CN1650922A - Chinese medicinal composition for treating blood depletion qi vacuity, menstral irregularity and its preparation method - Google Patents
Chinese medicinal composition for treating blood depletion qi vacuity, menstral irregularity and its preparation method Download PDFInfo
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Abstract
A Chinese medicine in the form of oral liquid, tablet, capsule, syrup, pill, or injection for nourishing blood and vital energy and treating menoxenia is prepared from 6 Chinese-medicinal materials including donkey-hide gelatin, astragalus root, Chinese angelica root, etc through decocting, distilling concentrating and adding auxiliary.
Description
Invention field
The present invention relates to a kind of Chinese medicine composition, particularly be used for the treatment of the Chinese medicine composition of weakness due to chronic disease and the menoxenia of women's anemia deficiency of vital energy, relate to the preparation method of said composition simultaneously.
Background technology
Hypomenorrhea, amenorrhea are the modal diseases of women, and the modern medicine treatment lacks effective Therapeutic Method, and Chinese medicine and pharmacy treatment primary disease has clear superiority.
Discharge obviously minimizing through blood volume, even drop is promptly clean, or the time of passing through is too short, less than two days, through measuring also thereby minimizing person, claim " hypomenorrhea ", also claim " scanty menorrhea ", primary disease " moon is few ... first few " promptly on the books in " General Treatise on the Cause and Symptoms of Diseases ", " danxi's experiential therapy " have another name called says " through the row pettiness ".The woman is over 18 one full year of life menstruation not menophania as yet, or passed through and interrupt reaching person more than three months, is called " amenorrhea ", and the former claims primary amenorrhea, and the latter claims secondary amenorrhea.Primary disease is promptly on the books as far back as " interior warp ", claims " morbid amenorrhea ", " amenorrhea ", also is provided with a special piece of writing in " Medical Treasures of the Golden Chamber " and discusses.
Summary of the invention
One object of the present invention is to disclose a kind of new treatment weakness due to chronic disease and the Chinese medicine composition of women's anemia deficiency of vital energy menoxenia; Another object of the present invention is the method for the Chinese medicine composition of a kind of new treatment weakness due to chronic disease of open preparation and the menoxenia of women's anemia deficiency of vital energy; The object of the invention also is to disclose a kind of method of quality control of new Chinese medicinal composition preparation.
The crude drug of pharmaceutical composition of the present invention is formed and proportioning following (by weight):
Colla Corii Asini 170-250 weight portion Radix Astragali 140-230 weight portion Radix Codonopsis 140-230 weight portion
Radix Rehmanniae Preparata 80-170 weight portion Rhizoma Atractylodis Macrocephalae 50-140 weight portion Radix Angelicae Sinensis 30-90 weight portion
Above Chinese medicine composition can add adjuvant and make any dosage form on the pharmaceutics meaning, comprises oral liquid, tablet, capsule, syrup, drop pill, pill (concentrated pill), injection etc., preferred oral liquid preparation, pill (concentrated pill).
The present composition is prepared into the oral liquid method:
Above Six-element, it is suitably disconnected broken to get Radix Angelicae Sinensis, the Rhizoma Atractylodis Macrocephalae, distill, it is standby to collect distillate, and the residue and the Radix Astragali, Radix Codonopsis, Radix Rehmanniae Preparata decoct with water 2-4 time, each 1-2.5 hour, collecting decoction filters, and filtrate is concentrated into the clear paste that relative density is 1.0-1.20 (65 ℃-85 ℃), after the cooling, add ethanol and make the alcohol amount of containing be 45-60%.Stir evenly, cooling is left standstill, and filters, and filtrate recycling ethanol is concentrated into relative density and is 1.0-1.15, and is standby; Get Colla Corii Asini and add suitable quantity of water and dissolve, filter, filtrate and the merging of above-mentioned concentrated solution; Sucrose is made syrup, merges with above-mentioned concentrated solution, distillate, and the adding antiseptic is an amount of, and adjusting total amount is 2000 parts by volume, leaves standstill, filter, and embedding, sterilization, that is, and every dress 20ml.
The present composition is prepared into the concentrated pill method:
Above Six-element, Colla Corii Asini is ground into fine powder, and is standby; Get Radix Angelicae Sinensis, the Rhizoma Atractylodis Macrocephalae distills, it is standby to collect distillate, residue and the Radix Astragali, Radix Codonopsis, Radix Rehmanniae Preparata decoct with water 2-4 time, at every turn during 1-2.5, collecting decoction filters, and filtrate is concentrated into the clear paste that relative density is 1.0-1.20 (65 ℃-85 ℃), after the cooling, add ethanol and make the alcohol amount of containing be 45-60%, stir evenly, leave standstill, filter, filtrate recycling ethanol is concentrated into thick paste, adds above-mentioned distillate, donkey-hide gelatin fine powder, mixing is made concentrated pill, oven dry, polishing, promptly.
The method of quality control that the present composition is made medicament comprises discriminating and/or assay.(used present composition preparation is a composition oral liquid in the following method of quality control, and this method is applicable to all dosage forms of said composition)
Discrimination method comprises a kind of and/or several in the following method:
A. get this composition oral liquid 40ml, the jolting that adds diethyl ether is extracted 1-3 time, and each 50ml divides and gets ether layer, volatilizes, and residue adds ethyl acetate 0.5ml makes dissolving, as need testing solution; Other gets Radix Angelicae Sinensis control medicinal material 0.2g, and the 30ml that adds diethyl ether flooded 1 hour, the time add jolting, filter, filtrate volatilizes, residue adds ethyl acetate 0.5ml makes dissolving, in contrast medical material solution; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), draw need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with 8-12: 1-3 normal hexane-ethyl acetate is developing solvent, launch, take out, dry, put under the 365nm ultraviolet light and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical light blue white fluorescent speckle;
B. get this composition oral liquid 40ml, add ethyl acetate extraction 1-3 time, each 40ml divides and gets ethyl acetate liquid, and evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Rhizoma Atractylodis Macrocephalae control medicinal material 2g, adds water 30ml, and reflux 1 hour filters, and filtrate adds ethyl acetate and shines medical material solution in pairs with legal system; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, chloroform-acetone-formic acid with 18-21: 1-3: 0.1-0.5 is 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 same color fluorescence principal spot;
C. according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000) test, precision is measured this composition oral liquid 25ml under the loading amount item, uses ether extraction 1-3 time, each 30ml divides and takes off a layer solution, with water saturated n-butanol extraction 5 times, each 25ml, merge n-butanol extracting liquid, extract 3 times, each 20ml with ammonia solution, divide and get n-butyl alcohol liquid, evaporate to dryness, residue add 10% ethanol 5ml makes dissolving, puts cold, by D101 type macroporous adsorptive resins, with water 50ml eluting, discard water liquid, reuse 30-50% ethanol 30ml eluting, discard the 30-50% ethanol elution, continue with 60-80% ethanol 100ml eluting, collect eluent, evaporate to dryness, with dissolve with methanol and be transferred in the 2ml measuring bottle, add methanol to scale, shake up, as need testing solution; Precision takes by weighing the astragaloside reference substance in addition, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Draw each 5 μ l of need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with 11-15: 5-8: lower floor's solution that 1-4 chloroform-methanol-water is placed below 10 ℃ is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing at 100 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, daylight shows down identical sepia speckle; The 365nm ultra-violet lamp shows identical orange-yellow fluorescence speckle down;
Assay:
The Radix Astragali: precision is measured this composition oral liquid 25ml under the loading amount item, uses ether extraction 1-3 time, each 30ml, divide and to take off a layer solution, with water saturated n-butanol extraction 4-6 time, 25ml at every turn, merge n-butanol extracting liquid, extract 2-4 time with ammonia solution, each 20ml divides and gets n-butyl alcohol liquid, evaporate to dryness, residue adds 10% ethanol 5ml makes dissolving, puts coldly, passes through D
101The type macroporous adsorptive resins, with water 50ml eluting, discard water liquid, reuse 30-50% ethanol 30ml eluting, discard the 30-50% ethanol elution, continue with 60-80% ethanol 100ml eluting, collect eluent, evaporate to dryness, with dissolve with methanol and be transferred in the 2ml measuring bottle, add methanol to scale, shake up, as need testing solution; Precision takes by weighing the astragaloside reference substance in addition, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), accurate need testing solution 2 to the 5 μ l that draw, reference substance solution 1 μ l and 3 μ l, the cross point is on same silica gel g thin-layer plate respectively, with [n-butyl alcohol-ethyl acetate-water (3-5: 1-3: upper solution 4-7)]-methanol (9-12: 1-3) be developing solvent, launch, take out, dry, spray is with the 9-12% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 100 ℃, takes out, on lamellae, cover onesize glass plate, use immobilization with adhesive tape on every side, scan wavelength according to thin layer chromatography (an appendix VIB of Chinese Pharmacopoeia version in 2000 thin layer chromatography scanning): λ
S=530nm, λ
R=700nm measures test sample trap integrated value and reference substance trap integrated value, calculates, that is, every 20ml contains the Radix Astragali with astragaloside (C
41H
68O
14) meter, must not be less than 0.40mg.
Present composition preparation has good nourishing YIN and supplementing blood, invigorating the spleen and benefiting QI, and the effect of regulating menstruation and nourishing blood, and have no side effect.Present composition preparation method advanced person, active ingredient is fully discharged; Method of quality control can carry out effective and stable control to the quality of product.
Following experimental example is used to further specify the present invention.
Experimental example 1
Through clinical and FUKANGBAO KOUFUYE (Colla Corii Asini, Folium Artemisiae Argyi, the Radix Paeoniae Alba, Rhizoma Chuanxiong, Radix Angelicae Sinensis, Radix Rehmanniae Preparata, Radix Glycyrrhizae) the 50 routine controlled observations of 150 examples, be reported as follows:
1, clinical data
Treatment is organized 150 examples and is clinic case, and the age is in 4 examples of person more than 40 years old, 21-39 year person 81 examples, 18-20 year person 65 examples, 4 months person's 21 examples of the course of disease, 5-10 month person 99 examples, person's 30 examples more than 10 months.Matched group 50 examples are clinic case, and the age is in 2 examples of person more than 40 years old, 21-39 year person's 30 examples, 18-20 year person's 18 examples; 4 months person's 7 examples of the course of disease, 5-10 month person 30 examples, person's 13 examples more than 10 months.
2, tcm diagnosis standard: according to " the clinical research guideline of new Chinese medicine treatment amenorrhea " of Ministry of Public Health promulgation
(1) amenorrhea diagnosis: a, woman over 18 one full year of life, menstruation not menophania as yet (primary amenorrhea); Once there were menorrhea b, the past, and existing menolipsis reaches person more than 3 months (secondary amenorrhea).All have above 1 person, can be diagnosed as amenorrhea.
(2) syndrome diagnosis:
A, syndrome of deficiency of spleen qi: light red through color, thin menses prolongs after the menstruation gradually, by closing down less and gradually; Dizzy weak, deficiency of QI with disinclination to talk, yellowish complexion, anorexia, tastelessness is dull, and the pale tongue tongue is few, and deficient pulse is unable.
B, syndrome of deficiency of blood: menses are by closing down less and gradually, dizziness and blurred vision, and severe palpitation, hair are not damp, thready pulse, the few tongue of light red tongue.
C, deficiency of both QI and blood: prolong after the menstruation gradually, amount is few, and matter thin through color is light, and it is not all right to close down then, feel dizzy, and shortness of breath and palpitation, fatigue in both spirit and physical strength, hair are not damp easily to come off, thin and sallow complexion, deep-slow pulse or imaginary number, the few tongue of light red tongue or thin white.
3, efficacy assessment standard
Recovery from illness: the menstruation recovery normal cycle, other symptoms disappear substantially, keep 3 above persons of menstrual cycle after the drug withdrawal.
Produce effects: near normal cycle (in 40 days), rise 1 time other sxs after the drug withdrawal in 3 months automatically through the treatment menstruation.
Effectively: through treating in 3 months menstrual onset more than 1 time, other sxs.Though perhaps amenorrhea is not in the period, check the ovarian function person of being significantly improved.
Invalid: with continuous treatment 36 months, menstruation did not see and rises that other symptoms and relevant laboratory etc. inspections all do not have improvement.
4, therapeutic outcome (seeing Table 1)
Table 1 liang group therapeutic outcome and comparison
Group example number recovery from illness produce effects enabledisable
Treatment organizes 150 72 54 17 7
Matched group 50 6 17 19 8
5, efficacy analysis: treatment group, the relation of Chinese medical discrimination typing and course of disease curative effect (seeing Table 2,3)
The relation of table 2 treatment group TCM Syndrome Type and curative effect
Pattern of syndrome example number recovery from illness produce effects enabledisable
Syndrome of deficiency of spleen qi 81 44 34 30
Syndrome of deficiency of blood 46 20 13 12 1
Deficiency of both QI and blood 23 8726
The relation of the table 3 treatment group course of disease and curative effect
Course of disease example number recovery from illness produce effects enabledisable
4 months 21 12 540
5-10 month 99 47 46 51
More than 10 months 30 13 386
Can find out that from above two tables best with deficiency of spleen-QI pattern of syndrome curative effect, 81 examples are all effective, produce effects, recovery from illness account for 96.29%; Blood-deficiency type is taken second place, and produce effects, cure rate account for 71.73%; QI and blood deficiency pattern of syndrome person produce effects, cure rate account for 65.21%.The course of disease is at 4 months produce effects, cure rate 86.95%; 5～10 months person's produce effects, cure rate 93.3%; The course of disease more than 10 months person's produce effects, cure rate account for 60%.Illustrate that the course of disease 4 months does not have significant difference with 5～10 months person's curative effects, but the course of disease is person more than 10 months, then there were significant differences for curative effect.
Conclusion: present composition oral liquid formulations is all effective to amenorrhea it " syndrome of deficiency of spleen qi ", " syndrome of deficiency of blood ", " deficiency of both QI and blood ", especially with " syndrome of deficiency of spleen qi " curative effect the best.Present composition oral liquid formulations treatment amenorrhea effective percentage 95.33%, matched group FUKANGBAO KOUFUYE effective percentage is 84%.
Experimental example 2Method of quality control research
[assay] is the content assaying method of the Radix Astragali.
(1) instrument and reagent
1, instrument: CS-9301PC thin-layer chromatogram scanner (day island proper Tianjin); Quantitative capillary tube (Drummond); MettlerAE100,200 electronic balances.
2, reagent: (Yongkang, Guangdong pharmaceutcal corporation, Ltd produces and provides No. 3 oral liquids of amenorrhea (present composition oral liquid formulations); Lot number: 020401,020402,020403); Astragaloside reference substance (781-9002, Nat'l Pharmaceutical ﹠ Biological Products Control Institute provides); D
101Type macropore absorption resin (Tianjin rubber plant); Chromatography neutral alumina (lot number: 200321 Guangzhou pharmaceuticals chemical reagent glass apparatus wholesale departments); Tlc silica gel G (60 type) (lot number: 990313 Chinese Qingdao Haiyang Chemical Industry Group Corp.); Other reagent: be analytical pure.
(2) assay method
1, the preparation of need testing solution: precision is measured this product 25ml under the loading amount item, uses ether extraction 2 times, each 30ml, divide and to take off a layer solution, with water saturated n-butanol extraction 5 times, 25ml at every turn, merge n-butanol extracting liquid, extract 3 times with ammonia solution, each 20ml divides and gets n-butyl alcohol liquid, evaporate to dryness, residue adds 10% ethanol 5ml makes dissolving, puts coldly, passes through D
101Type macroporous adsorptive resins (internal diameter 1cm, long 15cm), with water 50ml eluting, discard water liquid, reuse 40% ethanol 30ml eluting, discard 40% ethanol and take off liquid, continue with 70% ethanol 100ml eluting, collect eluent, evaporate to dryness, with dissolve with methanol and be transferred in the 2ml measuring bottle, add methanol to scale, shake up, as need testing solution.
2, the preparation of reference substance solution: get the astragaloside reference substance, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution.
3, lack the preparation of Radix Astragali negative control solution: in the ratio and the method for making of prescription, make the negative control sample that lacks the Radix Astragali, get 25ml, press the method for need testing solution preparation, make the negative control solution that lacks the Radix Astragali.
4, thin layer chromatography: according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000) test, accurate need testing solution and each 5 μ l of negative control solution of drawing, reference substance solution 1 μ l and 3 μ l, respectively the cross point on same silica gel g thin-layer plate (from making sheet, thick 0.3mm), with [upper solution of n-butyl alcohol-ethyl acetate-water (4: 1: 5)]-methanol (10: 1.5) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 100 ℃, takes out, on lamellae, cover onesize glass plate, use immobilization with adhesive tape on every side.The negative control chromatograph is noiseless on astragaloside contrast chromatograph relevant position.
5, thin slice scan: scan wavelength according to thin layer chromatography (an appendix VIB of Chinese Pharmacopoeia version in 2000 thin layer chromatography scanning): λ
S=530nm, λ
R=700nm, light beam=0.4 * 10.0mm, linear scanning, step pitch=0.1mm.Measure test sample trap integrated value and reference substance trap integrated value, calculate, promptly.
With λ
S=530nm; Light beam=0.4 * 10.0mm, linear scanning, step pitch=0.1mm scans from the initial point to the forward position, gets scintigram.Negative control scintigram no absworption peak on astragaloside reference substance relevant position disturbs.
(3) methodology checking:
1, the extracting method of need testing solution: the present extracting method of astragaloside is mainly sample after with water saturated n-butanol extraction, and alkali cleaning through little column purification, is made need testing solution again.And the pillar that purifies is aluminium oxide pillar and D
101The type macroporous adsorptive resins, through selecting following method test for use:
1. press the operation of text method.
2. sample is after alkali cleaning → washing, and evaporate to dryness, residue add ethanol 5ml makes dissolving, is added in neutral alumina post (100～200 orders, 5g, internal diameter 1.1cm, dry column-packing) on, with 40% methanol 100ml eluting, collect eluent, evaporate to dryness, residue is made need testing solution by 1. method.
3. sample is after alkali cleaning → washing, and evaporate to dryness, residue add ethanol 5ml makes dissolving, is added in neutral alumina-D
101Type macroporous adsorptive resins (internal diameter 1.1cm, lower floor: D101 type macroporous adsorbent resin, high 12cm; Upper strata: neutral alumina post, 100～200 orders, high 3cm; Wet method dress post) on, with 70% ethanol 100ml eluting, the collection eluent, evaporate to dryness, residue is made need testing solution by 1. method.
Through laboratory observation, 1. the astragaloside speckle is clear than additive method for method, ambient interferences is few, reason may be the result of pillar through water, 4% ethanol elution, the visible impurity speckle of 40% ethanol elution collection of illustrative plates wherein, but the content to astragaloside is noiseless, and the extracting method of tentative need testing solution is drafted as text.
2, the selection of developing solvent: the developing solvent of astragaloside is except that the text method, and lower floor's solution that available chlorine imitation-carbinol-water (13: 6: 2) is placed below 10 ℃ is as developing solvent.I.e. usefulness can be promptly joined in the developing solvent of text method, need not place and spend the night.
3, the selection of scanning wavelength: lamellae carries out the original position spectral scan to the astragaloside speckle after launching, there is absorption maximum at the place at the 530nm wavelength, and is consistent with scanning wavelength under " Radix Astragali " assay item that pharmacopeia is recorded.
Select scanning wavelength such as text.
(4) astragaloside standard curve: accurate astragaloside reference substance solution (1.030mg/ml) 1,2,3,4,5, the 6 μ l that draw, put respectively on same lamellae, launch colour developing, scanning by above-mentioned content assaying method, the gained data are abscissa with concentration, peak area is a vertical coordinate, and the drawing standard curve gets regression equation: Y=114.7X+48.007, r=1.000, reference substance is linear in 1.030～6.180 μ g scopes.
(5) precision test: on the lamellae after the above-mentioned expansion colour developing, astragaloside reference substance speckle (3 μ l) by above-mentioned condition continuous sweep 5 times, be the results are shown in Table 4.
Table 4
Number of scans 12345 RSD%
Peak area 328.876 329.872 331.597 332.771 332.408 0.50
(6) stability test: get the lamellae of above-mentioned assay, scanned 1 time by above-mentioned condition, the results are shown in Table 5 every 1 hour.
(7) repeatability test: get test sample (lot number: 020402) mixing, accurately draw 5 parts of each 25ml, measure the content of astragaloside by the content assaying method of drafting, the results are shown in Table 6.
(8) application of sample recovery test: get test sample (lot number: 020402) mixing, 6 parts of each 25ml of accurate absorption, 1 part of content of measuring astragaloside wherein, all the other 5 parts each accurate astragaloside reference substance solution (0.4401mg/ml) 1ml that add, mixing, carry out the application of sample recovery test as stated above, the results are shown in Table 7.
Table 5
Sweep time (hour)
Peak area RSD%
Instant 1234
Reference substance (1 μ) 171.800 176.544 176.719 180.653 179.516 1.93
Reference substance (3 μ) 482.983 488.765 492.903 496.083 499.394 1.27
Test sample 307.576 312.362 314.968 318.373 321.688 1.72
Table 6
Number 12345 RSD%
Content (mg/ props up) 0.672 0.661 0.659 0.701 0.669 2.76
Table 7
Numbering content (mg/ props up) adds reference substance (mg/ props up) application of sample and records the average RSD% of content (mg/ props up) response rate (%)
1 1.0725 99.19
2 1.0862 100.46
3 0.6411 0.4401 1.0290 95.17 97.36 2.40
4 1.0379 95.99
5 1.0373 95.94
(9) sample size is measured: get test sample, measure by the above-mentioned content assaying method of drafting, the results are shown in Table 7.
Table 8
Lot number 020,401 020,402 020403 is average
Content (mg/ props up) 0.69 0.66 0.58 0.64
Following embodiment all can realize the effect of above-mentioned experimental example.
Embodiment 1Oral liquid
Colla Corii Asini 216g Radix Astragali 180g Radix Codonopsis 180g
Radix Rehmanniae Preparata 120g Rhizoma Atractylodis Macrocephalae 90g Radix Angelicae Sinensis 60g
Above Six-element, it is suitably disconnected broken to get Radix Angelicae Sinensis, the Rhizoma Atractylodis Macrocephalae, distills, and it is standby to collect distillate, the residue and the Radix Astragali, Radix Codonopsis, Radix Rehmanniae Preparata decoct with water 3 times, 1.5 hours for the first time, second and third time each 1 hour, collecting decoction, filter, filtrate is concentrated into the clear paste that relative density is 1.08-1.10 (75 ℃-80 ℃), after the cooling, adds ethanol and makes the alcohol amount of containing be 50-55%.Stir evenly, cooling is left standstill, and filters, and filtrate recycling ethanol is concentrated into relative density and is 1.08, and is standby; Get Colla Corii Asini and add the suitable quantity of water fusing, filter, filtrate and above-mentioned concentrated solution merge; Sucrose is made syrup, merges with above-mentioned concentrated solution, distillate, and the adding antiseptic is an amount of, and the adjustment total amount is 2000ml, leaves standstill, filter, and embedding, sterilization, promptly.Every dress 20ml.
[inspection] total nitrogen is got this product 2ml, and accurate the title decides, and measures according to N2 method (appendix IXL first method), and nitrogen content must not be less than 0.65%, and the Radix Astragali every (20ml) is with astragaloside (C
41H
68O
14) meter, must not be less than 0.40mg.
[function cures mainly] nourishing YIN and supplementing blood, invigorating the spleen and benefiting QI, regulating menstruation and nourishing blood.Be used for weakness due to chronic disease, the anemia deficiency of vital energy, diseases such as women's blood deficiency, amenorrhea, infrequent menstruation.
[usage and dosage] is oral, a 20ml, (containing crude drug 8.46g), 2 times on the one.
Embodiment 2Concentrated pill
Colla Corii Asini 216g Radix Astragali 180g Radix Codonopsis 180g
Radix Rehmanniae Preparata 120g Rhizoma Atractylodis Macrocephalae 90g Radix Angelicae Sinensis 60g
Above Six-element, Colla Corii Asini is ground into fine powder, and is standby.Get Radix Angelicae Sinensis, the Rhizoma Atractylodis Macrocephalae distills, it is standby to collect distillate, the residue and the Radix Astragali, Radix Codonopsis, Radix Rehmanniae Preparata decoct with water three times, 1.5 hours for the first time, second and third time each 1 hour, collecting decoction, filter, filtrate is concentrated into the clear paste that relative density is 1.08-1.10 (75 ℃-80 ℃), after the cooling, adding ethanol makes the alcohol amount of containing be 50-55%, stir evenly, leave standstill, filter, filtrate recycling ethanol, be concentrated into thick paste, add above-mentioned distillate, donkey-hide gelatin fine powder and adjuvant, mixing, make concentrated pill, oven dry, total amount 400g, polishing, promptly.Character, this product are the concentrated pill of yellowish-brown.Oral, each 4g (quite containing crude drug 8.46g), 2 times on the one.Function cures mainly with embodiment 1.
Embodiment 3Tablet
Colla Corii Asini 240g Radix Astragali 220g Radix Codonopsis 220g
Radix Rehmanniae Preparata 150g Rhizoma Atractylodis Macrocephalae 130g Radix Angelicae Sinensis 80g
Above Six-element, Colla Corii Asini is ground into fine powder, and is standby.Get Radix Angelicae Sinensis, the Rhizoma Atractylodis Macrocephalae distills, it is standby to collect distillate, the residue and the Radix Astragali, Radix Codonopsis, Radix Rehmanniae Preparata decoct with water three times, 1.5 hours for the first time, second and third time each 1 hour, collecting decoction filters, filtrate is concentrated into the clear paste that relative density is 1.08-1.10 (75 ℃-80 ℃), after the cooling, add ethanol and make the alcohol amount of containing be 50-55%, stir evenly, leave standstill, filter, filtrate recycling ethanol is concentrated into thick paste, add above-mentioned distillate, donkey-hide gelatin fine powder and adjuvant, mixing, often regulation gets tablet, each dose quite contains crude drug 8.46g, and function cures mainly with embodiment 1.
Embodiment 4Capsule
Colla Corii Asini 180g Radix Astragali 160g Radix Codonopsis 160g
Radix Rehmanniae Preparata 90g Rhizoma Atractylodis Macrocephalae 65g Radix Angelicae Sinensis 45g
Above Six-element, Colla Corii Asini is ground into fine powder, and is standby.Get Radix Angelicae Sinensis, the Rhizoma Atractylodis Macrocephalae distills, it is standby to collect distillate, the residue and the Radix Astragali, Radix Codonopsis, Radix Rehmanniae Preparata decoct with water three times, 1.5 hours for the first time, second and third time each 1 hour, collecting decoction filters, filtrate is concentrated into the clear paste that relative density is 1.08-1.10 (75 ℃-80 ℃), after the cooling, add ethanol and make the alcohol amount of containing be 50-55%, stir evenly, leave standstill, filter, filtrate recycling ethanol is concentrated into thick paste, add above-mentioned distillate, donkey-hide gelatin fine powder and adjuvant, mixing, often regulation gets capsule, take at every turn and quite contain crude drug 8.46g, function cures mainly with embodiment 1.
Embodiment 5The oral liquid method of quality control
This product 40ml is got in [discriminating] (1), and the jolting that adds diethyl ether is extracted 2 times, and each 50ml divides and gets ether layer, volatilizes, and residue adds ethyl acetate 0.5ml makes dissolving, as need testing solution.Other gets Radix Angelicae Sinensis control medicinal material 0.2g, and the 30ml that adds diethyl ether flooded 1 hour, the time add jolting, filter, filtrate volatilizes, residue adds ethyl acetate 0.5ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (appendix .VIB of Chinese Pharmacopoeia version in 2000), draw need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate (9: 1) is developing solvent, launch, take out, dry, put under the ultraviolet light (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical light blue white fluorescent speckle.
(2) get this product 40ml, add ethyl acetate extraction 2 times, each 40ml divides and gets ethyl acetate liquid, and evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Rhizoma Atractylodis Macrocephalae control medicinal material 2g, adds water 30ml, and reflux 1 hour filters, and filtrate adds ethyl acetate and shines medical material solution in pairs with legal system.According to thin layer chromatography (appendix .VIB of Chinese Pharmacopoeia version in 2000) test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-acetone-formic acid (19: 1: 0.2) is developing solvent, launches, and takes out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show same color fluorescence principal spot.
(3) according to thin layer chromatography (appendix .VIB of Chinese Pharmacopoeia version in 2000) test, draw need testing solution and each 5 μ l of reference substance solution under [assay] Radix Astragali item, put respectively on same silica gel g thin-layer plate, lower floor's solution of placing below 10 ℃ with chloroform-methanol-water (13: 6: 2) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 100 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, daylight shows down identical sepia speckle; Ultra-violet lamp (365nm) shows identical orange-yellow fluorescence speckle down.
[assay] Radix Astragali: precision is measured this product 25ml under the loading amount item, uses ether extraction 2 times, each 30ml, divide and to take off a layer solution, with water saturated n-butanol extraction 5 times, 25ml at every turn, merge n-butanol extracting liquid, extract 3 times with ammonia solution, each 20ml divides and gets n-butyl alcohol liquid, evaporate to dryness, residue adds 10% ethanol 5ml makes dissolving, puts coldly, passes through D
101Type macroporous adsorptive resins (internal diameter 1cm, long 15cm) is with water 50ml eluting, discard water liquid, reuse 40% ethanol 30ml eluting discards 40% ethanol elution, continues with 70% ethanol 100ml eluting, collect eluent, evaporate to dryness with dissolve with methanol and be transferred in the 2ml measuring bottle, adds methanol to scale, shake up, as need testing solution.Precision takes by weighing the astragaloside reference substance in addition, adds methanol and makes the solution that every lml contains 1mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), accurate need testing solution 2 to the 5 μ l that draw, reference substance solution 1 μ l and 3 μ l), the cross point is on same silica gel g thin-layer plate respectively, with [upper solution of n-butyl alcohol-ethyl acetate-water (4: 1: 5)]-methanol (10: 1.5) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 100 ℃, takes out, on lamellae, cover onesize glass plate, use immobilization with adhesive tape on every side, scan wavelength according to thin layer chromatography (an appendix VIB of Chinese Pharmacopoeia version in 2000 thin layer chromatography scanning): λ
S=530nm, λ
R=700nm measures test sample trap integrated value and reference substance trap integrated value, calculates, promptly.Every of this product contains the Radix Astragali with astragaloside (C
41H
68O
14) meter, must not be less than 0.40mg.
Claims (14)
1, a kind of Chinese medicine composition for the treatment of weakness due to chronic disease and the menoxenia of women's anemia deficiency of vital energy is characterized in that this Chinese medicine composition made by following raw material medicaments:
Colla Corii Asini 170-250 weight portion Radix Astragali 140-230 weight portion Radix Codonopsis 140-230 weight portion
Radix Rehmanniae Preparata 80-170 weight portion Rhizoma Atractylodis Macrocephalae 50-140 weight portion Radix Angelicae Sinensis 30-90 weight portion.
2, Chinese medicine composition as claimed in claim 1 is characterized in that this Chinese medicine composition made by following raw material medicaments:
The Colla Corii Asini 216 weight portion Radixs Astragali 180 weight portion Radix Codonopsis 180 weight portions
The Radix Rehmanniae Preparata 120 weight portion Rhizoma Atractylodis Macrocephalaes 90 weight portion Radix Angelicae Sinensis 60 weight portions.
3, Chinese medicine composition as claimed in claim 1 is characterized in that this Chinese medicine composition made by following raw material medicaments:
The Colla Corii Asini 240 weight portion Radixs Astragali 220 weight portion Radix Codonopsis 220 weight portions
The Radix Rehmanniae Preparata 150 weight portion Rhizoma Atractylodis Macrocephalaes 130 weight portion Radix Angelicae Sinensis 80 weight portions.
4, Chinese medicine composition as claimed in claim 1 is characterized in that this Chinese medicine composition made by following raw material medicaments:
The Colla Corii Asini 180 weight portion Radixs Astragali 160 weight portion Radix Codonopsis 160 weight portions
The Radix Rehmanniae Preparata 90 weight portion Rhizoma Atractylodis Macrocephalaes 65 weight portion Radix Angelicae Sinensis 45 weight portions.
5, as the described Chinese medicine composition of claim 1-4, it is characterized in that this Chinese medicine composition can add adjuvant and make and comprise in oral liquid, tablet, capsule, syrup, drop pill, pill, the injection any, preferred oral liquid preparation, concentrated pill.
6, the preparation method of oral liquid as claimed in claim 5, it is characterized in that this method is: above Six-element, it is suitably disconnected broken to get Radix Angelicae Sinensis, the Rhizoma Atractylodis Macrocephalae, distills, the collection distillate is standby, the residue and the Radix Astragali, Radix Codonopsis, Radix Rehmanniae Preparata decoct with water 2-4 time, and each 1-2.5 hour, collecting decoction, filter, it is the clear paste of 1.0-1.20 that filtrate is concentrated into 65 ℃ of-85 ℃ of relative densities, after the cooling, adds ethanol and makes the alcohol amount of containing be 45-60%; Stir evenly, cooling is left standstill, and filters, and filtrate recycling ethanol is concentrated into relative density and is 1.0-1.15, and is standby; Get Colla Corii Asini and add the suitable quantity of water fusing, filter, filtrate and above-mentioned concentrated solution merge; Sucrose is made syrup, merges with above-mentioned concentrated solution, distillate, adds antiseptic, and adjusting total amount is 2000 parts by volume, leaves standstill, filter, and embedding, sterilization, promptly.
7, the preparation method of oral liquid as claimed in claim 6, it is characterized in that this method is: it is suitably disconnected broken to get Radix Angelicae Sinensis, the Rhizoma Atractylodis Macrocephalae, distills, and it is standby to collect distillate, the residue and the Radix Astragali, Radix Codonopsis, Radix Rehmanniae Preparata decoct with water 3 times, 1.5 hours for the first time, second and third time each 1 hour, collecting decoction, filter, it is the clear paste of 1.08-1.10 that filtrate is concentrated into 75 ℃ of-80 ℃ of relative densities, after the cooling, adds ethanol and makes the alcohol amount of containing be 50-55%; Stir evenly, cooling is left standstill, and filters, and filtrate recycling ethanol is concentrated into relative density and is 1.08, and is standby; Get Colla Corii Asini and add the suitable quantity of water fusing, filter, filtrate and above-mentioned concentrated solution merge; Sucrose is made syrup, merges with above-mentioned concentrated solution, distillate, and the adding antiseptic is an amount of, and the adjustment total amount is 2000ml, leaves standstill, filter, and embedding, sterilization, promptly.
8, the preparation method of concentrated pill as claimed in claim 5, it is characterized in that this method is: Colla Corii Asini is ground into fine powder, and is standby; Get Radix Angelicae Sinensis, the Rhizoma Atractylodis Macrocephalae distills, it is standby to collect distillate, residue and the Radix Astragali, Radix Codonopsis, Radix Rehmanniae Preparata decoct with water 2-4 time, at every turn during 1-2.5, collecting decoction filters, and it is the clear paste of 1.0-1.20 that filtrate is concentrated into 65 ℃ of-85 ℃ of relative densities, after the cooling, add ethanol and make the alcohol amount of containing be 45-60%, stir evenly, leave standstill, filter, filtrate recycling ethanol is concentrated into thick paste, add above-mentioned distillate, donkey-hide gelatin fine powder, mixing is made concentrated pill, oven dry, polishing, promptly.
9, the preparation method of concentrated pill as claimed in claim 7, it is characterized in that this method is: Colla Corii Asini is ground into fine powder, and is standby; Get Radix Angelicae Sinensis, the Rhizoma Atractylodis Macrocephalae distills, it is standby to collect distillate, the residue and the Radix Astragali, Radix Codonopsis, Radix Rehmanniae Preparata decoct with water three times, 1.5 hours for the first time, second and third time each 1 hour, collecting decoction, filter, it is the clear paste of 1.08-1.10 that filtrate is concentrated into 75 ℃ of-80 ℃ of relative densities, after the cooling, adding ethanol makes the alcohol amount of containing be 50-55%, stir evenly, leave standstill, filter, filtrate recycling ethanol, be concentrated into thick paste, add above-mentioned distillate, donkey-hide gelatin fine powder and adjuvant, mixing, make concentrated pill, oven dry, total amount 400 weight portions, polishing, promptly.
10, require the method for quality control of the described Chinese medicinal composition preparation of 1-4 as profit, it is characterized in that discrimination method in this method comprises one or more in the following discriminating:
A. get this composition oral liquid 40ml, the jolting that adds diethyl ether is extracted 1-3 time, and each 50ml divides and gets ether layer, volatilizes, and residue adds ethyl acetate 0.5ml makes dissolving, as need testing solution; Other gets Radix Angelicae Sinensis control medicinal material 0.2g, and the 30ml that adds diethyl ether flooded 1 hour, the time add jolting, filter, filtrate volatilizes, residue adds ethyl acetate 0.5ml makes dissolving, in contrast medical material solution; According to thin layer chromatography test, draw need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with 8-12: 1-3 normal hexane-ethyl acetate is developing solvent, launches, and takes out, and dries, and puts under the 365nm ultraviolet light and inspects; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical light blue white fluorescent speckle;
B. get this composition oral liquid 40ml, add ethyl acetate extraction 1-3 time, each 40ml divides and gets ethyl acetate liquid, and evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Rhizoma Atractylodis Macrocephalae control medicinal material 2g, adds water 30ml, and reflux 1 hour filters, and filtrate adds ethyl acetate and shines medical material solution in pairs with legal system; According to 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, be developing solvent with chloroform-acetone-formic acid of 18-21: 1-3: 0.1-0.5, 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 same color fluorescence principal spot;
C. according to the thin layer chromatography test, precision is measured this composition oral liquid 25ml under the loading amount item, uses ether extraction 1-3 time, each 30ml divides and takes off a layer solution, with water saturated n-butanol extraction 5 times, each 25ml merges n-butanol extracting liquid, extracts 3 times with ammonia solution, each 20ml, divide and get n-butyl alcohol liquid, evaporate to dryness, residue add 10% ethanol 5ml makes dissolving, put coldly, pass through D
101The type macroporous adsorptive resins, with water 50ml eluting, discard water liquid, reuse 30-50% ethanol 30ml eluting, discard the 30-50% ethanol elution, continue with 60-80% ethanol 100ml eluting, collect eluent, evaporate to dryness, with dissolve with methanol and be transferred in the 2ml measuring bottle, add methanol to scale, shake up, as need testing solution; Precision takes by weighing the astragaloside reference substance in addition, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Draw each 5 μ l of need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with 11-15: 5-8: lower floor's solution that 1-4 chloroform-methanol-water is placed below 10 ℃ is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing at 100 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, daylight shows down identical sepia speckle; The 365nm ultra-violet lamp shows identical orange-yellow fluorescence speckle down.
11, require the method for quality control of 10 described Chinese medicine compositions as profit, its feature comprises one or more of following discriminating at the discrimination method that is used for oral liquid formulations:
A. get this product 40ml, the jolting that adds diethyl ether is extracted 2 times, and each 50ml divides and gets ether layer, volatilizes, and residue adds ethyl acetate 0.5ml makes dissolving, as need testing solution; Other gets Radix Angelicae Sinensis control medicinal material 0.2g, and the 30ml that adds diethyl ether flooded 1 hour, the time add jolting, filter, filtrate volatilizes, residue adds ethyl acetate 0.5ml makes dissolving, in contrast medical material solution; According to the thin layer chromatography test, draw need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, be developing solvent with 9: 1 normal hexane-ethyl acetates, launch, take out, dry, put under the 365nm ultraviolet light and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical light blue white fluorescent speckle;
B. get this product 40ml, add ethyl acetate extraction 2 times, each 40ml divides and gets ethyl acetate liquid, and evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Rhizoma Atractylodis Macrocephalae control medicinal material 2g, adds water 30ml, and reflux 1 hour filters, and filtrate adds ethyl acetate and 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, be developing solvent with 19: 1: 0.2 chloroform-acetone-formic acid, 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 same color fluorescence principal spot;
C. according to the thin layer chromatography test, precision is measured this composition oral liquid 25ml under the loading amount item, uses ether extraction 2 times, each 30ml divides and takes off a layer solution, with water saturated n-butanol extraction 5 times, each 25ml merges n-butanol extracting liquid, extracts 3 times with ammonia solution, each 20ml, divide and get n-butyl alcohol liquid, evaporate to dryness, residue add 10% ethanol 5ml makes dissolving, put coldly, pass through D
101The type macroporous adsorptive resins, internal diameter 1cm, long 15cm, with water 50ml eluting, discard water liquid, reuse 40% ethanol 30ml eluting, discard 40% ethanol elution, continue with 70% ethanol 100ml eluting, collect eluent, evaporate to dryness, with dissolve with methanol and be transferred in the 2ml measuring bottle, add methanol to scale, shake up, as need testing solution; Precision takes by weighing the astragaloside reference substance in addition, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Draw each 5 μ l of need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, lower floor's solution of placing below 10 ℃ with 13: 6: 2 chloroform-methanol-water is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 100 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, daylight shows down identical sepia speckle; The 365nm ultra-violet lamp shows identical orange-yellow fluorescence speckle down.
12, require the method for quality control of the described Chinese medicine composition of 1-4 as profit, it is characterized in that the content assaying method in this method is: precision is measured this composition oral liquid 25ml under the loading amount item, uses ether extraction 1-3 time, each 30ml divides and takes off a layer solution, with water saturated n-butanol extraction 4-6 time, each 25ml merges n-butanol extracting liquid, extracts 2-4 time with ammonia solution, each 20ml, divide and get n-butyl alcohol liquid, evaporate to dryness, residue add 10% ethanol 5ml makes dissolving, put coldly, pass through D
101The type macroporous adsorptive resins, with water 50ml eluting, discard water liquid, reuse 30-50% ethanol 30ml eluting, discard the 30-50% ethanol elution, continue with 60-80% ethanol 100ml eluting, collect eluent, evaporate to dryness, with dissolve with methanol and be transferred in the 2ml measuring bottle, add methanol to scale, shake up, as need testing solution; Precision takes by weighing the astragaloside reference substance in addition, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, accurate need testing solution 2 to 5 μ l, reference substance solution 1 μ l and the 3 μ l of drawing, the cross point is on same silica gel g thin-layer plate respectively, with [n-butyl alcohol-ethyl acetate-water (3-5: 1-3: upper solution 4-7)]-methanol (9-12: 1-3) be developing solvent, launch, take out, dry, spray is with the 9-12% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 100 ℃, takes out, on lamellae, cover onesize glass plate, use immobilization with adhesive tape on every side, scan wavelength according to thin layer chromatography: λ
s=530nm, λ
R=700nm measures test sample trap integrated value and reference substance trap integrated value, calculates, that is, every 20ml contains the Radix Astragali in astragaloside, must not be less than 0.40mg.
13, require the method for quality control of 12 described Chinese medicine compositions as profit, it is characterized in that the content assaying method that is used for oral liquid formulations is: precision is measured this composition oral liquid 25ml under the loading amount item, uses ether extraction 2 times, each 30ml divides and takes off a layer solution, with water saturated n-butanol extraction 5 times, each 25ml merges n-butanol extracting liquid, extracts 3 times with ammonia solution, each 20ml, divide and get n-butyl alcohol liquid, evaporate to dryness, residue add 10% ethanol 5ml makes dissolving, put coldly, pass through D
101The type macroporous adsorptive resins, internal diameter 1cm, long 15cm, with water 50ml eluting, discard water liquid, reuse 40% ethanol 30ml eluting, discard 40% ethanol elution, continue with 70% ethanol 100ml eluting, collect eluent, evaporate to dryness, with dissolve with methanol and be transferred in the 2ml measuring bottle, add methanol to scale, shake up, as need testing solution; Precision takes by weighing the astragaloside reference substance in addition, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, accurate need testing solution 2 to 5 μ l, reference substance solution 1 μ l and the 3 μ l of drawing), the cross point is on same silica gel g thin-layer plate respectively, with [upper solution of n-butyl alcohol-ethyl acetate-water (4: 1: 5)]-methanol (10: 1.5) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 100 ℃, takes out, on lamellae, cover onesize glass plate, use immobilization with adhesive tape on every side, scan wavelength according to thin layer chromatography: λ
s=530nm, λ
R=700nm measures test sample trap integrated value and reference substance trap integrated value, calculates, that is, every 20ml contains the Radix Astragali in astragaloside, must not be less than 0.40mg.
14, the method for quality control as the described Chinese medicine composition of claim 1-4 comprises the steps:
Differentiate: a. gets this composition oral liquid 40ml, and the jolting that adds diethyl ether is extracted 1-3 time, and each 50ml divides and gets ether layer, volatilizes, and residue adds ethyl acetate 0.5ml makes dissolving, as need testing solution; Other gets Radix Angelicae Sinensis control medicinal material 0.2g, and the 30ml that adds diethyl ether flooded 1 hour, the time add jolting, filter, filtrate volatilizes, residue adds ethyl acetate 0.5ml makes dissolving, in contrast medical material solution; According to thin layer chromatography test, draw need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with 8-12: 1-3 normal hexane-ethyl acetate is developing solvent, launches, and takes out, and dries, and puts under the 365nm ultraviolet light and inspects; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical light blue white fluorescent speckle;
B. get this composition oral liquid 40ml, add ethyl acetate extraction 1-3 time, each 40ml divides and gets ethyl acetate liquid, and evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Rhizoma Atractylodis Macrocephalae control medicinal material 2g, adds water 30ml, and reflux 1 hour filters, and filtrate adds ethyl acetate and shines medical material solution in pairs with legal system; According to 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, be developing solvent with chloroform-acetone-formic acid of 18-21: 1-3: 0.1-0.5, 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 same color fluorescence principal spot;
C. according to the thin layer chromatography test, precision is measured this composition oral liquid 25ml under the loading amount item, uses ether extraction 1-3 time, each 30ml divides and takes off a layer solution, with water saturated n-butanol extraction 5 times, each 25ml merges n-butanol extracting liquid, extracts 3 times with ammonia solution, each 20ml, divide and get n-butyl alcohol liquid, evaporate to dryness, residue add 10% ethanol 5ml makes dissolving, put coldly, pass through D
101The type macroporous adsorptive resins, with water 50ml eluting, discard water liquid, reuse 30-50% ethanol 30ml eluting, discard the 30-50% ethanol elution, continue with 60-80% ethanol 100ml eluting, collect eluent, evaporate to dryness, with dissolve with methanol and be transferred in the 2ml measuring bottle, add methanol to scale, shake up, as need testing solution; Precision takes by weighing the astragaloside reference substance in addition, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Draw each 5 μ l of need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with 11-15: 5-8: lower floor's solution that 1-4 chloroform-methanol-water is placed below 10 ℃ is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing at 100 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, daylight shows down identical sepia speckle; The 365nm ultra-violet lamp shows identical orange-yellow fluorescence speckle down;
Assay: precision is measured this composition oral liquid 25ml under the loading amount item, uses ether extraction 1-3 time, each 30ml, divide and to take off a layer solution, with water saturated n-butanol extraction 4-6 time, 25ml at every turn, merge n-butanol extracting liquid, extract 2-4 time with ammonia solution, each 20ml divides and gets n-butyl alcohol liquid, evaporate to dryness, residue adds 10% ethanol 5ml makes dissolving, puts coldly, passes through D
101The type macroporous adsorptive resins, with water 50ml eluting, discard water liquid, reuse 30-50% ethanol 30ml eluting, discard the 30-50% ethanol elution, continue with 60-80% ethanol 100ml eluting, collect eluent, evaporate to dryness, with dissolve with methanol and be transferred in the 2ml measuring bottle, add methanol to scale, shake up, as need testing solution; Precision takes by weighing the astragaloside reference substance in addition, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, accurate need testing solution 2 to 5 μ l, reference substance solution 1 μ l and the 3 μ l of drawing, the cross point is on same silica gel g thin-layer plate respectively, with [n-butyl alcohol-ethyl acetate-water (3-5: 1-3: upper solution 4-7)]-methanol (9-12: 1-3) be developing solvent, launch, take out, dry, spray is with the 9-12% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 100 ℃, takes out, on lamellae, cover onesize glass plate, use immobilization with adhesive tape on every side, scan wavelength according to thin layer chromatography: λ
s=530nm, λ
R=700nm measures test sample trap integrated value and reference substance trap integrated value, calculates, that is, every 20ml contains the Radix Astragali in astragaloside, must not be less than 0.40mg.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102626462A (en) * | 2011-08-08 | 2012-08-08 | 李延忠 | Pharmaceutical composition with blood-enriching and leukogenic efficacy |
| CN102698075A (en) * | 2012-05-15 | 2012-10-03 | 陈少敏 | Health-care herb tea used after gynecological operation, and preparation method thereof |
| CN107929420A (en) * | 2017-11-23 | 2018-04-20 | 江西天元药业有限公司 | Improve energy and blood of human body function and improve the Chinese medicine composition and detection method of immunity |
| CN114246888A (en) * | 2018-05-21 | 2022-03-29 | 成都中医大华神药业有限责任公司 | Detection method of folium artemisiae argyi charcoal |
-
2004
- 2004-02-06 CN CNB2004100391069A patent/CN100502899C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102626462A (en) * | 2011-08-08 | 2012-08-08 | 李延忠 | Pharmaceutical composition with blood-enriching and leukogenic efficacy |
| CN102698075A (en) * | 2012-05-15 | 2012-10-03 | 陈少敏 | Health-care herb tea used after gynecological operation, and preparation method thereof |
| CN107929420A (en) * | 2017-11-23 | 2018-04-20 | 江西天元药业有限公司 | Improve energy and blood of human body function and improve the Chinese medicine composition and detection method of immunity |
| CN107929420B (en) * | 2017-11-23 | 2021-01-19 | 江西天元药业有限公司 | Traditional Chinese medicine composition for improving qi and blood functions and immunity of human body and detection method |
| CN114246888A (en) * | 2018-05-21 | 2022-03-29 | 成都中医大华神药业有限责任公司 | Detection method of folium artemisiae argyi charcoal |
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| CN100502899C (en) | 2009-06-24 |
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