CN101843670B - Chinese medicinal composition for clearing heat and detoxicating, promoting urination and treating stranguria - Google Patents
Chinese medicinal composition for clearing heat and detoxicating, promoting urination and treating stranguria Download PDFInfo
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- CN101843670B CN101843670B CN200910080667A CN200910080667A CN101843670B CN 101843670 B CN101843670 B CN 101843670B CN 200910080667 A CN200910080667 A CN 200910080667A CN 200910080667 A CN200910080667 A CN 200910080667A CN 101843670 B CN101843670 B CN 101843670B
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Abstract
The invention discloses a Chinese medicinal composition preparation for clearing heat and detoxicating, promoting urination and treating stranguria. The composition is prepared by decocting polygonum capitatum and plantain herb with water for three times, one hour for every time; combining and filtering the decoction, concentrating the filtrate to obtain clear paste; cooling the paste, adding ethanol and uniformly stirring the paste and the ethanol; standing the mixture for 24 hours, and recycling the ethanol from the supernatant; adding an appropriate amount of cane sugar and sorbic acid to prepare oral liquid. The composition preparation has good effects of clearing heat and detoxicating, promoting urination and treating stranguria.
Description
Technical field:
The present invention relates to a kind of Chinese medicine composition and method for preparing, particularly a kind of heat-clearing and toxic substances removing, the Chinese medicine composition of inducing diuresis for treating stranguria syndrome and method for preparing.
Background technology:
Urinary system infection is the urinary system common disease, and in the crowd of age groups, the sickness rate of urinary system infection is different.See with the boy in the neonate that women's infection rate is higher than the male far away among teenager and the adult crowd more.As far as the women, every increase of age 10 years old, infection rate just increases by 1%, can reach 10% during to 65 years old.There is 50% women to get a urinary tract infection to I haven't seen you for ages in life.In the elderly population, masculinity and femininity no matter, urinary tract infection all is a major issue.The old people suffers from urinary tract disease (like hyperplasia of prostate, neurogenic bladder and catheter use etc.) and increases, and can cause the complexity urinary system infection.Repeatedly recurrence appears in regular meeting after the first time, urinary tract infection took place.Perspective study to 179 routine cystitis women shows that 44% patient had once recurrence at least in 12 months, and wherein the pathogenic bacterium of 33% recurrent infection are consistent with the serotype of the pathogenic bacterium of primary infection.Although the recurrence of most urinary system infections comes from the infection again of new bacterial strain, the infection again of hiding with same bacterial strain after the treatment of primary infection pathogen also is shown in considerable patient.But should disease after treatment, clinical symptoms often obtains rapidly well then out in the coldly treats completely.Be prone to cause vicious cycle because of repeatedly treating and showing effect repeatedly, thereby form the chronic and prolonged state of an illness that do not heal.
This sick origin cause of formation also is subject to many factor affecting except the factor of bacterial infection, like the resistance of human body or immunoreation etc.Traditional medicine one thinks that to advocating wholistic therapy chronic urinary system infection belongs to the deficiency and excess accompanied symptoms type of " hinder just, heresy is still real " more; It is insufficiency of the spleen that its pathogenesis is mainly endogenous cause of ill, and healthy energy is not solid, and the diseases caused by exogenous pathogenic factor damp-heat virus is fallen ill; So that insufficiency of the spleen water is wet makes a bet and the damp-heat accumulation part of the body cavity below the umbilicus, housing the bladder, kidneys and bowels; Cause the imbalance of kidney and bladder function and fall ill, belong to the stranguria category of the traditional Chinese medical science, so need clearing away heat-damp and promoting diuresis and set upright the Therapeutic Method of laying equal stress on.
The present invention adopts clearing away heat-damp and promoting diuresis, spleen benefiting and strengthen kidney, clinically chronic urinary system infection or acute attack (urethritis, cystitis, pyelonephritis) is had splendid effect.
Summary of the invention:
First purpose of the present invention is to provide a kind of heat-clearing and toxic substances removing, the Chinese medicine composition of inducing diuresis for treating stranguria syndrome; Second purpose of the present invention is to provide the method for preparing of this Chinese medicinal composition preparation; The 3rd purpose of the present invention is to provide the quality determining method of this Chinese medicinal composition preparation.
The present invention seeks to realize through following technical scheme:
A kind of heat-clearing and toxic substances removing of the present invention, the raw material of the Chinese medicinal composition preparation of inducing diuresis for treating stranguria syndrome consists of:
Herba Polygoni Capitati 450-640 weight portion, Herba Plantaginis 200-300 weight portion.
Herba Polygoni Capitati is dry herb or the aerial parts of polygonaceae plant Herba Polygoni Capitati Polygonum capitatun Buch.-Ham.ex D.Don.Spring, summer, Qiu Sanji gather, using fresh herb or dry.
Herba Plantaginis is the dry herb of Plantaginaceae plant Herba Plantaginis Plantago asiatica L. or Plantago depressa Willd Plantago depressaWilld..Excavate summer, removes silt, dries.
A kind of heat-clearing and toxic substances removing of the present invention, the raw material composition of the Chinese medicinal composition preparation of inducing diuresis for treating stranguria syndrome is preferably:
Herba Polygoni Capitati 540 weight portions, Herba Plantaginis 260 weight portions.
A kind of heat-clearing and toxic substances removing of the present invention; The method for preparing of the Chinese medicinal composition preparation of inducing diuresis for treating stranguria syndrome is: two flavor medical materials, decocte with water 1-5 time, each 0.5-3 hour; Collecting decoction; Filter, filtrating concentrates, according to common process; Process clinical or pharmaceutically acceptable dosage form, include but not limited to tablet, capsule, powder, soft capsule, drop pill, honeyed pill, pill, granule, soft extract with bee honey agent, slow releasing preparation, quick releasing formulation, controlled release preparation, oral liquid, ejection preparation or external preparation.
A kind of heat-clearing and toxic substances removing of the present invention, the method for preparing of the Chinese medicine composition oral liquid of inducing diuresis for treating stranguria syndrome is preferably: two flavor medical materials, decocte with water three times, each 1 hour, collecting decoction; Filter, filtrating is concentrated into the clear paste that relative density is 1.10～1.15 (50 ℃), puts coldly, adds ethanol and makes and contain the alcohol amount and reach 50%; Stir, left standstill 24 hours, get supernatant and reclaim ethanol, add an amount of sucrose, sorbic acid; Add water adjustment total amount to 1000 parts by volume, stir, fill promptly gets; Said weight portion/parts by volume is corresponding with g/ml.
A kind of heat-clearing and toxic substances removing of the present invention, the method for preparing of the Chinese medicinal composition granules of inducing diuresis for treating stranguria syndrome is preferably: above two flavor medical materials, decocting three times, each 1 hour; Collecting decoction filters, and filtrating is concentrated into the clear paste that relative density is 1.10～1.15 (50 ℃), puts cold; Add ethanol and make and contain alcohol amount and reach 50%, stir, left standstill 24 hours, getting supernatant concentration to relative density is the thick paste of 1.35～1.40 (50 ℃); Add proper auxiliary materials, process granule, drying promptly gets.
A kind of heat-clearing and toxic substances removing of the present invention, the method for preparing of the Chinese medicinal composition capsules agent of inducing diuresis for treating stranguria syndrome is preferably: above two flavor medical materials, decocting three times, each 1 hour, collecting decoction; Filter, filtrating is concentrated into the clear paste that relative density is 1.10～1.15 (50 ℃), puts coldly, adds ethanol and makes and contain the alcohol amount and reach 50%; Stir, left standstill 24 hours, getting supernatant concentration to relative density is the thick paste of 1.35～1.40 (50 ℃), adds proper auxiliary materials; Process granule, drying, encapsulated, promptly get.
The present invention provides the method for quality control of this Chinese medicinal composition preparation, and the method comprising the steps of:
A, discriminating: get this Chinese medicine composition oral liquid formulations 5-50ml, extract 1-3 time, each 15-30ml with petroleum ether (60-90 ℃) jolting; Discard petroleum ether liquid; The jolting of water liquid reuse ethyl acetate is extracted 1-3 time, each 10-40ml, combined ethyl acetate liquid; Evaporate to dryness, residue add methanol 1ml makes dissolving as need testing solution; Other gets Herba Polygoni Capitati control medicinal material 0.5-5g, adds water 20-100ml and decocts 15-45 minute, filters, and filtrating is concentrated into 10-40ml, extracts 1-3 time with the ethyl acetate jolting, shines medical material solution in pairs with legal system; Drawing each 2-10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with cyclohexane extraction-acetone-formic acid mixed solvent of 3-5: 5-8: 0.4-0.7; Launch, take out, dry; Spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to the speckle colour developing clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
B, discriminating: the preparation of need testing solution: get this Chinese medicine composition oral liquid formulations 5-50ml, extract 1-3 time, each 15-30ml with petroleum ether (60-90 ℃) jolting; Discard petroleum ether liquid; The jolting of water liquid reuse ethyl acetate is extracted 1-3 time, each 10-40ml, combined ethyl acetate liquid; Evaporate to dryness, residue add methanol 1ml makes dissolving as need testing solution; Other gets Herba Plantaginis control medicinal material 0.5-5g and adds water 60-140ml decoction 15-45 minute, filters, and filtrating is concentrated into 10-40ml; Extract 1-3 time each 10-40ml, combined ethyl acetate liquid with the ethyl acetate jolting; Evaporate to dryness, residue add methanol 1ml as control medicinal material solution; Draw each 2-8 μ l of above-mentioned two kinds of solution, put respectively on same silica gel H lamellae, with 5-8: 3-6: cyclohexane extraction-acetone of 0.2-formic acid mixed solvent is developing solvent; Launch, take out, dry; Spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to the speckle colour developing clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
C, extract content measure: precision is measured this Chinese medicine composition oral liquid formulations 5-20ml, puts in the evaporating dish that is dried to constant weight, behind water bath method, in 105 ℃ of dryings 3 hours, puts in the exsiccator cooling 30 minutes, accurately rapidly claims to decide weight; Extract content must not be lower than 4.0%.
Preferably include following differential method in the above-mentioned quality determining method:
The Herba Polygoni Capitati thin layer is differentiated: get Chinese medicinal composition preparation 20ml, extract 2 times with petroleum ether (60-90 ℃) jolting, each 20ml; Discard petroleum ether liquid; The jolting of water liquid reuse ethyl acetate is extracted 2 times, each 20ml, combined ethyl acetate liquid; Evaporate to dryness, residue add methanol 1ml makes dissolving as need testing solution; Other gets Herba Polygoni Capitati control medicinal material 1g, adds water 50ml and decocts 30 minutes, filters, and filtrating is concentrated into 20ml, extracts 2 times with the ethyl acetate jolting, shines medical material solution in pairs with legal system; Drawing each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with cyclohexane extraction-acetone of 4: 6: 0.5-formic acid, launches, and takes out, and dries, and spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to the speckle colour developing clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
The Herba Plantaginis thin layer is differentiated: the preparation of need testing solution: with the method for preparing of differentiating need testing solution under the A item; Other gets Herba Plantaginis control medicinal material 1g and adds water 100ml decoction 30 minutes, filters, and filtrating is concentrated into 20ml, extracts 2 times with the ethyl acetate jolting, each 20ml, and combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml as control medicinal material solution; Drawing each 4 μ l of above-mentioned two kinds of solution, put respectively on same silica gel H lamellae, be developing solvent with cyclohexane extraction-acetone-formic acid (6: 4: 0.2), launches, and takes out, and dries, and spray is with 10% ethanol solution of sulfuric acid, 105 ℃ be heated to speckle develop the color clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
Extract content is measured: precision is measured Chinese medicinal composition preparation 10ml, puts in the evaporating dish that is dried to constant weight, behind water bath method, in 105 ℃ of dryings 3 hours, puts in the exsiccator cooling 30 minutes, accurately rapidly claims to decide weight; Extract content must not be lower than 4.0%.
The said Chinese medicinal composition preparation of above-mentioned quality determining method is: Herba Polygoni Capitati 540g, Herba Plantaginis 260g, decocte with water three times, each 1 hour, collecting decoction; Filter, filtrating is concentrated into the clear paste that relative density is 1.10～1.15 (50 ℃), puts coldly, adds ethanol and makes and contain the alcohol amount and reach 50%; Stir, left standstill 24 hours, get supernatant and reclaim ethanol, add an amount of sucrose, sorbic acid; Add water adjustment total amount to 1000ml, stir, fill promptly gets.
The present invention has good heat-clearing and toxic substances removing, and diuresis inducing function has obvious inhibitory action to the mice foot swelling, has tangible antiinflammatory action, can obviously increase the mouse retention amount and obviously promote K in the urine
+, Na
+Discharge.
The quality determining method of the Chinese medicinal composition preparation that the present invention is a kind of; Warp experiment proof: content assaying method of the present invention detects good, the stable height of specificity, favorable reproducibility, precision height; Be fit to industrialized production more, really guaranteed safety of clinical administration, effective, reliable.
Following experimental example and embodiment are used to further specify but are not limited to the present invention.
The preparation that all experimental examples of the present invention are selected for use is the tablet of the present invention that makes according to the embodiment of the invention 1, but experimental result of the present invention is not limited in this tablet.
Experimental example 1: pharmacodynamic experiment
1, experiment material:
Medicine and reagent: the Chinese medicinal composition preparation oral liquid, irritate stomach (ig) amount and be 3.5g crude drug/kg group, 7.0g crude drug/kg group, 14g crude drug/kg group, prednisoni acetas 5mg/ sheet, hydrochlorothiazide 25mg/ sheet.
Animal: Kunming kind white mice.
2, experimental technique:
2.1 influence to the foot swelling of Ovum Gallus domesticus album induced mice:
Get 50 of mices, body weight 25 ± 5g, complete male.Be divided into 5 groups at random by body weight, 10 every group, grouping and dosage are seen table 1.Every day, the ig administration was 1 time, continuous 4 times.30min after the last administration, the right foot of every Mus injects 20% Ovum Gallus domesticus album 30ul and causes inflammation, behind the 1h under ankle joint 0.5mm cut at place pair metapedes and weigh, be foot swelling degree (mg) with left and right sides heavy sensation in the foot difference.
2.2 the influence of on Carrageenan induced mice foot swelling:
Get 50 of mices, body weight 25 ± 5g, complete male.Be divided into 5 groups at random by body weight, 10 every group, grouping and dosage are seen table 1.Every day, the ig administration was 1 time, continuous 4 times.30min after the last administration, the right foot of every Mus injects 1% carrageenin 30ul and causes inflammation, behind the 3.5h under ankle joint 0.5mm cut at place pair metapedes and weigh, be foot swelling degree (mg) with left and right sides heavy sensation in the foot difference.
2.3 to K in mouse retention amount and the urine
+, Na
+, Cl
-The influence of content:
Get complete male mice, body weight 40 ± 10g, routine feeding is freely drunk water.The urine amount in the 2h chosen reaches 50 of the mices 40% or more of the amount of pouring into, and grouping and dosage are seen table 2.16～18h is prohibited in test ig administration the previous day 1 time, freely drinks water.1 mice is got in test at every turn, gently presses the thing lower abdomen and drains surplus urine, loads by the 0.4ml/10gip normal saline, then ig administration or 0.5%CMC-Na contrast liquid.At random animal is placed simple and easy metabolic cage, every cage is put 1 mice, collects the 4h total volume of urine, and urine amount and the urine amount of obtaining the every 10g body weight of mice increase percentage rate %.0 ℃ of preservation of collection urine airtight back refrigerator is dissolved urine before measuring in 37 ℃ of water-baths, shake up the back sampling and dilute 10 times with deionized water.Adopt electrolyte analyser to measure K in the urine
+, Na
+, Cl
-Content is obtained K in the urine
+, Na
+, Cl
-Output.
3, result
3.1 influence to Ovum Gallus domesticus album, the foot swelling of carrageenin induced mice
Visible by table 1, Chinese medicinal composition preparation administration group all can obviously be resisted the foot swelling of Ovum Gallus domesticus album induced mice, with model control group significant difference P＜0.01-0.001 is arranged relatively.Chinese medicinal composition preparation can obviously be resisted the foot swelling of carrageenin induced mice, with model control group significant difference P＜0.05 is arranged relatively.The prednisone group also can obviously suppress Ovum Gallus domesticus album, carrageenin induced mice foot swelling degree (P＜0.01-0.001).
Table 1 Chinese medicinal composition preparation to the influence of Ovum Gallus domesticus album, the foot swelling of carrageenin induced mice (x ± s, n=10)
Annotate: compare with model:
*P＜0.05,
*P＜0.01,
* *P＜0.001
3.2 to K in mouse retention amount and the urine
+, Na
+, Cl
-The influence of content
By shown in the table 2, Chinese medicinal composition preparation group and hydrochlorothiazide group mouse retention amount have obvious increase, with matched group significant difference (P＜0.05-0.01) are arranged relatively.
Visible from table 3, K in the Chinese medicinal composition preparation group mouse retention
+Output, all obviously increase, and with the normal control group significant difference P＜0.01 arranged more all.Chinese medicinal composition preparation group and hydrochlorothiazide group then can obviously promote Na in the mouse retention
+Discharge, with matched group significant difference P＜0.05-0.01 is arranged more all.Cl in each administration group urine
-, all there is increase trend P＞0.05 output.
Foot swelling has obvious inhibitory action to Chinese medicinal composition preparation to the Ovum Gallus domesticus album induced mice, can obviously increase the mouse retention amount and obviously promote K in the urine
+, Na
+Discharge.This result of the test shows: Chinese medicinal composition preparation have antiinflammatory, diuresis wherein diuresis maybe with promote K in the urine
+, Na
+, Cl
-Discharge relevant.
Experimental example 2: Herba Polygoni Capitati thin layer discrimination test
This Chinese medicinal composition preparation complicated component, the present invention utilizes thin layer chromatography to identify Herba Polygoni Capitati medical material in the preparation.
1, the selection of thin layer chromatography:
Common thin layer chromatography has silica gel thin-layer chromatography, ply of paper to analyse etc.Mostly composition is flavones ingredient in the Herba Polygoni Capitati, and middle polarity selects silica gel column chromatography to make an experiment.
2, the preparation of test sample:
2.1 the enrichment of Herba Polygoni Capitati effective ingredient, purification:
Use the stage extraction method that the Herba Polygoni Capitati composition in the preparation is carried out enrichment, purification.
Get Chinese medicinal composition preparation 20ml, extract 2 times with petroleum ether (60-90 ℃) jolting, each 20ml discards petroleum ether liquid, merges petroleum ether liquid, and evaporate to dryness, residue add methanol 1ml makes dissolving as need testing solution 1.
The surplus water liquid reuse ethyl acetate jolting of need testing solution 1 collection is extracted 2 times, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving as need testing solution 2.
The surplus water liquid reuse n-butyl alcohol jolting of need testing solution 2 collections is extracted 2 times, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving as need testing solution 3.
Get Herba Polygoni Capitati control medicinal material 1g, add water 50ml and decocted 30 minutes, filter, filtrating is concentrated into 20ml, produces control medicinal material solution 1,2,3 respectively by the test sample extracting process.
Drawing each 5 μ l of above-mentioned solution, o'clock on three silica gel g thin-layer plates, be developing solvent with cyclohexane extraction-acetone-formic acid (4: 6: 0.5) respectively, launches, and takes out, and dries, and spray is with 10% ethanol solution of sulfuric acid, 105 ℃ be heated to speckle develop the color clear.
Experimental result is following:
Do not observe obvious speckle in control medicinal material solution 1 chromatograph.
In control medicinal material solution 2 chromatographs obvious speckle is arranged, and clear spot.
Do not observe obvious speckle in control medicinal material solution 3 chromatographs.
In need testing solution 1 chromatograph with control medicinal material solution 2 chromatograph relevant positions on do not observe obvious speckle.
In need testing solution 2 chromatographs with control medicinal material solution 2 chromatograph relevant positions on, the speckle of same color is arranged, clear spot, the plate face is clean and tidy.
In need testing solution 3 chromatographs with control medicinal material solution 3 chromatograph relevant positions on do not observe obvious speckle.Therefore use need testing solution 2 and control medicinal material solution 2 method for preparinies to prepare need testing solution and control medicinal material solution.
2.2 the test sample method for preparing is preferred:
(1), the method for removing of low polar impurity is preferred:
3 factors utilizing orthogonal test that low polar impurity is removed in influence are investigated, and are respectively solvent species, extractant amount, extraction times, and each factor is established 3 levels, EXPERIMENTAL DESIGN such as table 4:
Table 4
By orthogonal table L9 (3
4) experiment arrangement.Experimental technique such as table 5:
Table 5
After removing in the preparation low composition impurity through above experiment, water liquid extracts 2 times with the ethyl acetate jolting, 20ml at every turn, and combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving as need testing solution.Prepare 9 parts of need testing solutions altogether through above test.
Get Herba Polygoni Capitati control medicinal material 1g, add water 50ml and decocted 30 minutes, filter, filtrating is concentrated into 20ml, extracts 2 times with the ethyl acetate jolting, processes control medicinal material solution.
Drawing each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, be developing solvent with cyclohexane extraction-acetone-formic acid (4: 6: 0.5), launches, and takes out, and dries, and spray is with 10% ethanol solution of sulfuric acid, 105 ℃ be heated to speckle develop the color clear.
Result of the test shows:
Adopt in the test sample chromatograph of petroleum ether (60-90 ℃) remove impurity, with control medicinal material chromatograph relevant position, show the speckle of same color, clear spot, the plate face is clean and tidy, free from admixture disturbs.
When adopting benzene, dichloromethane remove impurity, in the need testing solution chromatograph with control medicinal material chromatograph relevant position on, spot colors is used in the need testing solution chromatograph of petroleum ether (60-90 ℃) remove impurity a little less than the spot colors.
Do not use solvent-extracted sample (extraction times is 0), need testing solution is denseer thick, the point sample difficulty, and impurity is many in the chromatograph, disturbs Herba Polygoni Capitati to differentiate.
Confirm to select for use petroleum ether (60-90 ℃) remove impurity.
The best practice of removing low polar impurity in the preparation is: get this Chinese medicinal composition preparation oral liquid 20ml, extract 2 times with petroleum ether (60-90 ℃) jolting, each 20ml discards petroleum ether liquid.
(2), the investigation of Semi-polarity section enrichment composition:
Herba Polygoni Capitati becomes 3 factors of separating/enriching to investigate in the preparation to influencing to utilize orthogonal test, is respectively solvent species, extractant amount, extraction times, and each factor is established 3 levels, EXPERIMENTAL DESIGN such as table 6:
Table 6
By orthogonal table L9 (3
4) experiment arrangement.Experimental technique such as table 7:
Table 7
More than experiment is at first used and is got this Chinese medicinal composition preparation oral liquid 20ml, extracts 2 times with petroleum ether (60-90 ℃) jolting, and each 20ml discards petroleum ether liquid, experimentizes according to experimental design again, prepares 9 parts of need testing solutions altogether.
Get Herba Polygoni Capitati control medicinal material 1g, add water 50ml and decocted 30 minutes, filter, filtrating is concentrated into 20ml, extracts 2 times with the ethyl acetate jolting, processes control medicinal material solution.
Drawing each 5 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, be developing solvent with cyclohexane extraction-acetone-formic acid (4: 6: 0.5), launches, and takes out, and dries, and spray is with 10% ethanol solution of sulfuric acid, 105 ℃ be heated to speckle develop the color clear.
Result of the test shows,
Adopt in the test sample chromatograph of Herba Polygoni Capitati composition in the ethyl acetate enrichment preparation, with control medicinal material chromatograph relevant position, show the speckle of same color, clear spot, the plate face is clean and tidy, free from admixture disturbs.
When adopting in ether, the chloroform enrichment preparation Herba Polygoni Capitati composition, in the need testing solution chromatograph with control medicinal material chromatograph relevant position on, spot colors is used in the need testing solution chromatograph of ethyl acetate extraction a little less than the spot colors.
Confirm to select for use Herba Polygoni Capitati composition in the ethyl acetate enrichment preparation.
Optimum test sample method for preparing is: get this Chinese medicinal composition preparation oral liquid 20ml, extract 2 times with petroleum ether (60-90 ℃) jolting, each 20ml; Discard petroleum ether liquid; The jolting of water liquid reuse ethyl acetate is extracted 2 times, each 20ml, combined ethyl acetate liquid; Evaporate to dryness, residue add methanol 1ml makes dissolving as need testing solution.
2.3 the control medicinal material solution manufacturing method is investigated
Control medicinal material should be followed preparation process, and after decocting boiled, the corresponding composition of Herba Polygoni Capitati made an experiment in the extraction water extract.
(1), the investigation of control medicinal material decocting time:
Get three parts of Herba Polygoni Capitati control medicinal material 1g, add water 50ml and decocted respectively 15,30,60 minutes, filter, filtrating is concentrated into 20ml, extracts 2 times with the ethyl acetate jolting, processes control medicinal material solution 1,2,3.
Drawing each 5 μ l of above-mentioned solution, o'clock on three silica gel g thin-layer plates, be developing solvent with cyclohexane extraction-acetone-formic acid (4: 6: 0.5) respectively, launches, and takes out, and dries, and spray is with 10% ethanol solution of sulfuric acid, 105 ℃ be heated to speckle develop the color clear.
Experimental result shows: decoct and can extract in 30 minutes fully.
(2), control medicinal material extracts the investigation of quantity of solvent:
Get three parts of Herba Polygoni Capitati control medicinal material 1g, add water 25,50,100ml decoction 30 minutes respectively, filter, filtrating is concentrated into 20ml, extracts 2 times with the ethyl acetate jolting, processes control medicinal material solution 1,2,3.
Drawing each 5 μ l of above-mentioned solution, o'clock on three silica gel g thin-layer plates, be developing solvent with cyclohexane extraction-acetone-formic acid (4: 6: 0.5) respectively, launches, and takes out, and dries, and spray is with 10% ethanol solution of sulfuric acid, 105 ℃ be heated to speckle develop the color clear.
Experimental result shows: the 50ml decocting boils and can extract in 30 minutes fully.
(3), the investigation of Herba Polygoni Capitati composition experiment condition in the enrichment control medicinal material:
Method one: get Herba Polygoni Capitati control medicinal material 1g, add water 50ml and decocted 30 minutes, filter; Filtrating is concentrated into 20ml, extracts 2 times with petroleum ether (60-90 ℃) jolting, each 20ml; Discard petroleum ether liquid, the jolting of water liquid reuse ethyl acetate is extracted 2 times, each 20ml; Combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving as control medicinal material solution.
Method two: get Herba Polygoni Capitati control medicinal material 1g, add water 50ml and decocted 30 minutes, filter, filtrating is concentrated into 20ml, extracts 2 times with the ethyl acetate jolting, each 20ml, and combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving as control medicinal material solution.
Drawing each 5 μ l of above-mentioned solution, o'clock on two silica gel g thin-layer plates, be developing solvent with cyclohexane extraction-acetone-formic acid (4: 6: 0.5) respectively, launches, and takes out, and dries, and spray is with 10% ethanol solution of sulfuric acid, 105 ℃ be heated to speckle develop the color clear.
Experimental result shows: need not use petroleum ether (60-90 ℃) extraction to remove low polarity component during preparation control medicinal material solution, this part composition does not disturb detecting.
Final definite control medicinal material solution manufacturing method is: get Herba Polygoni Capitati control medicinal material 1g, add water 50ml and decocted 30 minutes, filter; Filtrating is concentrated into 20ml, extracts 2 times with the ethyl acetate jolting, each 20ml; Combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving as control medicinal material solution.
2.4 the investigation of need testing solution and control medicinal material solution point sample amount
Be equipped with need testing solution by 2.2,2.3 below legal systems.
Drawing each 2 μ l of above-mentioned solution, 5 μ l, 10 μ l, o'clock on three silica gel g thin-layer plates, be developing solvent with cyclohexane extraction-acetone-formic acid (4: 6: 0.5) respectively, launches, and takes out, and dries, and spray is with 10% ethanol solution of sulfuric acid, 105 ℃ be heated to speckle develop the color clear.
Experimental result is following:
When control medicinal material solution point sample amount was 2 μ l, the fluorescence spot intensity was lower, should not observe;
When the point sample amount was 5 μ l, fluorescence clear spot on the Herba Polygoni Capitati control medicinal material solution thin layer was of moderate size;
When the point sample amount was 10 μ l, speckle was too big, hangover.
Therefore, the best point sample amount of confirming Herba Polygoni Capitati control medicinal material solution is 5 μ l.
When need testing solution point sample amount was 2 μ l, spot intensity was lower on the corresponding position of Herba Polygoni Capitati control medicinal material solution, should not observe;
When the point sample amount was 5 μ l, speckle was obvious on the corresponding position of Herba Polygoni Capitati control medicinal material solution, and spot size is moderate, and front and back are noiseless;
When the point sample amount was 10 μ l, the fluorescence speckle was bigger on the corresponding position of Herba Polygoni Capitati control medicinal material solution, and obviously hangover links to each other with front and back fluorescence speckle.
Dimension confirms that the best point sample amount of test sample is 5 μ l.
2.5 the selection of developing solvent:
Be equipped with need testing solution by 2.2,2.3 below legal systems.
Draw each 5 μ l of above-mentioned solution, launch with following developing solvent respectively, take out, dry, spray is with 10% ethanol solution of sulfuric acid, 105 ℃ be heated to speckle develop the color clear.Result of the test is following:
Method 1: developing solvent is cyclohexane extraction-acetone-formic acid (20: 6: 0.5), and developing solvent polarity is less, and test sample, control medicinal material spot and R f value are near 0.2, and Herba Polygoni Capitati composition speckle does not separate with the front and back speckle in the test sample chromatograph.
Method 2: developing solvent is cyclohexane extraction-acetone-formic acid (4: 6: 0.5), and polarity is suitable, and the control medicinal material spot and R f value in the test sample chromatograph, is the corresponding speckle of control medicinal material solution near 0.5, separates well, and front and back are noiseless;
Method 3: developing solvent is cyclohexane extraction-acetone-formic acid (1: 6: 0.5), and polarity is higher, and test sample, Hesperidin spot and R f value are near 0.85, and Herba Polygoni Capitati composition speckle does not separate with the front and back speckle in the test sample chromatograph;
Through above-mentioned experiment, confirm that the optimum thin-layer developing agent of Herba Polygoni Capitati composition is cyclohexane extraction-acetone-formic acid (4: 6: 0.5) in the separating traditional Chinese medicine composite preparation.
2.6 the selection of developer
Composition daylight in the Herba Polygoni Capitati does not have color, considers the observation of colour developing back.Universal developer commonly used is 10% ethanol solution of sulfuric acid and iodine vapor.
Prepare need testing solution, control medicinal material solution as stated above.Get three silica gel thin-layers respectively point sample, launch, dry.
Method one: inspect under the ultra-violet lamp (365nm);
Method two: spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to the speckle colour developing clear;
Method three: iodine vapor colour developing.
Experimental result is following:
Method one, thin layer is observed down at ultra-violet lamp (365nm), does not observe color and the consistent speckle of Rf value in need testing solution and the control medicinal material solution chromatograph.
With 10% ethanol solution of sulfuric acid, 105 ℃ to be heated to the speckle colour developing clear in spray for method two, thin layer.On the corresponding position of Herba Polygoni Capitati control medicinal material, need testing solution has the speckle of obvious same color, clear spot, and front and back are noiseless.
Method three, the smoked back of iodine vapor speckle is more.On the corresponding position of Herba Polygoni Capitati control medicinal material, speckle and other speckles are overlapped in the need testing solution chromatograph, disturb and differentiate.
Finally, the best color condition of confirming Herba Polygoni Capitati composition in the separating traditional Chinese medicine composite preparation for spray with 10% ethanol solution of sulfuric acid, 105 ℃ to be heated to the speckle colour developing clear.
Experimental example 3: Herba Plantaginis thin layer discrimination test
Mainly contain flavone compound such as plantagin etc. in the Herba Plantaginis, be the effective ingredient of Herba Plantaginis.This prescription flavour of a drug are more, and complicated component, thin layer discrimination method are relatively unique.
1, the selection of test sample method for preparing and lamellae is selected
Utilize in the Herba Plantaginis in the chemical constituent and Herba Polygoni Capitati the chemical constituent polar phase seemingly among the present invention, differentiate in the test sample at the Herba Polygoni Capitati thin layer and also contain composition in the Herba Plantaginis, below this is verified:
The preparation of need testing solution: get Chinese medicinal composition preparation 20ml, extract 2 times, each 20ml with petroleum ether (60-90 ℃) jolting; Discard petroleum ether liquid; The jolting of water liquid reuse ethyl acetate is extracted 2 times, each 20ml, combined ethyl acetate liquid; Evaporate to dryness, residue add methanol 1ml makes dissolving as need testing solution.
Get Herba Plantaginis control medicinal material 1g and add water 100ml decoction 30 minutes, filter, filtrating is concentrated into 20ml, extracts 2 times with the ethyl acetate jolting, each 20ml, and combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml as control medicinal material solution.
Drawing each 4 μ l of above-mentioned two kinds of solution, put respectively on same silica gel H lamellae, be developing solvent with cyclohexane extraction-acetone-formic acid (6: 4: 0.2), launches, and takes out, and dries, and spray is with 10% ethanol solution of sulfuric acid, 105 ℃ be heated to speckle develop the color clear.
The result shows: in the test sample chromatograph, with Herba Plantaginis control medicinal material chromatograph relevant position on, show the speckle of same color.The Herba Polygoni Capitati thin layer differentiates that the need testing solution method for preparing is equally applicable to prepare the thin layer discriminating test sample of Herba Plantaginis.
2, the control medicinal material solution manufacturing method is investigated
Control medicinal material should be followed preparation process, and after decocting boiled, the corresponding composition of Herba Plantaginis made an experiment in the extraction water extract.
(1), the investigation of control medicinal material decocting time:
Get three parts of Herba Plantaginis control medicinal material 1g, add water 100ml and decocted respectively 15,30,60 minutes, filter, filtrating is concentrated into 20ml, extracts 2 times with the ethyl acetate jolting, processes control medicinal material solution 1,2,3.
Drawing each 4 μ l of above-mentioned three kinds of solution, put respectively on same silica gel H lamellae, be developing solvent with cyclohexane extraction-acetone-formic acid (6: 4: 0.2), launches, and takes out, and dries, and spray is with 10% ethanol solution of sulfuric acid, 105 ℃ be heated to speckle develop the color clear.
Experimental result shows: decoct and can extract in 30 minutes fully.
(2), control medicinal material extracts the investigation of quantity of solvent:
Get three parts of Herba Plantaginis control medicinal material 1g, add water 50,100,150ml decoction 30 minutes respectively, filter, filtrating is concentrated into 20ml, extracts 2 times with the ethyl acetate jolting, processes control medicinal material solution 1,2,3.
Drawing each 4 μ l of above-mentioned three kinds of solution, put respectively on same silica gel H lamellae, be developing solvent with cyclohexane extraction-acetone-formic acid (6: 4: 0.2), launches, and takes out, and dries, and spray is with 10% ethanol solution of sulfuric acid, 105 ℃ be heated to speckle develop the color clear.
Experimental result shows: the 100ml decocting boils and can extract in 30 minutes fully.
(3), the investigation of Herba Plantaginis composition experiment condition in the enrichment control medicinal material:
Method one: get Herba Plantaginis control medicinal material 1g, add water 100ml and decocted 30 minutes, filter; Filtrating is concentrated into 20ml, extracts 2 times with petroleum ether (60-90 ℃) jolting, each 20ml; Discard petroleum ether liquid, the jolting of water liquid reuse ethyl acetate is extracted 2 times, each 20ml; Combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving as control medicinal material solution.
Method two: get Herba Plantaginis control medicinal material 1g, add water 100ml and decocted 30 minutes, filter, filtrating is concentrated into 20ml, extracts 2 times with the ethyl acetate jolting, each 20ml, and combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving as control medicinal material solution.
Drawing each 4 μ l of above-mentioned two kinds of solution, put respectively on same silica gel H lamellae, be developing solvent with cyclohexane extraction-acetone-formic acid (6: 4: 0.2), launches, and takes out, and dries, and spray is with 10% ethanol solution of sulfuric acid, 105 ℃ be heated to speckle develop the color clear.
Experimental result shows: need not use petroleum ether (60-90 ℃) extraction to remove low polarity component during preparation control medicinal material solution, this part composition does not disturb detecting.
Final definite control medicinal material solution manufacturing method is: get Herba Plantaginis control medicinal material 1g and add water 100ml decoction 30 minutes, filter, filtrating is concentrated into 20ml; Extract 2 times each 20ml, combined ethyl acetate liquid with the ethyl acetate jolting; Evaporate to dryness, residue add methanol 1ml as control medicinal material solution.
3, the investigation of need testing solution and control medicinal material solution point sample amount
Be equipped with need testing solution, control medicinal material solution by 2.1,2.2 below legal systems.
Draw above-mentioned need testing solution, each 2 μ l of control medicinal material solution, 4 μ l, 8 μ l respectively; O'clock on three blocks of silica gel H lamellaes, be developing solvent respectively, launch with cyclohexane extraction-acetone-formic acid (6: 4: 0.2); Take out; Dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to speckle colour developing clear.
Experimental result is following:
When Herba Plantaginis control medicinal material solution point sample amount was 2 μ l, the fluorescence spot intensity was lower, should not observe;
When the point sample amount was 4 μ l, fluorescence clear spot on the Herba Polygoni Capitati control medicinal material solution thin layer was of moderate size;
When the point sample amount was 8 μ l, speckle was too big, hangover.
Therefore, the best point sample amount of confirming Herba Plantaginis control medicinal material solution is 4 μ l.
When need testing solution point sample amount was 2 μ l, spot intensity was lower on the corresponding position of Herba Plantaginis control medicinal material solution, should not observe;
When the point sample amount was 4 μ l, speckle was obvious on the corresponding position of Herba Plantaginis control medicinal material solution, and spot size is moderate, and front and back are noiseless;
When the point sample amount was 8 μ l, the fluorescence speckle was bigger on the corresponding position of Herba Plantaginis control medicinal material solution, and obviously hangover links to each other with front and back fluorescence speckle.
Dimension confirms that the best point sample amount of test sample is 4 μ l.
4, the selection of developing solvent:
Prepare need testing solution and control medicinal material solution as stated above.Draw each 4 μ l of above-mentioned solution, o'clock on three blocks of silica gel H lamellaes, launch with following developing solvent respectively respectively, take out, dry, spray is with 10% ethanol solution of sulfuric acid, 105 ℃ be heated to speckle develop the color clear.Result of the test is following:
Method 1: developing solvent is cyclohexane extraction-acetone-formic acid (15: 4: 0.2), and developing solvent polarity is less, and test sample, control medicinal material spot and R f value are near 0.3.Speckle is all launched preferably in test sample and the control medicinal material chromatograph.
Method 2: developing solvent is cyclohexane extraction-acetone-formic acid (6: 4: 0.2), and polarity is suitable, and the control medicinal material spot and R f value is near 0.4-0.6, but the speckle form is bad, and rounding not too need improve the consumption of formic acid;
Method 3: developing solvent is cyclohexane extraction-acetone-formic acid (1: 4: 0.2), and polarity is suitable, and the control medicinal material spot and R f value is near 0.4-0.6, and the speckle rounding, and is clear.
Through compare adjustment developing solvent ratio with the Herba Polygoni Capitati unfolding condition.Confirm that the optimum thin-layer developing agent of Herba Plantaginis composition is cyclohexane extraction-acetone-formic acid (6: 4: 0.2) in the separating traditional Chinese medicine composite preparation.
5, the selection of developer:
Composition daylight in the Herba Plantaginis does not have color, considers the observation of colour developing back.Universal developer commonly used is 10% ethanol solution of sulfuric acid and iodine vapor.
Prepare need testing solution, control medicinal material solution as stated above.Get three silica gel thin-layers respectively point sample, launch, dry.
Method one: inspect under the ultra-violet lamp (365nm);
Method two: spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to the speckle colour developing clear;
Method three: iodine vapor colour developing.
Experimental result is following:
Method one, thin layer is observed down at ultra-violet lamp (365nm), does not observe color and the consistent speckle of Rf value in need testing solution and the control medicinal material solution chromatograph.
With 10% ethanol solution of sulfuric acid, 105 ℃ to be heated to the speckle colour developing clear in spray for method two, thin layer.On the corresponding position of Herba Plantaginis control medicinal material, need testing solution has the speckle of obvious same color, clear spot, and front and back are noiseless.
Method three, the smoked back of iodine vapor speckle is more.On the corresponding position of Herba Polygoni Capitati control medicinal material, speckle and other speckles are overlapped in the need testing solution chromatograph, disturb and differentiate.
Finally, the best color condition of confirming Herba Plantaginis composition in the separating traditional Chinese medicine composite preparation for spray with 10% ethanol solution of sulfuric acid, 105 ℃ to be heated to the speckle colour developing clear.
6, the selection of lamellae:
Common silica gel thin-layer plate has two kinds, and a kind of is silica gel G, a kind of for the silica gel H lamellae, and the ability difference of among the present invention these two kinds of lamellaes being separated the Herba Plantaginis compositions compares, preferred optimal separation condition.
Prepare need testing solution, control medicinal material solution as stated above.
Get silica gel G, H lamellae, all point sample 4 μ l need testing solutions and control medicinal material solution be developing solvent with cyclohexane extraction-acetone-formic acid (6: 4: 0.2), launch, and take out, and dry, spray with 10% ethanol solution of sulfuric acid, 105 ℃ be heated to speckle develop the color clear.
Experimental result shows; Chemical constituent in all separable Herba Plantaginis of silica gel G and silica gel H lamellae; But silica gel H is better than the silica gel g thin-layer plate experimental result; Separate with the front and back speckle at speckle in the test sample chromatograph with control medicinal material solution chromatograph relevant position better, so select the silica gel H lamellae to separate composition in the Herba Plantaginis.
Experimental example 4: the mensuration of Chinese medicinal composition preparation oral liquid total solid
Changed the content regulation quality of the pharmaceutical preparations of utilizing HPLC to measure Quercetin in the preparation in original standard among the present invention, measured the total solid regulation quality of the pharmaceutical preparations and use instead.Following advantage is arranged:
Complex chemical composition in the Chinese medicinal composition preparation; Quercetin only is a composition in the countless compositions, do not represent globality, and Quercetin does not have heat-clearing and toxic substances removing; The effect of inducing diuresis for treating stranguria syndrome, the quality of use Quercetin regulation preparation can not well guarantee the curative effect of preparation.
The Quercetin unstable chemcial property, oxidized easily, need testing solution extracts after 24 hours and decays seriously, can increase the difficulty of analysis so use Quercetin to detect index as assay, and can cause quality fluctuation bigger.
Can measure the total solid of medicine for the indefinite Chinese medicine preparation of effective ingredient, just extract content regulation formulation content.Utilize total solid regulation formulation content among the present invention, the quality of the pharmaceutical preparations is stable, through the diuresis experiment proof efficacy stability of 10 lot sample article, measures quercetin content in the preparation simultaneously, and it is bigger to fluctuate, so select to measure the total solid regulation quality of the pharmaceutical preparations.
Attach:
1,10 lot sample article diuresis experimental results:
Get 120 of mices and be divided into 12 groups, be respectively blank control group, 10 administration groups, 1 positive drug control group.1 mice is got in test at every turn, gently presses the thing lower abdomen and drains surplus urine, loads by the 0.4ml/10gip normal saline, then ig administration or 0.5%CMC-Na contrast liquid.At random animal is placed simple and easy metabolic cage, every cage is put 1 mice, collects the 4h total volume of urine, and urine amount and the urine amount of obtaining the every 10g body weight of mice increase percentage rate %.Experimental result is seen table 8:
10 batches of preparation diuresis of table 8 relatively
Annotate: compare with the normal control group:
*P＜0.05,
*P＜0.01
The diuresis experiment proof efficacy stability of 10 lot sample article all can increase the mouse retention amount.
2, sharp total solid of 10 lot sample article and quercetin content are measured the result, see table 9:
Table 9 sharp total solid of 10 lot sample article and quercetin content are measured the result
Experimental result show this Chinese medicinal composition preparation oral liquid with Quercetin as the assay index, less stable as a result, and use total solid as the assay index, the result is stable.The drug effect result is stable simultaneously, so this Chinese medicinal composition preparation oral liquid is selected the index of total solid as assay for use.
The specific embodiment
Embodiment 1
Herba Polygoni Capitati 540g Herba Plantaginis 260g
More than two the flavor medical materials, decocte with water three times, each 1 hour, collecting decoction; Filter, filtrating is concentrated into the clear paste that relative density is 1.10～1.15 (50 ℃), puts coldly, adds ethanol and makes and contain the alcohol amount and reach 50%; Stir, left standstill 24 hours, get supernatant and reclaim ethanol, add an amount of sucrose, sorbic acid; Add water adjustment total amount to 1000ml, stir, fill promptly gets.
Differentiate:
(1) get these article 20ml, extract 2 times with petroleum ether (60-90 ℃) jolting, each 20ml discards petroleum ether liquid, and the jolting of water liquid reuse ethyl acetate is extracted 2 times, each 20ml, and combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving as need testing solution.Other gets Herba Polygoni Capitati control medicinal material 1g, adds water 50ml and decocts 30 minutes, filters, and filtrating is concentrated into 20ml, extracts 2 times with the ethyl acetate jolting, shines medical material solution in pairs with legal system.According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate; With cyclohexane extraction-acetone-formic acid (4: 6: 0.5) is developing solvent, launches, and takes out; Dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to speckle colour developing clear.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(2) preparation of need testing solution: with differentiating (1) item method for preparing of need testing solution down.Other gets Herba Plantaginis control medicinal material 1g and adds water 100ml decoction 30 minutes, filters, and filtrating is concentrated into 20ml, extracts 2 times with the ethyl acetate jolting, each 20ml, and combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml as control medicinal material solution.According to the thin layer chromatography test, draw each 4 μ l of above-mentioned two kinds of solution, put respectively on same silica gel H lamellae; With cyclohexane extraction-acetone-formic acid (6: 4: 0.2) is developing solvent, launches, and takes out; Dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to speckle colour developing clear.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Extractum: precision is measured these article 10ml, puts in the evaporating dish that is dried to constant weight, behind water bath method, in 105 ℃ of dryings 3 hours, puts in the exsiccator cooling 30 minutes, accurately rapidly claims to decide weight.These article extract content must not be lower than 4.0%.
Function cures mainly: heat-clearing and toxic substances removing, inducing diuresis for treating stranguria syndrome.Be used for stranguria due to the damp-heat accumulation, card is seen: it is not smooth to urinate, odynuria.
Usage and dosage is oral, one time 1,3 times on the one; 5 days one courses of treatment.
Specification: every 10ml
Embodiment 2
Herba Polygoni Capitati 740g Herba Plantaginis 460g
More than two the flavor medical materials, decocte with water three times, each 1 hour, collecting decoction; Filter, filtrating is concentrated into the clear paste that relative density is 1.10～1.15 (50 ℃), puts coldly, adds ethanol and makes and contain the alcohol amount and reach 50%; Stir, left standstill 24 hours, get supernatant and reclaim ethanol, add an amount of sucrose, sorbic acid; Add water adjustment total amount to 1000ml, stir, fill promptly gets.
Embodiment 3
Herba Polygoni Capitati 640g Herba Plantaginis 260g
More than two the flavor medical materials, decocte with water three times, each 1 hour, collecting decoction; Filter, filtrating is concentrated into the clear paste that relative density is 1.10～1.15 (50 ℃), puts coldly, adds ethanol and makes and contain the alcohol amount and reach 50%; Stir, left standstill 24 hours, get supernatant and reclaim ethanol, add an amount of sucrose, sorbic acid; Add water adjustment total amount to 1000ml, stir, fill promptly gets.
Embodiment 4
Herba Polygoni Capitati 540g Herba Plantaginis 260g
More than two the flavor medical materials, decocte with water three times, each 1 hour, collecting decoction; Filter, filtrating is concentrated into the clear paste that relative density is 1.10～1.15 (50 ℃), puts coldly, adds ethanol and makes and contain the alcohol amount and reach 50%; Stir, left standstill 24 hours, getting supernatant concentration to relative density is the thick paste of 1.35～1.40 (50 ℃), adds proper auxiliary materials; Process granule, drying, encapsulated, promptly get.
Embodiment 5
Herba Polygoni Capitati 540g Herba Plantaginis 260g
More than two the flavor medical materials, decocte with water three times, each 1 hour, collecting decoction; Filter, filtrating is concentrated into the clear paste that relative density is 1.10～1.15 (50 ℃), puts coldly, adds ethanol and makes and contain the alcohol amount and reach 50%; Stir, left standstill 24 hours, getting supernatant concentration to relative density is the thick paste of 1.35～1.40 (50 ℃), adds proper auxiliary materials; Process granule, drying promptly gets.
Claims (3)
1. the quality determining method of the Chinese medicine composition of a heat-clearing and toxic substances removing, inducing diuresis for treating stranguria syndrome is characterized in that this method comprises the steps:
A, discriminating: get this Chinese medicine composition oral liquid formulations 5-50ml, use boiling range to extract 1-3 time, each 15-30ml as 60-90 ℃ petroleum ether jolting; Discard petroleum ether liquid; The jolting of water liquid reuse ethyl acetate is extracted 1-3 time, each 10-40ml, combined ethyl acetate liquid; Evaporate to dryness, residue add methanol 1ml makes dissolving as need testing solution; Other gets Herba Polygoni Capitati control medicinal material 0.5-5g, adds water 20-100ml and decocts 15-45 minute, filters, and filtrating is concentrated into 10-40ml, extracts 1-3 time with the ethyl acetate jolting, shines medical material solution in pairs with legal system; Drawing each 2-10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with cyclohexane extraction-acetone-formic acid mixed solvent of 3-5: 5-8: 0.4-0.7; Launch, take out, dry; Spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to the speckle colour developing clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
B, discriminating: the preparation of need testing solution: get this Chinese medicine composition oral liquid formulations 5-50ml, use boiling range to extract 1-3 time, each 15-30ml as 60-90 ℃ petroleum ether jolting; Discard petroleum ether liquid; The jolting of water liquid reuse ethyl acetate is extracted 1-3 time, each 10-40ml, combined ethyl acetate liquid; Evaporate to dryness, residue add methanol 1ml makes dissolving as need testing solution; Other gets Herba Plantaginis control medicinal material 0.5-5g and adds water 60-140ml decoction 15-45 minute, filters, and filtrating is concentrated into 10-40ml; Extract 1-3 time each 10-40ml, combined ethyl acetate liquid with the ethyl acetate jolting; Evaporate to dryness, residue add methanol 1ml as control medicinal material solution; Draw each 2-8 μ l of above-mentioned two kinds of solution, put respectively on same silica gel H lamellae, with 5-8: 3-6: cyclohexane extraction-acetone of 0.2-formic acid mixed solvent is developing solvent; Launch, take out, dry; Spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to the speckle colour developing clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
C, extract content measure: precision is measured this Chinese medicine composition oral liquid formulations 5-20ml, puts in the evaporating dish that is dried to constant weight, behind water bath method, in 105 ℃ of dryings 3 hours, puts in the exsiccator cooling 30 minutes, accurately rapidly claims to decide weight; Extract content must not be lower than 4.0%;
Wherein, the crude drug of said Chinese medicine composition consists of: Herba Polygoni Capitati 450-640 weight portion, Herba Plantaginis 200-300 weight portion; This Chinese medicine composition is processed by following method: Herba Polygoni Capitati, Herba Plantaginis decocte with water 1-5 time; Each 0.5-3 hour; Collecting decoction filters, and filtrating concentrates; According to common process, process clinical or pharmaceutically acceptable tablet, capsule, powder, drop pill, honeyed pill, pill, granule, soft extract with bee honey agent, slow releasing preparation, quick releasing formulation, controlled release preparation, oral liquid, ejection preparation or external preparation.
2. quality determining method as claimed in claim 1 is characterized in that the crude drug of said Chinese medicine composition consists of: Herba Polygoni Capitati 540 weight portions, Herba Plantaginis 260 weight portions; This Chinese medicine composition is processed by following method: Herba Polygoni Capitati, Herba Plantaginis decocte with water three times, and each 1 hour, collecting decoction filtered; Filtrating when being concentrated into 50 ℃ relative density be 1.10～1.15 clear paste, put coldly, add ethanol and make and contain the alcohol amount and reach 50%, stir; Left standstill 24 hours, and got supernatant and reclaim ethanol, add an amount of sucrose, sorbic acid, add water adjustment total amount to 1000 parts by volume; Stir, fill promptly gets.
3. like the quality determining method of the described Chinese medicine composition of claim 1-2, it is characterized in that this method comprises the steps:
A, Herba Polygoni Capitati thin layer are differentiated: get Chinese medicinal composition preparation 20ml, use boiling range to extract 2 times as 60-90 ℃ of petroleum ether jolting, each 20ml; Discard petroleum ether liquid; The jolting of water liquid reuse ethyl acetate is extracted 2 times, each 20ml, combined ethyl acetate liquid; Evaporate to dryness, residue add methanol 1ml makes dissolving as need testing solution; Other gets Herba Polygoni Capitati control medicinal material 1g, adds water 50ml and decocts 30 minutes, filters, and filtrating is concentrated into 20ml, extracts 2 times with the ethyl acetate jolting, shines medical material solution in pairs with legal system; Drawing each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with cyclohexane extraction-acetone of 4: 6: 0.5-formic acid, launches, and takes out, and dries, and spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to the speckle colour developing clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
B, Herba Plantaginis thin layer are differentiated: the preparation of need testing solution: with the method for preparing of differentiating need testing solution under the A item; Other gets Herba Plantaginis control medicinal material 1g and adds water 100ml decoction 30 minutes, filters, and filtrating is concentrated into 20ml, extracts 2 times with the ethyl acetate jolting, each 20ml, and combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml as control medicinal material solution; Drawing each 4 μ l of above-mentioned two kinds of solution, put respectively on same silica gel H lamellae, is developing solvent with cyclohexane extraction-acetone of 6: 4: 0.2-formic acid, launches, and takes out, and dries, and spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to the speckle colour developing clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
C, extract content measure: precision is measured Chinese medicinal composition preparation 10ml, puts in the evaporating dish that is dried to constant weight, behind water bath method, in 105 ℃ of dryings 3 hours, puts in the exsiccator cooling 30 minutes, accurately rapidly claims to decide weight; Extract content must not be lower than 4.0%.
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| CN1785264A (en) * | 2005-11-29 | 2006-06-14 | 北京亚东生物制药有限公司 | Chinese medicinal composition for treating strangury patterns and preparation method of its oral liquid, tablet and capsule |
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|---|---|
| CN101843670A (en) | 2010-09-29 |
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