaneously.
Background technology
Traditional Chinese medical science hoove, modern medicine indication: cirrhotic ascites, tuberculous peritonitis, chylous ascites, pernicious swell and ache etc., and many morbidity with hepatic ascites, cirrhotic ascites of traditional Chinese medical science distension disease is many, according to relevant bibliographical information: because the liver pathological changes that hepatitis causes, and the hepatic ascites, the liver cirrhosis patient sickness rate that produce account for 20%.At present, this disease medicine of clinical treatment is many based on the Western medicine diuretic.As hydrochlorothiazide, spironolactone etc., these medicines can only relief of symptoms, and poor effect is taken for a long time and caused Water-Electrolyte disorder (high and low potassium mass formed by blood stasis).
Summary of the invention
One object of the present invention is to disclose a kind of Chinese medicine composition of new treatment hoove; Another object of the present invention is the method for the Chinese medicine composition of a kind of new treatment hoove of open preparation; The object of the invention also is to disclose a kind of method of quality control of new Chinese medicine composition.
The crude drug of pharmaceutical composition of the present invention is formed and proportioning following (by weight):
Melanteritum 150-250 weight portion Radix Kansui 15-25 weight portion Fructus Jujubae 150-250 weight portion
Radix Aucklandiae 15-25 weight portion Semen Tritici aestivi 60-130 weight portion.
It is (by weight) that the crude drug of pharmaceutical composition of the present invention is formed optimum ratio:
Melanteritum 230 weight portion Radix Kansuis 23 weight portion Fructus Jujubaes 180 weight portions
The Radix Aucklandiae 23 weight portion Semen Tritici aestivis 80 weight portions.
It is (by weight) that the crude drug of pharmaceutical composition of the present invention is formed optimum ratio:
Melanteritum 180 weight portion Radix Kansuis 18 weight portion Fructus Jujubaes 230 weight portions
The Radix Aucklandiae 18 weight portion Semen Tritici aestivis 120 weight portions.
It is (by weight) that the crude drug of pharmaceutical composition of the present invention is formed optimum ratio:
Melanteritum 200 weight portion Radix Kansuis 20 weight portion Fructus Jujubaes 200 weight portions
The Radix Aucklandiae 20 weight portion Semen Tritici aestivis 100 weight portions.
The above Melanteritum is to give birth to being good, and Fructus Jujubae is good with the enucleation stir-fry, and Semen Tritici aestivi is to fry to good.
Press practice of pharmacy, preparation of pharmaceutical compositions of the present invention can be become the various clinical pharmaceutical dosage form, comprise the dosage form of oral formulations or parenterai administration.Said oral formulations is selected from a kind of in the middle of the tablet, capsule, pill, granule, suspensoid, drop pill, oral liquid; Said parenterai administration dosage form is selected from a kind of in the middle of injection, aerosol, suppository or the subcutaneous administration dosage form.
Medicine of the present invention also can add conventional drug excipient, as solvent, disintegrating agent, correctives, antiseptic, coloring agent etc.
This preparation of drug combination method:
The above five tastes are ground into fine powder, sieve mixing; Close the pill that sticks together with hot water, dry below 60-70 ℃, at last directly or add pharmaceutically acceptable excipient and make clinical acceptable forms through conventional operation, as pill, tablet, oral liquid, capsule, granule.
The medicament that this compositions is made adopts following a kind of and/or several discrimination method to carry out quality control:
A. get this composite preparation 1g, porphyrize adds water 10ml, boils 8-12 minute, filters, and gets filtrate 1ml, adds iron potassuim cyanide test liquid 2-3 and drips, and promptly generates blue precipitation, separates, and is deposited in the dilute hydrochloric acid and does not dissolve, and hydro-oxidation sodium test solution is brown precipitate;
B. get this composite preparation 15g, porphyrize adds 60-90 ℃ of petroleum ether 50ml, flooded 25-35 minute, and supersound process 25-35 minute, filter, filtrate volatilizes, and residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets Radix Aucklandiae control medicinal material 0.5g, adds ethyl acetate 10ml, and supersound process 25-35 minute, filter, filtrate is medical material solution in contrast; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with 8-12: 0.5-1.5 cyclohexane extraction one acetone is developing solvent, launch, taking-up is dried, and spray is with 10% ethanol solution of sulfuric acid, and is moistening fully to the plate face; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
C. get this composite preparation 20g, porphyrize adds ethanol 60ml, reflux 0.5-2 hour, filters, filtrate evaporate to dryness, residue add water 30ml makes dissolving, uses ethyl acetate extraction three times, each 20ml, merge ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Kansui control medicinal material 2g, adds ethanol 40ml, and reflux 1 hour filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, in contrast medical material solution; Test according to thin layer chromatography (appendix V1B of middle traditional Chinese medicines version in 2000), draw need testing solution 10 μ l, control medicinal material solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent with the carboxymethyl cellulose sodium, with 18-25: 1-3: 1.5-1.5 chloroform-ethyl acetate-formic acid is developing solvent, launch, take out, dry, put under the ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.The preparation that excipient is arranged in the described method of quality control can be removed its excipient according to a conventional method earlier.
The present composition has inducing diuresis to remove edema, dehumidifying spleen invigorating effect in the treatment hoove, distension and fullness of the chest and abdomen, extremity edema, constipation, oliguria with reddish urine disease are had good effect.
Below further specify the present invention by pharmacodynamics, clinical and experimental study.
The pharmacodynamic study of experimental example 1 group thing preparation (ascites pill)
Test material: 1. animal: mice: Kunming mouse, hero, body weight: 20-22g.Available from the department of the Chinese Academy of Sciences of laboratory animal section of Beijing Medical University, one-level, the quality certification number: the moving word of doctor 01-3049 number.Rat: Wistar kind rat, hero, body weight: 150-200g.Available from the department of the Chinese Academy of Sciences of laboratory animal section of Beijing Medical University, one-level, the quality certification number: the moving word of doctor 01-3056 number.2. be subjected to the reagent thing: ascites pill medicated powder, cross 100 orders, Handan Pharmaceutical Co., Ltd provides .3. reagent and medicine: hydrochlorothiazide tablet, 25mg/ sheet, the Bohai Sea, Tangshan City pharmaceutical factory, lot number: 970801.The neostigmine methylsulfate injection, 0.5mg/ml, Chinese Shanghai Xinyi Pharmaceutical Factory, lot number: 960404.Gum arabic powder, the packing of Shanghai chemical reagents corporation, lot number: 880414.Carbon powder: Beijing chemical reagents corporation product.Total protein (TP) is measured test kit (the urea method contracts again), lot number 990921; Albumin (ALB) test kit, lot number 991008: blood urea nitrogen (BUN) test kit (Diacetylmonoxime method), lot number: 991228; Creatinine (Cr) test kit (picric acid does not remove protein method), lot number: 991028.Be Beijing northization fine chemicals Co., Ltd product.Other reagent are analytical pure, available from Beijing chemical reagents corporation.
One, to the diuresis of normal mouse and highly rush down effect
(1) ascites pill is to the discharge function and the diuresis of normal mouse
1. method: Kunming mouse, hero, fasting 12h, experimental animal are divided into 6 groups, 20 of normal control groups, ascites pill 0.7g/kg, 1.0g/kg, 3 groups of 1.4g/kg, hydrochlorothiazide 30mg/kg, 60mg/kg2 group, every group of 10 animals are respectively organized in administration.Gently press the thing hypogastric region before the experiment, drain surplus urine.Every Mus lumbar injection 2ml, 37 ℃ of warm salines are loaded as water, simultaneously ig medicine 0.2ml/10g body weight, 0-2h, 2-6h urine amount after the record administration, with the significance of t check comparing difference between group, each group is rushed down number of animals down in the record administration 6h, with X2 check carrying out statistics relatively.
2. result: see Table 1, significantly increase after the administration animal voided volume between 2-6h behind the ascites pill dosage 0.7g/kg single gastric infusion, but do not have obvious dose-effect relationship.Ascites pill 1.4g/kg dosage, half animal passage of loose stools, with normal control group ratio, the passage of loose stools number of animals significantly increases (P＜0.01).
Table 1 ascites pill is to the discharge function and the diuresis of normal mouse
| Group | Number of animals | Dosage g/kg | Rush down animal down | Urine amount ml | |
| 1-2h | ＞2-6h | ||||
| Normal control group ascites pill ascites pill ascites pill hydrochlorothiazide hydrochlorothiazide | 20 10 10 10 10 10 | - 0.7 1.0 1.4 0.03 0.06 | 0 0 1 5** 0 0 | 2.77±0.84 2.07±0.47 2.26±0.48 1.87±0.76 3.40±1.01 3.17±0.55 | 1.34±0.50 2.49±0.638* 2.14±0.51 2.49±0.69 1.70±0.38 1.97±0.51 |
Annotate: with the normal control group than * P＜0.05, * * P＜0.01.
3. conclusion: ascites pill has diuresis and diarrhea inducing effect to normal mouse.
(2) the normal mouse carbon powder is advanced and intestinal in the influence of water content
1. method: Kunming mouse, male, weigh behind the fasting 24h, be divided into 5 groups at random, every group of 10 animals.Be followed successively by normal control group, ascites pill 0.7g/kg, 1.0g/kg, 1.4g/kg, neostigmine 0.1mg/kg group, gastric infusion 0.2ml/10g.Ig 5% carbon powder 0.2ml/ only puts to death animal to behind the carbon powder 20min behind the 2h, gets small intestinal total length (pylorus is to ileocecus) and large intestine (ileocecus is to rectum) total length, and the carbon determination end advances length, small intestinal weight in wet base, large intestine weight in wet base.Intestinal tube in 80 ℃ dry after, take by weighing each section dry weight again, calculate carbon powder by following formula and advance percentage rate, moisture percentage rate in the small intestinal, big enteral moisture percentage rate.Significance with t check comparable group differences between group.
Carbon powder advances percentage rate=carbon powder advance distance (cm)/small intestinal total length (cm) * 100% in small intestinal
2. result: (1) sees Table 2 to the influence of intestinal propulsion function, ascites pill 0.7g/kg-1.4g/kg significantly promote the small intestinal carbon powder advance percentage rate (with normal control than P＜0.05 or P＜0.01).
Table 2 ascites pill single-dose is to the influence of small intestine movement of mice propulsion functions
| Group | Number of animals | Dosage g crude drug/kg | Carbon powder advances percentage rate % |
| Normal control group ascites pill ascites pill ascites pill neostigmine | 12 10 10 10 10 | - 0.7 1.0 1.4 0.0001 | 46.17±13.61 74.95±15.05* 73.93±13.45* 82.20±11.12** 75.57±8.34** |
Annotate: with the normal control group than * P＜0.05, * * p＜0.01.
(2) to the influence of intestinal water content, see Table 3,4, ascites pill significantly increases small intestinal intestinal moisture (P＜0.001) at 0.7g/kg-1.4g/kg, and increases the small intestinal weight in wet base.
Table 3 ascites pill single-dose is to the influence of normal mouse intestinal water content
| Group | Number of animals | Dosage g/kg | Intestinal moisture (%) | |
| Small intestinal | Large intestine | |||
| Normal control group ascites pill ascites pill ascites pill neostigmine | 12 10 10 10 10 | - 0.7 1.0 1.4 0.0001 | 79.30±0.84 82.46±0.91*** 81.75±0.87*** 81.81±0.80*** 79.15±3.97 | 92.75±4.28 94.75±0.12 94.25±0.67 94.15±0.65 94.09±1.14 |
Annotate: with the normal control group than * * * P＜0.001.
Table 4 ascites pill single-dose is to the influence of intestinal weight in wet base
| Group | Number of animals | Dosage g/kg | Small intestinal weight in wet base (g) | Full intestinal weight in wet base (g) |
| Normal control group ascites pill ascites pill ascites pill neostigmine | 12 10 10 10 10 | - 0.7 1.0 1.4 0.0001 | 1.78±0.20 2.25±0.21* 2.15±0.15 1.89±0.18 1.82±0.25 | 2.52±0.25 2.96±0.26 2.93±0.18 2.64±0.25 2.59±0.30 |
Annotate: with the normal control group than * p＜0.05.
3. conclusion: ascites pill is given mice single gastric infusion, and 0.7g/kg has obvious diuresis, and the 0.7g/kg-1.4g/kg administration significantly promotes the intestinal propulsion function after 2 hours, increase the small intestinal water content, and 1.4g/kg has obvious diarrhea inducing effect.According to above result of the test ascites pill normal mouse there is diuresis and highly rushes down effect.
Two, ascites pill is to the diuresis of normal rat
1. method: choose 150-200g male Wistar kind rat, make it to adapt to the living environment 1-2 day of metabolic cage in advance.Animal is weighed before the experiment, and 38 ℃ of warm water of ig 25ml/kg are collected 2h urine amount, selects the urine amount to reach the institute animal of the amount of pouring into more than 40% and is used for diuresis and tests.Animal fasting 18h before the experiment.Water load is with 38 ℃ of normal saline 25ml/kg ig per hour 1 time, totally 2 times.Ig gives ascites pill 0.34g/kg, 0.49g/kg, 0.7g/kg, 1.0g/kg totally 4 dosage groups, positive drug hydrochlorothiazide 15mg/kg when the 2nd water load.Each organizes the administration volume is 1ml/100g, the normal control group give with the volume ordinary water.Gently press the thing lower abdomen during experiment beginning, drain surplus urine.Animal is put into metabolic cage, observe after the medication 1,2,4,6,8,12,24h urine amount; 24h defecate total weight in wet base, gross dry weight; The 24h amount of drinking water.Significance with t check comparable group differences between group.
2. result: ascites pill single ig administration 0.49g/kg, 1.0g/kg dosage, the normal matched group of 6-24h urine amount significantly increases (P＜0.05 or P＜0.01) after the administration, and 0.49g/g group specific gravity of urine significantly reduces (P＜0.01), sees Table 5.The interior urine amount of 6h significantly increases (P＜0.01) than matched group after the administration of positive drug hydrochlorothiazide group, but 6-24h then significantly reduces (P＜0.05).Ascites pill 1.0g/kg does not have obvious influence (P＞0.05) to animal stool weight in wet base and dry weight, sees Table 6.
Each treated animal amount of drinking water of ascites pill administration has increase trend, but does not reach statistics marked difference (P＞0.05) as yet, sees Table 7.
Table 5 ascites pill single gastric infusion is to the influence of normal rat urine amount (n=10 X ± SD)
| Group | Dosage g/kg | Urine amount (ml) | Specific gravity of urine | ||
| 0-6h | 6-24h | 0-24h | |||
| Normal control group ascites pill ascites pill ascites pill ascites pill hydrochlorothiazide | - 0.34 0.49 0.70 1.00 0.01 | 5.65±1.25 5.19±1.97 3.08±2.03* 3.02±1.21** 5.84±1.57 10.65±1.31** | 6.62±1.19 8.37±2.18 15.83±6.95* 9.30±4.73 11.55±2.57** 4.88±1.18* | 12.28±1.20 13.57±3.34 18.91±8.23 12.32±4.32 17.39±3.05** 15.53±2.42** | 1.0315±0.0045 1.0404±0.0067* 1.0141±0.0072** 1.0278±0.0068 1.0262±0.0138 1.0119±0.0063** |
Annotate: with the same period normal control group than * P＜0.05, * * P＜0.01.
Table 6 ascites pill single gastric infusion is to the influence of normal rat stool amount and water content (n=10 X ± SD)
| Group | Dosage g/kg | 24h dries by the fire just weight (g) | |
| Total weight in wet base | Gross dry weight | ||
| Normal control group ascites pill ascites pill ascites pill ascites pill hydrochlorothiazide | - 0.34 0.49 0.70 1.00 0.01 | 3.04±0.48 3.60±0.75 2.95±0.85 3.03±0.97 2.57±0.80 4.12±1.32 | 1.40±0.38 1.69±0.45 1.36±0.60 1.25±0.55 1.24±0.33 1.43±0.35 |
Table 7 ascites pill single gastric infusion is to the influence of normal rat amount of drinking water (n=10 X ± SD)
| Group | Dosage g/kg | 24h amount of drinking water (ml) |
| Normal control group ascites pill ascites pill ascites pill ascites pill hydrochlorothiazide | - 0.34 0.49 0.70 1.00 0.015 | 14.1±10.6 13.0±6.6 25.1±15.2 19.7±12.8 20.9±8.1 12.1±4.6 |
3. conclusion: ascites pill single gastric infusion 0.49g/kg/1.0g/kg dosage, after administration 6-24h significantly increase rat urine amount (with the normal control group than P＜0.05 or P＜0.01), and reduce specific gravity of urine.
Three, to the therapeutical effect of rat hemoglobinuria acute renal failure model
1. method: Wistar kind male white rat, body weight 170-220g places metabolic cage, writes down normal amount of drinking water and urine amount.Animal is prohibited water 24h before modeling, selects the above animal of 30g that loses weight, and intramuscular injection 50% glycerol is pressed 10ml/kg and injected at rat both sides hindlimb muscle respectively.Injection relief rat ad lib and drinking-water.50% glycerol moulding 30h gets hematometry BUN, Cr through the eye socket vein.The administration of dividing into groups behind the moulding 33h is respectively the normal control group, 50% glycerol moulding group, 50% glycerol moulding ascites pill 0.25g/kg, 0.5g/kg, 1.0g/kg dosage treatment group and hydrochlorothiazide 10mg/kg dosage treatment group.Every group of 10 animals, gastric infusion 3d irritates the long-pending 10ml/kg of being of body of stomach continuously, and matched group is given with the volume ordinary water.Animal is put record amount of drinking water every day, urine amount, specific gravity of urine, pH in the metabolic cage, and 24h after the last administration gets hematometry TP, ALB, BUN, SCr and blood Na through the eye socket vein
+, K
+Live to kill all animals then, get kidney and weigh and be fixed in 10% formaldehyde, through paraffin section, HE dyeing, the microscopically animal is got kidney and weighs and be fixed in 10% formaldehyde, through paraffin section, HE dyeing, microscopically is observed the nephropathy degree.Measurement data is carried out statistical with t check between group, and renal tissue pathological change rank is carried out statistical with rank test.
2. result: (1) sees Table 8,9,10 to the influence of renal failure rat urine amount, proportion, pH.Ascites pill 0.25g/kg-1.0g/kg does not have obvious influence to acute renal failure rat urine amount, specific gravity of urine and pH.
Table 8 ascites pill causes the influence (n=10) of acute renal failure rat urine amount to 50% glycerol
| Group | Dosage g/kg | Urine amount (ml) | ||
| 24h | 48h | 72h | ||
| Normal control group 50% glycerol moulding acute renal failure+ascites pill acute renal failure+ascites pill acute renal failure+ascites pill acute renal failure+hydrochlorothiazide | - 0.34 0.25 0.50 1.00 0.01 | 3.06±1.90 20.62±7.33 ## 22.57±6.58 15.83±11.62 19.75±6.16 15.71±8.48 | 7.09±6.39 19.69±12.31 # 23.00±11.19 15.83±11.62 19.29±7.09 19.25±2.99 | 8.6±6.82 15.43±8.79 20.29±9.91 18.20±11.48 13.00±6.03 13.20±2.17 |
Annotate: with the same period normal control group than #P＜0.05, ##P＜0.01.
Table 9 ascites pill causes the influence (n=10) of acute renal failure rat specific gravity of urine to 50% glycerol
| Group | Dosage g/kg | Specific gravity of urine (g/ml) | ||
| 24h | 48h | 72h | ||
| Normal control group 50% glycerol moulding acute renal failure+ascites pill acute renal failure+ascites pill acute renal failure+ascites pill acute renal failure+hydrochlorothiazide | - 0.34 0.25 0.50 1.00 0.01 | 3.060±0.009 1.029±0.009 ## 1.027±0.006 1.024±0.008 1.035±0.014 1.026±0.011 | 1.078±0.027 1.040±0.098 ## 1.039±0.006 1.036±0.011 1.032±0.005 1.029±0.006 * | 1.077±0.020 1.037±0.013 ## 1.035±0.009 1.039±0.009 1.038±0.007 1.032±0.007 |
Annotate: with friend's normal control group than #P＜0.05, ##P＜0.01.
With the same period 50% glycerol moulding moulding group than * P＜0.05.
Table 10 ascites pill causes the influence (n=10) of acute renal failure rat urine pH to 50% glycerol
| Group | Dosage g/kg | Specific gravity of urine (g/ml) | ||
| 24h | 48h | 72h | ||
| Normal control group 50% glycerol moulding acute renal failure+ascites pill acute renal failure+ascites pill acute renal failure+ascites pill acute renal failure+hydrochlorothiazide | - 0.34 0.25 0.50 1.00 0.01 | 8.79±0.03 8.64±0.019 # 8.73±0.05 8.78±0.06 8.72±0.12 8.69±0.09 | 8.72±0.06 8.75±0.05 8.72±0.07 8.72±0.03 8.73±0.03 8.69±0.07 | 8.79±0.02 8.79±0.03 8.78±0.05 8.81±0.01 8.76±0.04 8.80±0.02 |
Annotate: with the same period normal control group than #P＜0.05.
(2) to the influence of acute renal failure rat blood biochemical indicator, see Table 11.Ascites pill does not have obvious influence at 0.25g/kg-1.0g/kg to acute renal failure rat blood serum BUN, SCr, TP, ALB concentration.
Table 11 ascites pill causes the influence (n=10) of acute renal failure rat blood biochemical indicator to 50% glycerol
| Group | Dosage g/kg | BUN Mmol/L | SCr μmol/L | TP g/L | ALB g/L |
| Normal control group 50% glycerol moulding acute renal failure+ascites pill acute renal failure+ascites pill acute renal failure+ascites pill acute renal failure+hydrochlorothiazide | - - 0.25 0.50 1.00 0.01 | 7.53±1.34 17.85±7.20 ## 19.79±8.93 23.71±8.09 18.15±5.29 13.50±2.72 | 108.99±12.42 152.46±31.02 # 161.24±5.51 185.64±43.76 135.83±18.48 156.53±15.27 | 71.56±4.37 73.32±3.97 72.52±3.62 76.24±4.44 73.96±6.66 73.12±3.60 | 40.88±9.64 39.60±1.87 37.02±3.22 39.26±1.04 38.47±2.37 37.56±2.97 |
Annotate: with the normal control group than #P＜0.05 ##P＜0.01.
(3) to acute renal failure rat blood serum Na
+, K
+The influence of concentration sees Table 12.Ascites pill has rising serum N a
+, K
+The effect of concentration (with model group than P＜0.05 or P＜0.01)
Table 12 ascites pill causes the influence (n=10) of acute renal failure rat blood serum Na+, K+ concentration to 50% glycerol
| Group | Dosage g/kg | Na + mmol/L | K + mmol/L |
| Normal control group 50% glycerol moulding acute renal failure+ascites pill acute renal failure+ascites pill acute renal failure+ascites pill acute renal failure+hydrochlorothiazide | - - 0.25 0.50 1.00 0.01 | 121.27±26.78 105.26±14.65 146.20±17.58 # 108.79±31.48 128.74±13.06 # 103.87±31.16 | 6.03±0.68 6.80±1.33 6.81±1.14 7.07±0.69 8.84±0.98 ## 13.77±2.71 ## |
Annotate: with 50% glycerol moulding group than * P＜0.05.**P＜0.01。
(4) to the influence of acute renal failure rat kidney lesion degree
The continuous gastric infusion of ascites pill 0.25g/kg-1.0g/kg is after 3 days, and the kidney coefficient that kidney injury due to 50% glycerol is caused increases does not have obviously influence, and obvious therapeutic action is not seen by Histological change to kidney pathology, sees Table 13.
Table 13 ascites pill causes the influence (n=10) of acute renal failure kidney of rats coefficient to 50% glycerol
| Group | Dosage g/kg | Kidney coefficient g/100g body weight |
| Normal control group 50% glycerol moulding acute renal failure+ascites pill acute renal failure+ascites pill acute renal failure+ascites pill acute renal failure+hydrochlorothiazide | - - 0.25 0.50 1.00 0.01 | 0.824±0.058 1.418±0.235** 1.411±0.187 1.585±0.220 1.504±0.218 1.336±0.165 |
Annotate: with the normal control group than * * p＜0.01.
3, conclusion: ascites pill does not have obvious diuresis to rat acute renal failure animal due to 50% glycerol, blood parameters is not had obvious sound, but rising serum N a is arranged
+, K
+Effect.
Four, ascites pill is to the influence of cancer ascites animal ascites volume
1. method: Kunming mouse, 70, body weight 19-21g, male, female half and half, all the other animal abdominal cavities inoculation S180 ehrlich ascites carcinoma except that the normal control treated animal, cancerous cell concentration 1.12 * 106/ml, every 0.2ml, animal is divided into 5 groups at random by body weight, both lotus tumor matched groups, ascites pill 0.25g/kg, 0.5g/kg, 1.0g/kg group, positive drug hydrochlorothiazide 15mg/kg group, ig administration 0.2ml/10g body weight is in lotus tumor the 8th, 9,10 days, administration every day 1 time, before administration, claim the weight of animals and fasting, prohibit water, after the administration 4-6 hour, weigh, with the body weight difference as the index of urinating.In lotus tumor the 11st day, weigh, put to death animal, open abdomen, with syringe sucking-off ascites and measurement volumes.The significance that compares body weight, ascites volume, urine amount difference with t check between group.
2. result: ascites pill 1g/kg dosage ig administration 3 days, can significantly reduce ehrlich ascites carcinoma mouse ascites amount (P＜0.01), see Table 14; The tumor animal body weight there is reduction trend, but does not have significance,statistical.See Table 15; But after administration every day in 6 hours urine amount and lotus tumor group see Table 16 than no obvious increase.Ascites pill 1.0g/kg group part animal has loose stool, and positive drug hydrochlorothiazide 15mg/kg dosage has the effect (P＜0.05) of remarkable minimizing lotus S180 ehrlich ascites carcinoma animal ascites volume.See Table 14.
Table 14 ascites pill is to the influence of lotus S180 ehrlich ascites carcinoma mouse ascites amount
| Group | Number of animals | Dosage g/kg | Administration natural law d | Ascites volume ml |
| Normal control group ehrlich ascites carcinoma model group lotus tumor+ascites pill lotus tumor+ascites pill lotus tumor+ascites pill lotus tumor+hydrochlorothiazide | 10 20 9 9 9 9 | - - 0.25 0.50 1.00 0.015 | - - 3 3 3 3 | - 13.86±4.58 12.67±2.74 12.30±1.64 9.19±2.68** 9.05±2.97* |
Annotate: in lotus S180 administration in the 8th, 9,10 days, continuous 3d, 11d gets ascites.With the ehrlich ascites carcinoma model group than * P＜0.05, * * P＜0.01.
Table 15 ascites pill is to the influence of lotus S180 ehrlich ascites carcinoma mice body weight
| Group | Number of animals | Dosage g/kg | Body weight g before the administration | 11 days body weight g of lotus tumor |
| Normal control group ehrlich ascites carcinoma model group lotus tumor+ascites pill lotus tumor+ascites pill lotus tumor+ascites pill lotus tumor+hydrochlorothiazide | 10 20 9 9 9 9 | - - 0.25 0.50 1.00 0.015 | 20.5±1.1 20.7±1.1 20.7±1.1 20.7±1.1 20.9±1.0 20.7±1.1 | 29.7±3.7 33.6±3.5 34.4±2.9 33.8±5.5 30.1±4.3 28.4±4.4 |
Table 16 ascites pill is to the influence of lotus S180 ehrlich ascites carcinoma mouse retention amount
| Group | Number of animals | Dosage g/kg | 6h urine amount (g) | ||
| The 1st day | The 2nd day | The 3rd day | |||
| Normal control group ehrlich ascites carcinoma model group lotus tumor+ascites pill lotus tumor+ascites pill lotus tumor+ascites pill lotus tumor+hydrochlorothiazide | 10 20 9 9 9 9 | - 0.34 0.25 0.50 1.00 0.01 | 4.12±0.56 3.97±0.60 3.83±0.87 2.96±1.31 3.04±1.22 4.69±0.91 | 4.34±0.53 2.88±0.77 ## 2.94±0.41 2.89±0.75 2.58±0.62 3.08±0.94 | 4.00±0.36 2.59±1.07 ## 2.52±0.89 2.60±0.96 1.98±0.62 2.01±0.77 |
Annotate: with the same period normal control group than ##P＜0.05
3. conclusion: ascites pill 1g/kg gastric infusion 3 days, significantly reduce lotus S180 ehrlich ascites carcinoma mouse ascites amount (P＜0.01).
Conclusion (of pressure testing): 1. ascites pill single gastric infusion has diuresis and diarrhea inducing effect (P＜0.05 or P＜0.01) at 0.7g/kg-1.4g/kg to normal mouse, and promotes small intestinal carbon powder propulsion functions (P＜0.05 or P＜0.01).2. ascites pill single gastric infusion has diuresis at 0.49g/kg, 1.0g/kg dosage to normal rat, significantly increases 6-24h urine amount (P＜0.05 or P＜0.01) after the administration.The ascites pill gastric infusion for three days on end, 0.25g/g-1.0g/kg causes the acute renal failure rat to 50% glycerol and does not show obvious diuresis, but can significantly increase blood Na
+, K
+Concentration.4. ascites pill gastric infusion 1.0g/kg has the effect (P＜0.01) of remarkable minimizing ascites volume for three days on end to lotus S180 ehrlich ascites carcinoma mice.
The clinical and experimental study of experimental example 2 groups thing preparation (ascites pill)
One, physical data: according to " clinical verification scheme " requirement, conscientiously select standard compliant case totally 400 examples of including in, adopt clinical random packet method, be divided into treatment and organize 300 examples, matched group 100 examples.
Not Fen Bu: see Table 1
Table 1 liang group sex distribution situation
| Group | The example number | Man (%) | Woman (%) |
| Treatment group matched group | 300 100 | 219(73.0) 76(76.0) | 81(27.0) 24(24.0) |
Two groups of case sexes distribute to learn by statistics and handle (P＞0.05), and no significance has comparability.
2. age distribution: see Table 2
Table 2 liang group age distribution situation
| Group | The example number | ＜30 years old | 31～40 years old | 41～50 years old | 51～60 years old | ＞60 years old |
| Treatment group matched group | 300 100 | 19 7 | 77 29 | 111 36 | 79 24 | 14 4 |
Two groups of minimum 20 years old of case ages, maximum 65 years old, mean age treatment group 44.94 ± 8.59 years old, matched group 44.51 ± 8.93 years old is learned by statistics and is handled (P＞0.05), and there was no significant difference has comparability.
3. occupation distributes: see Table 3
The table 3 liang professional distribution situation of group
| Group | The example number | Cadre (%) | Workman (%) | Peasant (%) |
| Treatment group matched group | 300 100 | 77(25.67) 31(31.0) | 111(37.0) 37(37.0) | 112(37.33) 32(32.0) |
Two groups of case occupations distribute to learn by statistics and handle (P＞0.05), and no significance has comparability.
4. the course of disease distributes: see Table 4
Table 4 liang group course of disease distribution situation
| Group | The example number | ＜1 year (%) | 1～5 year (%) | 6～10 years (%) | ＞10 years (%) |
| Treatment group matched group | 300 100 | 61(20.33) 18(18.0) | 125(41.67) 45(45.0) | 65(21.67) 24(24.0) | 49(16.33) 13(13.0) |
Two groups of case courses of disease are the shortest 0.5 year, and are the longest 30 years, average course of disease treatment group 7.16 ± 3.71 years, and matched group 7.08 ± 3.55 years is learned by statistics and is handled (P＞0.05), and no significance has comparability.
5. traditional Chinese medical science primary symptom distributes: see Table 5
Table 5 liang group traditional Chinese medical science primary symptom is light, in, the severe distribution situation
| Group | The example number | Slightly (%) | Moderate (%) | Severe (%) |
| Treatment group matched group | 300 100 | 63(21.0) 22(22.0) | 166(55.33) 52(52.0) | 71(23.67) 26(26.0) |
Two groups of traditional Chinese medical science primary symptoms are light, in, severe distributes to learn by statistics and handles (P＞0.05), there was no significant difference has comparability.
6. the doctor trained in Western medicine Clinical types distributes: see Table 6
Table 6 liang group doctor trained in Western medicine Clinical types distribution situation
| Group | The example number | Active liver cirrhosis (%) | Stability liver cirrhosis (%) |
| Treatment group matched group | 300 100 | 203(67.67) 70(70.0) | 97(32.33) 26(26.0) |
Two groups of doctor trained in Western medicine Clinical types distribute to learn by statistics and handle (P＞0.05), and there was no significant difference has comparability.
7. clinical stages, distribute: see Table 7
Table 7 clinical stages distribution situation
| Group | The example number | (%) in early days | Middle and advanced stage (%) |
| Treatment group matched group | 300 100 | 161(53.67) 55(55.0) | 139(46.33) 45(45.0) |
Two groups of clinical stagess, distribute, and learns by statistics and handle (P＞0.05), and there was no significant difference has comparability.
Two, case choice criteria
According to " the new Chinese medicine clinical research guideline " of Ministry of Public Health formulation, and, draft in conjunction with the characteristics of this medicine with reference to the related content in the books such as existing university teaching.
1. traditional Chinese medical science differential diagnosis of diseases syndrome differential diagnosis standard
(1) differential diagnosis of diseases: distension disease.(2) dialectical: insufficiency of the spleen leading to overabundance of dampness, water liquid are stagnated the damp-heat gluing each other card of holding concurrently.Primary symptom: abdominal distension such as drum, or distension and fullness of the chest and abdomen.Double disease: diet reduces, or anorexia, or abdominal distention after meal.Edema of lower limbs, or general edema.Oliguria, or oliguria with reddish urine.It is not well to defecate, or constipation.The tongue arteries and veins: tongue tip side of red, tongue are greasy in vain or yellow greasy, stringy pulse or stringy and rapid pulse.
(3) diagnosis: all possess 1 of above-mentioned primary symptom, holds concurrently disease more than 2, and corresponding tongue arteries and veins, can make diagnosis.
2. primary symptom severity extent grade scale
Abdominal part swells: slight (+): the time sense abdominal distention, that presses is still soft, kowtow as drum, or see side of body distension down.Moderate (++): the enlarged abdomen distension, by wrap up in water as capsule, the underwater sound of shaking is arranged when changing one's position, or sees distension and fullness of the chest and abdomen.Severe (+++): the abdominal part urgency that stretches tight that swells, the heavily fortified point of pressing is full, and the acromphalus is outstanding, or sees that blue veins exposes.
3. Western medicine diagnose standard
(1) Western medicine diagnose: the doctor trained in Western medicine disease that assertive evidence is involved, as liver cirrhosis, main with more simple or stable cirrhosis patients in decompensation such as hepatitis liver cirrhosis, alcoholic cirrhosis, parasitic liver cirrhosis, clinical visible abdominal part distension, hypourocrinia, the abdominal part shifting dullness positive, two lower limbs edema, abnormal liver function, serum albumin is below 30g is several.B ultrasound shows: liver dwindles, portal vein diameter broadening, and spleen increases, and the ascites dark space is arranged.Or the x ray examination has right pleural effusion.Other situation is carried out by the clinical corresponding diagnostic criteria of this disease.
(2) Clinical types: (with reference to the 5th the national infectious disease meeting revision scheme in nineteen ninety-five Beijing)
Active liver cirrhosis: the clinical manifestation of chronic hepatitis still exists, particularly the transaminase increase, jaundice, albumin attenuating, the hardening of liver quality, splenomegaly, portal hypertension.The stability liver cirrhosis: have or do not have the liver medical history, the transaminase is normal, does not have obvious jaundice, splenomegaly companion portal hypertension, hypoalbuminemia.
(3) clinical stages: early stage: occur the two lower limbs edema of ascites for the first time, general situation is good, and without any diuretic treatment, albumin is between 28-30g is several.In, late period: show effect repeatedly more than 2 times, or ascites is through the diuretic therapy person that continues not disappear more than 2 months, albumin is below 25g/L.
Three, test case standard
1. include the case standard in: allly meet the above-mentioned differential diagnosis in tcm of distension disease diagnostic criteria person, all can include the test case in.
2. get rid of case standard (comprise inadaptation or reject case)
(1) syndrome differential diagnosis is indeterminate or the double person that holds the card under the arm arranged too much.(2) age is at under-18s, or the over-65s person, and trimester of pregnancy or women breast-feeding their children are to this medicine allergy sufferers.(3) merge important organs such as the heart, brain, kidney and hemopoietic system serious primary disease and psychotic are arranged.(4) be associated with primary peritonitis, primary hepatocarcinoma, or agnogenic courage and uprightness, milky ascites patient.(5) do not meet the standard of including in, not medication in accordance with regulations can't be judged that curative effect or data are not congruent to affect the treatment or safety judgement person.
Four, observation index
1. safety observation: general health check-up project.(2) blood, urine, just routine test.(3) heart, liver, kidney function test.
2. health giving quality is observed the situation of change of primary symptoms such as (1) abdominal part swells.(2) diet, two just waits the variation of situation.(3) sign, picture of the tongue, pulse condition and twenty-four-hour urine quantitative change situation.(4) B-type ultrasonography: liver, spleen, ascites situation of change.
Five, curative effect determinate standard: 1. produce effects: primary symptom disappears or alleviates more than (++), and light and heavy degree changes (+) into by (+++), or (++) disappear, and other symptoms, sign are clearly better or disappear, and the urine amount obviously increases.2. effective: primary symptom alleviates more than (+), and light and heavy degree changes (++) into by (+++), or (++) change (+) into, or (+) change (-), and other symptoms, sign take a turn for the better to some extent, and the urine amount increases.3. invalid: symptom, sign alleviate and do not reach above-mentioned standard person, or no change before the treatment, or do not increase the weight of the person to some extent.
Six, verification method: clinical verification adopts single at random blind method contrast principle to carry out, and MethodsThe cases enrolled is assigned as treatment group and matched group according to the prescription on individual diagnosis serial number by table of random number.1. treatment group: ascites pill (production of Hebei province Handan Pharmaceutical Co., Ltd), oral, each 10, every day 3 times.2. matched group: spironolactone, oral, each 40mg, every day 3 times.3. course of treatment: 1 week was a course of treatment, changed the healthy Spleen Nourishing Bolus of clothes after the course of treatment, and cooperation is lain up, and restriction water salt is taken in, and can be interrupted defeated albumin, with kind thereafter.
Seven, statistical procedures: checking result, various data all learn by statistics and handle, and measurement data is checked with t, enumeration data X
2Check, P＜0.05 is a significant difference.
Eight, checking result
1. clinical total effects: see Table 8
Table 8 liang group total effects relatively
| Group | The example number | Produce effects (%) | Effectively (%) | Invalid (%) | Total effective rate (%) |
| Treatment group matched group | 300 100 | 163(54.33) 34(34.0) | 111(37.0) 39(39.0) | 26(8.67) 27(27.0) | 274(91.33) 73(73.0) |
Two groups of total effectses are learned processing, X by statistics
2=25.4013, there is significant difference P＜0.01.
2. traditional Chinese medical science primary symptom changes before and after the treatment: see Table 9
Traditional Chinese medical science primary symptom situation of change relatively before and after the table 9 liang group treatment
| Group | The example number | Primary symptom | Before the treatment | After the treatment |
| Treatment group matched group | 300 100 | Slight slight (%) moderate (%) severe (%) of (%) moderate (%) severe (%) | 63(21.0) 166(55.33) 71(23.67) 22(22.0) 52(52.0) 26(26.0) | 189(63.0) 65(21.67) 25(8.33) 53(53.0) 27(27.0) 13(13.0) |
Before and after two groups of treatments traditional Chinese medical science primary symptom light, in, severe changes, learn by statistics and handle treatment group X
2=150.2018, P＜0.01; Matched group X
2=32.0581, group all there is significance P＜0.01, two.
3. accompanied symptoms and sign change before and after the treatment: see Table 10
Accompanied symptoms and sign change relatively before and after the table 10 liang group treatment
| Group | The example number | Accompanied symptoms and sign | Before the treatment | After the treatment |
| Treatment group matched group | 300 100 | Diet reduces edema stool abnormity oliguria diet and reduces edema stool abnormity oliguria | 260(86.67) 228(76.0) 147(49.0) 279(93.0) 87(87.0) 73(73.0) 50(50.0) 92(92.0) | 72(24.0) 57(19.0) 51(17.0) 27(9.0) 33(33.0) 30(30.0) 24(24.0) 27(27.0) |
Accompanied symptoms and sign change before and after two groups of treatments, learn by statistics and handle treatment group X
2=209.7011, P＜0.01 matched group X
2=44.2907, group all there is significance P＜0.01, two.
4. body weight, abdominal circumference, 24h urinate quantitative changeization before and after the treatment: see Table 11
Body weight before and after table 11 treatment, abdominal circumference, 24h urine quantitative changeization (x ± s)
| Group | The example number | Main physical signs | Before the treatment | After the treatment | The t value | The P value |
| Treatment group matched group | 300 100 | Body weight (kg) abdominal circumference (cm) urine amount (ml/24h) body weight (kg) abdominal circumference (cm) urine amount (ml/24h) | 71.96±3.62 106.39±7.85 539.68±86.9 70.88±3.79 103.8±8.21 532.78±89.3 | 62.55±4.04 92.22±4.49 1622±185.5 66.22±9.94 96.11±6.05 1149±221.5 | 3.16 3.81 6.49 2.19 2.06 4.14 | ＜0.01 ＜0.01 ＜0.01 ＜0.05 ＜0.05 ＜0.01 |
5, changes of liver function before and after the treatment: see Table 12
Changes of liver function before and after the table 12 liang group treatment (x ± s)
| Group | The example number | Main physical signs | Before the treatment | After the treatment | The t value | The P value |
| Treatment group matched group | 300 100 | ALT(IU/L) TBIL( UMol/L) A (albumin) (g/L) ALT (IU/L) TBIL ( UMol/L) A (albumin) (g/L) | 87.29±2.61 47.03±1.66 26.28±1.34 83.33±2.81 43.94±2.01 26.17±1.43 | 69.91±3.07 26.39±2.09 35.77±1.56 76.56±2.49 37.09±2.26 31.26±1.02 | 2.85 3.62 2.74 2.14 2.39 2.07 | ＜0.01 ＜0.01 ＜0.01 ＜0.05 ＜0.05 ＜0.05 |
Nine, checking is summed up: by to ascites pill 300 routine clinical observations, confirm that this medical instrument has the effect of inducing diuresis to remove edema, dehumidifying spleen invigorating 1..The clinical diseases such as distension disease, distension and fullness of the chest and abdomen, extremity edema, constipation, oliguria with reddish urine that are applicable to.By clinical observation, two groups aspect curative effect, treatment group obvious effective rate and total effective rate are respectively 54.33% and 91.33%, obviously are better than matched group 34.0% and 73.0%, learn handling by statistics all has significant difference (P＜0.01).2. ascites pill can obviously improve cirrhotic ascites patient's symptoms such as abdominal distention, edema, oliguria, stool abnormity, and the urine amount increases after patient's medication, and ascites disappears gradually, and abdominal circumference diminishes, and loses weight, and liver function and each main symptom and accompanied symptoms all have improvement.Two groups of each change of illness state of comparison all obviously are better than taking the matched group patient of spironolactone.The patient of clinical observation all through the necessary security physico-chemical examination, the result does not see any unusual before and after the medication.The patient does not also find serious toxic and side effects and untoward reaction after period in a medicine and medication.
The following example all can be realized the effect of above-mentioned experimental example.
Embodiment 1 pill
Melanteritum (vinegar system) 200g Radix Kansui 20g Fructus Jujubae (enucleation stir-fry) 200g
Radix Aucklandiae 20g Semen Tritici aestivi (stir-fry) 100g
The above five tastes are ground into fine powder, sieve mixing; Close the pill that sticks together with hot water, dry below 60 ℃, sugar coating, that is, and per 10 heavy 1.3g.Taking medicine before meal, one time 10,3 times on the one, the child is cut down according to the circumstance.Can not obey together with Radix Glycyrrhizae, avoid Sal and Fagopyrum esculentum Moench.
Embodiment 2 capsules
Melanteritum 230g Radix Kansui 23g Fructus Jujubae 180g
Radix Aucklandiae 23g Semen Tritici aestivi 80g
The capsule method for making: the above five tastes, be ground into fine powder, sieve mixing; Promptly encapsulated, every heavy 0.4g.Taking medicine before meal, one time 3,3 times on the one, the child is cut down according to the circumstance.Can not obey together with Radix Glycyrrhizae, avoid Sal and Fagopyrum esculentum Moench.
Embodiment 3 granules
Melanteritum 180g Radix Kansui 18g Fructus Jujubae 230g
Radix Aucklandiae 18g Semen Tritici aestivi 120g
The granule method for making: the above five tastes, decocting boil 2 times, filter, and merging filtrate is condensed into cream, add adjuvant, and mixing is granulated, and drying is packed promptly every bag of 3-5g.Taking medicine before meal usefulness, one time 1 bag, 3 times on the one, the child is cut down according to the circumstance.Can not obey together with Radix Glycyrrhizae, avoid Sal and Fagopyrum esculentum Moench.
The discriminating method of quality control of embodiment 4 pills
A. get this product 1g, remove sugar-coat, porphyrize adds water 10ml, boils 10 minutes, filters, and gets filtrate 1ml, adds iron potassuim cyanide test liquid 2-3 and drips, and promptly generates blue precipitation, separates, and is deposited in the dilute hydrochloric acid and does not dissolve, and hydro-oxidation sodium test solution is brown precipitate;
B. get this product 15g, porphyrize adds 60-90 ℃ of petroleum ether 50ml, floods 30 minutes, and supersound process 30 minutes filters, and filtrate volatilizes, and residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets Radix Aucklandiae control medicinal material 0.5g, adds ethyl acetate 10ml, and supersound process 30 minutes filters, and filtrate is medical material solution in contrast; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with 10: 1 cyclohexane extraction one acetone was developing solvent, launch, taking-up is dried, and spray is with 10% ethanol solution of sulfuric acid, and is moistening fully to the plate face; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
C. get this product 20g, porphyrize adds ethanol 60ml, and reflux 1 hour filters, and filtrate evaporate to dryness, residue add water 30ml makes dissolving, uses ethyl acetate extraction three times, and each 20ml merges ethyl acetate liquid, and evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Kansui control medicinal material 2g, adds ethanol 40ml, and reflux 1 hour filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, in contrast medical material solution; Test according to thin layer chromatography (appendix V1B of middle traditional Chinese medicines version in 2000), draw need testing solution 10 μ l, control medicinal material solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent with the carboxymethyl cellulose sodium, with 20: 2: 1 chloroform-ethyl acetate-formic acid was developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
Claims (11)
1, a kind of method of quality control of pharmaceutical composition is characterized in that the discrimination method in this method comprises following discriminating:
A. get this composite preparation 15g, porphyrize adds 60-90 ℃ of petroleum ether 50ml, flooded 25-35 minute, and supersound process 25-35 minute, filter, filtrate volatilizes, and residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets Radix Aucklandiae control medicinal material 0.5g, adds ethyl acetate 10ml, and supersound process 25-35 minute, filter, filtrate is medical material solution in contrast; According to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with 8-12: 0.5-1.5 cyclohexane extraction-acetone is developing solvent, launches, and taking-up is dried, spray is with 10% ethanol solution of sulfuric acid, and is moistening fully to the plate face; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
B. get this composite preparation 20g, porphyrize adds ethanol 60ml, reflux 0.5-2 hour, filters, filtrate evaporate to dryness, residue add water 30ml makes dissolving, uses ethyl acetate extraction three times, each 20ml, merge ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Kansui control medicinal material 2g, adds ethanol 40ml, and reflux 1 hour filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, in contrast medical material solution; Test according to thin layer chromatography, draw need testing solution 10 μ l, control medicinal material solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent with the carboxymethyl cellulose sodium, with 18-25: 1-3: 1.5-1.5 chloroform-ethyl acetate-formic acid is developing solvent, launch, take out, dry, put under the ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
Wherein the preparation of pharmaceutical composition is by Melanteritum 150-250 weight portion, Radix Kansui 15-25 weight portion, Fructus Jujubae 150-250 weight portion, Radix Aucklandiae 15-25 weight portion and Semen Tritici aestivi 60-130 weight portion add excipient and make pill, tablet, oral liquid, capsule or granule.
2, the method for quality control of pharmaceutical composition as claimed in claim 1 is characterized in that this method also comprises following discrimination method:
Get this composite preparation 1g, porphyrize adds water 10ml, boils 8-12 minute, filters, and gets filtrate 1ml, adds iron potassuim cyanide test liquid 2-3 and drips, and promptly generates blue precipitation, separates, and is deposited in the dilute hydrochloric acid and does not dissolve, and hydro-oxidation sodium test solution is brown precipitate.
3, the method for quality control of pharmaceutical composition as claimed in claim 1 is characterized in that the discrimination method that is used for pill in this method comprises following discriminating:
A. get pill 15g, porphyrize adds 60--90 ℃ of petroleum ether 50ml, floods 30 minutes, and supersound process 30 minutes filters, and filtrate volatilizes, and residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets Radix Aucklandiae control medicinal material 0.5g, adds ethyl acetate 10ml, and supersound process 30 minutes filters, and filtrate is medical material solution in contrast; According to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with 10: 1 cyclohexane extraction-acetone was developing solvent, launched, and taking-up is dried, spray is with 10% ethanol solution of sulfuric acid, and is moistening fully to the plate face; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
B. get pill 20g, porphyrize adds ethanol 60ml, and reflux 1 hour filters, and filtrate evaporate to dryness, residue add water 30ml makes dissolving, uses ethyl acetate extraction three times, and each 20ml merges ethyl acetate liquid, and evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Kansui control medicinal material 2g, adds ethanol 40ml, and reflux 1 hour filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, in contrast medical material solution; Test according to thin layer chromatography, draw need testing solution 10 μ l, control medicinal material solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent with the carboxymethyl cellulose sodium, with 20: 2: 1 chloroform-ethyl acetate-formic acid was developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
4, the method for quality control of pharmaceutical composition as claimed in claim 3 is characterized in that the discrimination method that is used for pill in this method also comprises following discrimination method:
Get pill 1g, remove sugar-coat, porphyrize adds water 10ml, boils 10 minutes, filters, and gets filtrate 1ml, adds iron potassuim cyanide test liquid 2-3 and drips, and promptly generates blue precipitation, separates, and is deposited in the dilute hydrochloric acid and does not dissolve, and hydro-oxidation sodium test solution is brown precipitate.
5, as the method for quality control of claim 1,2,3 or 4 described pharmaceutical compositions, it is characterized in that wherein drug combination preparation is made by following raw material medicaments:
Melanteritum 230 weight portion Radix Kansuis 23 weight portion Fructus Jujubaes 180 weight portions
The Radix Aucklandiae 23 weight portion Semen Tritici aestivis 80 weight portions.
6, as the method for quality control of claim 1,2,3 or 4 described pharmaceutical compositions, it is characterized in that wherein drug combination preparation is made by following raw material medicaments:
Melanteritum 180 weight portion Radix Kansuis 18 weight portion Fructus Jujubaes 230 weight portions
The Radix Aucklandiae 18 weight portion Semen Tritici aestivis 120 weight portions.
7, as the method for quality control of claim 1,2,3 or 4 described pharmaceutical compositions, it is characterized in that wherein drug combination preparation is made by following raw material medicaments:
Melanteritum 200 weight portion Radix Kansuis 20 weight portion Fructus Jujubaes 200 weight portions
The Radix Aucklandiae 20 weight portion Semen Tritici aestivis 100 weight portions.
8, the method for quality control of pharmaceutical composition as claimed in claim 5 is characterized in that wherein Melanteritum is given birth to usefulness in this drug combination preparation, and Removing Kernel for Date is fried, and Semen Tritici aestivi is for frying Semen Tritici aestivi.
9, the method for quality control of pharmaceutical composition as claimed in claim 6 is characterized in that wherein Melanteritum is given birth to usefulness in this drug combination preparation, and Removing Kernel for Date is fried, and Semen Tritici aestivi is for frying Semen Tritici aestivi.
10, the method for quality control of pharmaceutical composition as claimed in claim 7 is characterized in that wherein Melanteritum is given birth to usefulness in this drug combination preparation, and Removing Kernel for Date is fried, and Semen Tritici aestivi is for frying Semen Tritici aestivi.
11,, it is characterized in that five tastes crude drug in this drug combination preparation wherein through being ground into fine powder, sieves mixing as the method for quality control of claim 8,9 or 10 described pharmaceutical compositions; Close the pill that sticks together with hot water, dry below 60-70 ℃, excipient direct through conventional operation at last or that adding is pharmaceutically accepted is made pill, tablet, oral liquid, capsule or granule.
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| CN101406654B (en) * | 2007-10-12 | 2011-04-13 | 王学岭 | Oral liquid for treating hoove |
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| CN102305840B (en) * | 2008-01-21 | 2014-01-22 | 邯郸摩罗丹药业股份有限公司 | Hoove pill and quality standard and test method for preparation of hoove pill |
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| CN105749017A (en) * | 2016-04-28 | 2016-07-13 | 邯郸制药股份有限公司 | Traditional Chinese medicine composition for treating hoove and preparation of traditional Chinese medicine composition |
| CN105749018A (en) * | 2016-04-28 | 2016-07-13 | 邯郸制药股份有限公司 | Traditional Chinese medicine composition for treating hoove and preparation of traditional Chinese medicine composition |
| CN105920390A (en) * | 2016-04-28 | 2016-09-07 | 邯郸制药股份有限公司 | Traditional Chinese medicinal composition for treating hoove and preparation of traditional Chinese medicinal composition |
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| CN105770567A (en) * | 2016-04-28 | 2016-07-20 | 邯郸制药股份有限公司 | Traditional Chinese medicine composition for treating hoove and preparation thereof |
| CN105749020A (en) * | 2016-04-28 | 2016-07-13 | 邯郸制药股份有限公司 | Traditional Chinese medicine composition for treating hoove and preparation of traditional Chinese medicine composition |
| CN105796976A (en) * | 2016-04-28 | 2016-07-27 | 邯郸制药股份有限公司 | Traditional Chinese medicine composition and preparation capable of treating hoove |
| CN105749019A (en) * | 2016-04-28 | 2016-07-13 | 邯郸制药股份有限公司 | Traditional Chinese medicine composition for treating hoove and preparation of traditional Chinese medicine composition |
| CN105770566A (en) * | 2016-04-28 | 2016-07-20 | 邯郸制药股份有限公司 | Traditional Chinese medicine composition for treating hoove and preparation thereof |
| CN105920389A (en) * | 2016-04-28 | 2016-09-07 | 邯郸制药股份有限公司 | Traditional Chinese medicinal composition for treating hoove and preparation of traditional Chinese medicinal composition |
| CN105796975A (en) * | 2016-04-28 | 2016-07-27 | 邯郸制药股份有限公司 | Traditional Chinese medicine composition capable of treating hoove |
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| CI01 | Publication of corrected invention patent application |
Correction item: Denomination of Invention Correct: The quality control method of a traditional Chinese medicine composition for treating Hoove. False: Quality control method of traditional Chinese medicine composition for treating swelling disease Number: 45 Page: 926 Volume: 22 |
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| CI03 | Correction of invention patent |
Correction item: Denomination of Invention Correct: The quality control method of a traditional Chinese medicine composition for treating Hoove. False: Quality control method of traditional Chinese medicine composition for treating swelling disease Number: 45 Page: The title page Volume: 22 |
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| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTION NAME; FROM: QUALITY CONTROLLING MEANS OF A CHINESE MEDICINAL COMPOSITION FOR THE TREATMENT OF SWELLING DISEASE TO: A QUALITY CONTROL METHOD OF A CHINESE MEDICINAL COMPOSITION CURING TYMPANITES |
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Free format text: CORRECT: INVENTION NAME; FROM: QUALITY CONTROLLING MEANS OF A CHINESE MEDICINAL COMPOSITION FOR THE TREATMENT OF SWELLING DISEASE TO: A QUALITY CONTROL METHOD OF A CHINESE MEDICINAL COMPOSITION CURING TYMPANITES |
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Owner name: HANDAN MOLUODAN PHARMACEUTICAL CO., LTD. Free format text: FORMER NAME: HANDAN PHARMACEUTICAL CO., LTD. |
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Address after: 056005 No. 309 National Road, Handan Hebei Industrial Park, No. 18 Patentee after: HANDAN MOLUODAN PHARMACEUTICAL Co.,Ltd. Address before: 056001 No. 321 Heping Road, Hebei, Handan Patentee before: HANDAN PHARMACEUTICAL Co.,Ltd. |
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Owner name: HANDAN PHARMACY CO., LTD. Free format text: FORMER NAME: HANDAN MOLUODAN PHARMACEUTICAL CO., LTD. |
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Address after: 056005 No. 309 National Road, Handan Hebei Industrial Park, No. 18 Patentee after: HANDAN PHARMACEUTICAL Co.,Ltd. Address before: 056005 No. 309 National Road, Handan Hebei Industrial Park, No. 18 Patentee before: HANDAN MOLUODAN PHARMACEUTICAL Co.,Ltd. |
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