CN1814127A - Shenbao preparation, its preparing method and quality control method - Google Patents
Shenbao preparation, its preparing method and quality control method Download PDFInfo
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- CN1814127A CN1814127A CN 200510200743 CN200510200743A CN1814127A CN 1814127 A CN1814127 A CN 1814127A CN 200510200743 CN200510200743 CN 200510200743 CN 200510200743 A CN200510200743 A CN 200510200743A CN 1814127 A CN1814127 A CN 1814127A
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Landscapes
- Cosmetics (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a Shenbao preparation, relating to the preparing method and quality control method thereof. It has advantages of good stability, no sugar, no antiseptic, convenient to take and carry, suitable to industrialized production, low production cost, etc, and great marketing potential, and the quality control method can identify Chinese Angelica, Rhizoma Chuanxiong, Common Cnidium Fruit, prepared Tuber Fleeceflower Root, Epimedium Herb, and Malaytea Scurfpea Fruit in the Shenbao preparation, and making content determination on active substance of prepared Tuber Fleeceflower Root-2, 3, 5, 4'-tetrahydroxy diphenylethylene -2-0-b-D- glucoside, active substance of Epimedium Herb-Icariin, active substance ofCommon Cnidium Fruit-Osthole, and active substance of Chinese Magnoliavine Fruit- Chinese Magnoliavine Fruit methanol.
Description
Technical field
The present invention relates to a kind of Chinese medicine preparation, particularly relate to Shenbao preparation, relate to the preparation method method of quality control of said preparation simultaneously.
Background technology
The sexual impotence that causes by suffering from a deficiency of the kidney, seminal emission, soreness of waist pain, fear of cold is afraid of cold, nocturia, and diseases such as spiritlessness and weakness, alopecia tinnitus, women leucorrhea, menorrhagia are common clinically common frdquently encountered disease diseases, the renal aid prescription is rigorous, and compatibility is thorough, has YIN and YANG balance regulating, temperature male wind-supplying kidney, the controlling nocturnal emission with astringent drugs of calming the nerves, the merit of strengthening the body resistance, the product of regulating the flow of vital energy with yin nourishing because of Fang Zhongzuo, oiliness so mend, temperature and not dry, the good medicine of nourishing for the four seasons.Clinically be widely used in above-mentioned disease, evident in efficacy.
Shenbao preparation is the Chinese medicine preparation of being processed into through extraction by 22 flavor Chinese medicines such as Herba Epimedii, Radix Polygoni Multiflori Preparata, existing SHENBAO HEJI, renal aid syrup on the market, its prescription and method of quality control all record for the standard laid down by the ministries or commissions of the Central Government, both quality standard basically identicals, the existing syrupy quality standard of renal aid that records with the standard laid down by the ministries or commissions of the Central Government is:
[prescription] Fructus Cnidii 28g Rhizoma Chuanxiong 28.3g Semen Cuscutae 66g
Fructus Psoraleae 28.5g Poria 30g Radix Ginseng Rubra 20g
Fructus Foeniculi 14.4g Fructus Schisandrae Chinensis 36g Fructus Rosae Laevigatae 94.6g
Rhizoma Atractylodis Macrocephalae 14.2g Radix Angelicae Sinensis 46.8g Fructus Rubi 32.9g
Radix Polygoni Multiflori Preparata 74.4g Semen Plantaginis 16.5g Radix Rehmanniae Preparata 94g
Fructus Lycii 66g Rhizoma Dioscoreae 46.3g Herba Epimedii 94.6g
Semen Trigonellae 94g Radix Astragali 51.4g Herba Cistanches 47.3g
Radix Glycyrrhizae Preparata 14.2g
[method for making] above 22 flavors, Fructus Cnidii, Herba Epimedii, Radix Angelicae Sinensis, Rhizoma Chuanxiong, Fructus Foeniculi are ground into coarse powder, according to the percolation under fluid extract and the extractum item (appendix IO), make solvent with 70% ethanol, flood after 48 hours, with the speed of per minute 1～3ml percolation slowly, collect percolate 1500ml, reclaim ethanol, being evaporated to relative density is the clear paste of 1.10 (80 ℃ of heat are surveyed), filter filtrate for later use; Red ginseng powder is broken into coarse powder, adds 20% alcohol dipping after 8 hours, the reflux, extract, secondary, and each 2 hours, merge extractive liquid, filtered, and filtrate recycling ethanol is concentrated into relative density and is the clear paste of 1.10 (80 ℃ of heat are surveyed), and is standby; Ten Six-elements such as all the other Fructus Rubies, after suitably cataclasm,, decoct with water secondary with the medicinal residues of Radix Ginseng Rubra through alcohol extraction, each 2 hours, collecting decoction filters, and filtrate is concentrated into the clear paste that relative density is 1.16 (80 ℃ of heat are surveyed), adding ethanol makes and contains alcohol amount and reach 65%, left standstill 48 hours, and got supernatant and reclaim ethanol, being concentrated into relative density is the clear paste of 1.10 (80 ℃ of heat are surveyed).The alcohol extract that adds extracting solution such as above-mentioned Fructus Cnidii and Radix Ginseng Rubra, mixing adds the about 700ml of simple syrup, boils 10 minutes, and it is an amount of to add sodium benzoate, adds water to 1000ml, filtration, promptly.
[character] this product is tan thick liquid; Sweet, little hardship of distinguishing the flavor of.
This product 40ml is got in [discriminating] (1), puts in the separatory funnel, adds hydrochloric acid 2ml and ether 40ml, and jolting is extracted, and divides and gets ether layer, and evaporate to dryness, residue add methanol 1ml makes dissolving, and 2～3 of dropping sodium test solutions promptly show red.
(2) get this product 10ml, put in the separatory funnel, add petroleum ether (30～60 ℃), 10ml, jolting is extracted, petroleum ether extract is put in the evaporating dish, volatilizes, and adds methanol 1ml and makes dissolving, add 2%3,2 of the methanol saturated solutions of 2～3 of the methanol solutions of 5-dinitrobenzoic acid and potassium hydroxide, heating promptly shows reddish violet.
(3) get this product 10ml, by H type strongly acidic cation-exchange post (the internal diameter 1cm that has handled well, storng-acid cation exchange resin 2g), wash with water to effluent colourless, discard water lotion, reuse (2mol/L) ammonia solution 50ml eluting discards colourless first washing liquid, collects continuous washing liquid 30ml, put evaporate to dryness in the water-bath, residue adds 3% hydrochloric acid solution 3ml makes dissolving, filters, and filtrate is placed in 3 test tubes, add the silico-tungstic acid test solution respectively, each 2 of bismuth potassium iodide test solution and test solution of mercuric potassium iodide promptly generate the light brown precipitation respectively, red-brown precipitation and brown precipitate.
[inspection] relative density should be not less than 1.26.
PH value should be 4.2～5.5.
Other should meet every regulation relevant under the syrup item.
[function with cure mainly] YIN and YANG balance regulating, temperature male wind-supplying kidney, the controlling nocturnal emission with astringent drugs of calming the nerves, strengthening the body resistance.Be used for sexual impotence, seminal emission, waist and leg ache, lassitude, nocturia, fear of cold is afraid of cold; Women's menorrhagia, all diseases of clear and thin leucorrhea.
[usage and consumption] is oral, a 10～20ml, 3 times on the one.
[attention] cold, fever phase withdraws.
[specification] every 10ml, every bottle of 100ml, 200ml
Shady and cool dry place is put in [storage] sealing.
The subject matter that prior art exists is: (1) liquid preparation instability, put easy generation precipitation for a long time; (2) production cost height, and carry transportation inconvenience; (3) existing dosage form all contains antiseptic; (4) all there is the high deficiency of sugar content in existing dosage form, is unsuitable for diabetes, hepatopath etc. and takes; (5) quality control standard of existing preparation is low, one of discriminating three physicochemical identification is only arranged, and specificity is poor, and does not have assay, and difficulty is really controlled product quality.
The invention provides a kind of Shenbao preparation, overcome the weak point of above-mentioned preparation aspect, have good stability, do not contain antiseptic, take easy to carry, be suitable for advantages such as suitability for industrialized production, production cost be low.And owing to do not contain sugar, not only be suitable for general patient and take, and be suitable for comprising diabetics all be unsuitable for taking the patient who contains sugared medicine and take.A kind of method of quality control of Shenbao preparation is provided simultaneously, promptly can differentiate the Radix Angelicae Sinensis in the Shenbao preparation and Rhizoma Chuanxiong, Fructus Cnidii, Radix Polygoni Multiflori Preparata, Herba Epimedii with thin layer chromatography, with high-efficient liquid phase technique the Fructus Psoraleae in the Shenbao preparation is differentiated, measure in the Shenbao preparation 2 with high-efficient liquid phase technique, 3,5, the content of 4 '-tetrahydroxystilbene-2-O-b-D-glucoside, icariin, osthole, schisandrin.Shenbao preparation must be controlled product quality if can adopt above-mentioned discriminating and assay project to carry out Quality Control wholly or in part, guarantees the safe and effective of medication, improves the quality of product.
Summary of the invention
1. Shenbao preparation, this Chinese medicine is the solid preparation of Chinese medicine of being made by following Chinese medicinal raw materials, following proportioning can change in proportion,
Fructus Cnidii 28 weight portion Rhizoma Chuanxiongs 28.3 weight portion Semen Cuscutae 66 weight portions
Fructus Psoraleae 28.5 weight portion Poria 30 weight portion Radix Ginseng Rubra 20 weight portions
Fructus Foeniculi 14.4 weight portion Fructus Schisandrae Chinensis 36 weight portion Fructus Rosae Laevigatae 94.6 weight portions
The Rhizoma Atractylodis Macrocephalae 14.2 weight portion Radix Angelicae Sinensis 46.8 weight portion Fructus Rubies 32.9 weight portions
Radix Polygoni Multiflori Preparata 74.4 weight portion Semen Plantaginiss 16.5 weight portion Radix Rehmanniae Preparata 94 weight portions
Fructus Lycii 66 weight portion Rhizoma Dioscoreaes 46.3 weight portion Herba Epimedii 94.6 weight portions
The Semen Trigonellae 94 weight portion Radixs Astragali 51.4 weight portion Herba Cistanches 47.3 weight portions
Radix Glycyrrhizae Preparata 14.2 weight portions
Its preparation method process following steps:
(1) ethanol percolation or the reflux, extract, of Fructus Cnidii, Herba Epimedii, Radix Angelicae Sinensis, Rhizoma Chuanxiong, Fructus Foeniculi usefulness 50-80% in the prescription;
(2) ethanol percolation or the reflux, extract, of Radix Ginseng Rubra usefulness 10-50% in the prescription, medicinal residues are standby;
(3) all the other ten Six-elements such as Fructus Rubi are with above-mentioned Radix Ginseng Rubra medicinal residues in the prescription, and water is carried or water extract-alcohol precipitation;
(4) extracting solution of above-mentioned (1), (2), (3) gained is concentrated in right amount, mixing after mixing/adding appropriate amount of auxiliary materials, vacuum drying/spray drying/lyophilization;
(5) dried cream powder of above-mentioned (4) gained is made various solid preparations according to a conventional method.
Described solid preparation, the various solid dosage formss that comprise renal aid are as tablet, sugar coated tablet, film coated tablet, chewable tablet, effervescent tablet, dispersible tablet, capsule, hard capsule, soft capsule, pellt capsule, suck agent, electuary, granule, effervescent granule, pill, drop pill, pellet.
2. the method for quality control of a Shenbao preparation, contain in following assay and the qualitative identification one or more:
(1) assay a. measures in the Shenbao preparation 2,3,5 with high-efficient liquid phase technique, the content of 4 '-tetrahydroxystilbene-2-O-b-D-glucoside; B. measure content Determination of Icariin in the Shenbao preparation with high-efficient liquid phase technique; C. measure the content of osthole in the Shenbao preparation with high-efficient liquid phase technique; D. measure the content of schisandrin in the Shenbao preparation with high-efficient liquid phase technique.
(2) qualitative identification a. differentiates Radix Angelicae Sinensis and Rhizoma Chuanxiong in the Shenbao preparation with thin layer chromatography; B. differentiate Fructus Cnidii in the Shenbao preparation with thin layer chromatography; C. differentiate Radix Polygoni Multiflori Preparata in the Shenbao preparation with thin layer chromatography; D. differentiate Herba Epimedii in the Shenbao preparation with thin layer chromatography; E. differentiate Fructus Psoraleae in the Shenbao preparation with high-efficient liquid phase technique.
3. the method for quality control of a Shenbao preparation, contain in following assay and the qualitative identification one or more:
(1) assay
A. high-efficient liquid phase technique measures 2,3,5, the content of 4 '-tetrahydroxystilbene-2-O-b-D-glucoside
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels; Second eyeball-water (5-70: 95-30) be mobile phase; UV-detector or diode array detector.Number of theoretical plate is by 2,3,5, and 4 '-tetrahydroxystilbene-2-O-b-D-glucoside peak calculates should be not less than 2000.
The preparation precision of reference substance solution takes by weighing 2,3,5, and 4 '-tetrahydroxystilbene-2-O-b-D-glucoside reference substance adds ethanol or Diluted Alcohol or other The suitable solvent and makes the solution of determining concentration, product solution in contrast.
The preparation precision of need testing solution takes by weighing product or the product content thing is an amount of, with the methanol/ethanol extraction of suitable concentration, as need testing solution.
Accurate respectively reference substance solution and an amount of volume of need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly.
B. high-efficient liquid phase technique is measured icariin content in the Shenbao preparation
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels; Second eyeball-water (5-70: 95-30) be mobile phase; UV-detector or diode array detector.Number of theoretical plate calculates by the icariin peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the icariin reference substance, adds methanol or other The suitable solvent and makes the solution of determining concentration, product solution in contrast.
The preparation precision of need testing solution takes by weighing product or the product content thing is an amount of, adds the suitable quantity of water dissolving, extract with ethyl acetate or other The suitable solvent, and the extracting solution evaporate to dryness, residue dissolves with The suitable solvent, as need testing solution.
Accurate respectively absorption reference substance solution of algoscopy and need testing solution are an amount of, inject chromatograph of liquid, measure promptly.
C. high-efficient liquid phase technique is measured osthole content in the Shenbao preparation
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels; Methanol-water (40-85: 60-15) be mobile phase; UV-detector or diode array detector.Number of theoretical plate calculates by the osthole peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the osthole reference substance, adds methanol or other The suitable solvent and makes the solution of determining concentration, product solution in contrast.
The preparation precision of need testing solution takes by weighing product or the product content thing is an amount of, with the methanol/ethanol extraction of suitable concentration, as need testing solution.
Accurate respectively absorption reference substance solution of algoscopy and need testing solution are an amount of, inject chromatograph of liquid, measure promptly.
D. high-efficient liquid phase technique is measured schisandrin content in the Shenbao preparation
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels; Methanol-water (5-30: 2-15) be mobile phase; UV-detector or diode array detector.Number of theoretical plate calculates by the schisandrin peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the schisandrin reference substance, adds methanol or other The suitable solvent and makes the solution of determining concentration, product solution in contrast.
The preparation precision of need testing solution takes by weighing product or the product content thing is an amount of, with the methanol/ethanol extraction of suitable concentration, as need testing solution.
Accurate respectively absorption reference substance solution of algoscopy and need testing solution are an amount of, inject chromatograph of liquid, measure promptly.
(2) qualitative identification
A. thin layer chromatography is differentiated Radix Angelicae Sinensis and Rhizoma Chuanxiong in the Shenbao preparation
Get product or the product content thing is an amount of, add diethyl ether or other The suitable solvent is extracted, extracting solution is as need testing solution, or extracting solution steams/volatilize, and residue adds The suitable solvent makes dissolving, as need testing solution.Other gets Radix Angelicae Sinensis and the Rhizoma Chuanxiong control medicinal material is an amount of, makes control medicinal material solution after the extraction.Each is an amount of to draw above-mentioned need testing solution and control medicinal material solution, puts respectively on same silica gel G or silica gel H lamellae, with normal hexane-ethyl acetate (3-20: 0.3-2) be developing solvent, launch, take out, dry, put under the ultra-violet lamp and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
B. thin layer chromatography is differentiated Fructus Cnidii in the Shenbao preparation
Get product or the product content thing is an amount of, add diethyl ether or other The suitable solvent is extracted, extracting solution is as need testing solution, or extracting solution steams/volatilize, and residue adds The suitable solvent makes dissolving, as need testing solution.It is an amount of that other gets the osthole reference substance, and solubilizer is made reference substance solution in right amount.Each is an amount of to draw above-mentioned need testing solution and reference substance solution, puts respectively on same silica gel G or silica gel H lamellae, with cyclohexane extraction-ethyl acetate (3-20: 0.5-5) be developing solvent, launch, take out, dry, put under the ultra-violet lamp and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
C. thin layer chromatography is differentiated Radix Polygoni Multiflori Preparata in the Shenbao preparation
Get product or the product content thing is an amount of, adding ethyl acetate or other The suitable solvent extracts, extracting solution extracts with the sodium carbonate liquor of suitable concentration, sodium carbonate extraction liquid hydrochloric acid adjust pH to 1～4, reuse ethyl acetate or the extraction of other The suitable solvent, extract is as need testing solution, or extract steams/volatilizes, residue adds The suitable solvent makes dissolving, as need testing solution.It is an amount of that other gets the Radix Polygoni Multiflori control medicinal material, makes control medicinal material solution after the extraction.It is an amount of to get the emodin reference substance again, and solubilizer is made reference substance solution in right amount.Each is an amount of to draw above-mentioned need testing solution, control medicinal material and reference substance solution, put respectively on same silica gel G or silica gel H lamellae, (5-25: 2-8: upper solution 0.4-2) is developing solvent with petroleum ether (30～60 ℃)-Ethyl formate-formic acid, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show identical orange-yellow fluorescence speckle.Put in the ammonia steam smoked after, inspect under the daylight, speckle becomes redness.
D. thin layer chromatography is differentiated Herba Epimedii in the Shenbao preparation
Get product or the product content thing is an amount of, add n-butyl alcohol or other The suitable solvent and extract, extracting solution washs with ammonia solution, discards ammonia solution, and extracting solution is as need testing solution, or extracting solution steams/volatilize, and residue adds The suitable solvent makes dissolving, as need testing solution.Other gets the icariin reference substance, and solubilizer is made reference substance solution in right amount.Each is an amount of to draw above-mentioned two kinds of solution, put respectively on same silica gel G or silica gel H lamellae, with ethyl acetate-butanone-formic acid-water (3-30: 0.4-4: 0.4-4: 0.4-4) be developing solvent, launch, take out, dry, spray is heated to colour developing with 10% ethanol solution of sulfuric acid, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
E. high-efficient liquid phase technique is differentiated Fructus Psoraleae in the Shenbao preparation
Get product or the product content thing is an amount of, add methanol or other The suitable solvent and extract, extracting solution is as need testing solution.Other gets psoralen and the isopsoralen reference substance is an amount of, and solubilizer is made reference substance solution in right amount.With the octadecylsilane chemically bonded silica is filler; Methanol-water (20-80: 80-20) be mobile phase, UV-detector or diode array detector.Accurate respectively reference substance solution and each an amount of volume of need testing solution drawn injects chromatograph of liquid, measures.The retention time of main peak should be consistent with reference substance in the test sample chromatogram.
Described extraction can be adopted conventional methods such as supersound process, reflux, extract,, microwave extraction, vibration extraction;
2,3,5, the mobile phase of the assay of 4 '-tetrahydroxystilbene-2-O-b-D-glucoside can also be methanol-acetonitrile-water (2-10: 0.5-2: 4-20), methanol-water (5-70: 95-30) or other suitable mobile phase;
The mobile phase that content Determination of Icariin is measured can also be methanol-water-glacial acetic acid (40-80: 20-60: 0.2-1), methanol-water (5-70: 95-30) or other suitable mobile phase;
The mobile phase of the assay of osthole can also be methanol-water-oxolane (30-75: 20-60: 2-10), acetonitrile-water (5-70: 95-30) or other suitable mobile phase;
The mobile phase of schisandrin assay can also be acetonitrile-water (5-70: 95-30) or other suitable mobile phase;
The developing solvent that the thin layer chromatography of Radix Angelicae Sinensis and Rhizoma Chuanxiong is differentiated can also be petroleum ether-ethyl acetate (5-25: 0.5-5), cyclohexane extraction-ethyl acetate (5-25: 0.5-5) or other suitable developing solvent;
The developing solvent that the thin layer chromatography of Fructus Cnidii is differentiated can also be benzene-ethyl acetate (10-50: 0.3-2), normal hexane-ethyl acetate (4-20: 0.4-4) or other suitable developing solvent;
The developing solvent that the thin layer chromatography of Radix Polygoni Multiflori Preparata is differentiated can also be chloroform-methanol (5-15: 0.5-5), petroleum ether (30-60 ℃)-ethyl acetate-glacial acetic acid (50-150: 5-50: 0.5-5) or other suitable developing solvent;
Both can adopt reference substance among qualitative identification a, b, c, the d, and also can adopt control medicinal material to compare, or both all adopt; Both can adopt two kinds of reference substances among the qualitative identification e, also can only adopt wherein a kind of reference substance in contrast.
4. the method for quality control of a Shenbao preparation, contain in following assay and the qualitative identification one or more:
(1) assay
A. high-efficient liquid phase technique measures 2,3,5, the content of 4 '-tetrahydroxystilbene-2-O-b-D-glucoside
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Second eyeball-water (25: 75) is mobile phase; The detection wavelength is 320nm.Number of theoretical plate is by 2,3,5, and 4 '-tetrahydroxystilbene-2-O-b-D-glucoside peak calculates should be not less than 2000.
The preparation precision of reference substance solution takes by weighing 2,3,5, and 4 '-tetrahydroxystilbene-2-O-b-D-glucoside reference substance adds Diluted Alcohol and makes the solution that every 1ml contains 20ug, promptly.
Product is got in the preparation of need testing solution or the product content thing is an amount of, puts in the conical flask, and the accurate Diluted Alcohol 50ml that adds claims decide weight, and reflux 30 minutes is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with Diluted Alcohol, shakes up, and filtration is got subsequent filtrate, promptly.
Accurate respectively reference substance solution and each 20ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures promptly.
B. high-efficient liquid phase technique is measured icariin content in the Shenbao preparation
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Second eyeball-water (30: 70) is mobile phase; The detection wavelength is 270nm.Number of theoretical plate calculates by the icariin peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the icariin reference substance, adds methanol and makes the solution that every 1ml contains 40ug, promptly.
Product is got in the preparation of need testing solution or the product content thing is an amount of, adds water 10ml, puts in the tool plug separatory funnel, uses ethyl acetate extraction 4 times, each 10ml, combined ethyl acetate layer, evaporate to dryness, residue add dissolve with methanol and are transferred in the 25ml measuring bottle, add methanol to scale, shake up, promptly.
Accurate respectively reference substance solution and the need testing solution 20ml of drawing of algoscopy injects chromatograph of liquid, measures promptly.
C. high-efficient liquid phase technique is measured osthole content in the Shenbao preparation
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (67: 33) is a mobile phase; The detection wavelength is 249nm.Number of theoretical plate calculates by the osthole peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the osthole reference substance, adds methanol and makes the solution that every 1ml contains 50ug, promptly.
Product is got in the preparation of need testing solution or the product content thing is an amount of, puts in the tool plug conical flask, the accurate ethanol 50ml that adds, and close plug claims to decide weight, and supersound process 1 hour claims to decide weight again, supplies the weight that subtracts mistake with ethanol, shakes up, and filters, and gets subsequent filtrate, promptly.
Accurate respectively reference substance solution and the need testing solution 20ml of drawing of algoscopy injects chromatograph of liquid, measures, promptly.
D. high-efficient liquid phase technique is measured schisandrin content in the Shenbao preparation
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (13: 7) is a mobile phase; The detection wavelength is 250nm.Number of theoretical plate calculates by the schisandrin peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the schisandrin reference substance, adds methanol and makes the solution that every 1ml contains 30ug, promptly.
Product is got in the preparation of need testing solution or the product content thing is an amount of, puts in the tool plug conical flask, the accurate methanol 50ml that adds, and close plug claims to decide weight, and supersound process 20 minutes claims to decide weight again, supplies the weight that subtracts mistake with methanol, shakes up, and filters, and gets subsequent filtrate, promptly.
Accurate respectively reference substance solution and each 20ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures promptly.
(2) qualitative identification
A. thin layer chromatography is differentiated Radix Angelicae Sinensis and Rhizoma Chuanxiong in the Shenbao preparation
Get product or the product content thing is an amount of, the 30ml that adds diethyl ether, reflux 1 hour filters. and filtrate volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Other gets Radix Angelicae Sinensis and each 0.5g of Rhizoma Chuanxiong control medicinal material, shines medical material solution in pairs with legal system.Drawing above-mentioned need testing solution and control medicinal material solution 2 μ l, put respectively on same silica gel g thin-layer plate, is developing solvent with normal hexane-ethyl acetate (9: 1), launches, and takes out, and dries, and puts under the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
B. thin layer chromatography is differentiated Fructus Cnidii in the Shenbao preparation
Get product or the product content thing is an amount of, the 30ml that adds diethyl ether, reflux 1 hour filters. and filtrate volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Get the osthole reference substance, add ethanol and make the solution that every 1ml contains 1mg, in contrast product solution.Drawing each 1 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-ethyl acetate (7: 2), launches, and takes out, and dries, and puts under the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
C. thin layer chromatography is differentiated Radix Polygoni Multiflori Preparata in the Shenbao preparation
Get product or the product content thing is an amount of, the 30ml that adds diethyl ether, reflux 1 hour filters. and filtrate volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Add ethyl acetate 30ml, reflux 1 hour is put cold, filter, filtrate is extracted 3 times with 5% sodium carbonate liquor jolting, and each 20ml merges sodium carbonate extraction liquid, with hydrochloric acid adjust pH to 2～3, the jolting of reuse ethyl acetate is extracted 2 times, each 30ml, combined ethyl acetate extracting solution, be concentrated into 1ml, as need testing solution.Other gets Radix Polygoni Multiflori control medicinal material 0.3g, shines medical material solution in pairs with legal system.Get the emodin reference substance again, add methanol and make the solution that every 1ml contains 0.2mg, in contrast product solution.Draw above-mentioned need testing solution 10 μ l, each 2 μ 1 of control medicinal material and reference substance solution, put respectively on same silica gel g thin-layer plate, upper solution with petroleum ether (30～60 ℃)-Ethyl formate-formic acid (15: 5: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show identical orange-yellow fluorescence speckle.Put in the ammonia steam smoked after, inspect under the daylight, speckle becomes redness.
D. thin layer chromatography is differentiated Herba Epimedii in the Shenbao preparation
Get product or the product content thing is an amount of, the 30ml that adds diethyl ether, reflux 1 hour filters. and filtrate volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Add n-butyl alcohol 30ml, supersound extraction 30 minutes filters, and filtrate adds ammonia solution washing 2 times, and each 30ml discards ammonia solution, and n-butyl alcohol liquid evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets the icariin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (10: 1: 1: 1) be developing solvent, expansion was taken out with ethyl acetate-butanone-formic acid-water, dry, spray is put 105 ℃ of bakings several minutes, in the test sample chromatograph with 10% ethanol solution of sulfuric acid, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
E. high-efficient liquid phase technique is differentiated Fructus Psoraleae in the Shenbao preparation
Get product or the product content thing is an amount of, add methanol 40ml, supersound extraction 30 minutes is put coldly, filters, and filtrate is as need testing solution.Other gets psoralen and the isopsoralen reference substance is an amount of, adds methanol and makes the mixed solution that every 1ml contains 4 μ g, in contrast product solution.Measure according to high performance liquid chromatography (appendix ID of Chinese Pharmacopoeia version in 2005).With the octadecylsilane chemically bonded silica is filler; Methanol-water (40: 60) is a mobile phase, and the detection wavelength is 246nm.Accurate respectively reference substance solution and each 20ul of need testing solution of drawing injects chromatograph of liquid, measures.The retention time of main peak should be consistent with reference substance in the test sample chromatogram.
The amount of described extraction sample or dissolving extract solvent for use, ultrasonic or time, standardize solution or dissolving back volume, point sample amount or the sample size of reflux, extract,, the concentration of reference substance can be that benchmark changes with described occurrence, or change in proportion.
Both can adopt reference substance among described qualitative identification a, b, c, the d, and also can adopt control medicinal material to compare, or both all adopt, both can adopt two kinds of reference substances among the qualitative identification e, also can only adopt wherein a kind of reference substance in contrast.
Described supersound process also can adopt conventional extracting method such as reflux, extract,, microwave extraction, vibration extraction, and described reflux, extract, also can adopt conventional extracting method such as supersound process, microwave extraction, vibration extraction.
5. above-mentioned 2,3,4 described methods, can be used to detect any dosage form of the Shenbao preparation that makes by above-mentioned 1 described preparation method or make by other preparation method, as tablet, sugar coated tablet, film coated tablet, chewable tablet, effervescent tablet, dispersible tablet, capsule, hard capsule, soft capsule, pellt capsule, oral liquid, syrup, suck agent, electuary, granule, effervescent granule, pill, drop pill, pellet.
6. in the Shenbao preparation 2,3,5, the content limit of 4 '-tetrahydroxystilbene-2-O-b-D-glucoside is: contain Radix Polygoni Multiflori Preparata with 2,3,5 in the once minimum dose, 4 '-tetrahydroxystilbene-2-O-b-D-glucoside (C
20H
22O
9) meter, must not be less than 1.3mg; The content Determination of Icariin limit is: contain Herba Epimedii with icariin (C in the once minimum dose
33H
40O
15) meter, must not be less than 1.5mg; The content limit of osthole is: contain Fructus Cnidii with osthole (C in the once minimum dose
15H
16O
3) meter, must not be less than 0.8mg; The content limit of schisandrin is: contain Fructus Schisandrae Chinensis with schisandrin (C in the once minimum dose
24H
32O
7) meter, must not be less than 0.4mg; Above-mentioned content limit is the minimum content limit, can improve content limit according to the concrete condition of producing.
Experimental example 1: Shenbao preparation Study on Preparation
(1) Radix Ginseng Rubra extraction process
With dried cream yield and ginsenoside Re+Rg1 extracted amount is evaluation index, the Radix Ginseng Rubra reflux technique is investigated, got three parts of Radix Ginseng Rubra coarse powder 100g, add 20% alcohol dipping after 8 hours, add 6 times, 9 times, 12 times solvents respectively, the reflux, extract, secondary, each 2 hours, merge extractive liquid,, filter, filtrate recycling ethanol, concentrating under reduced pressure, vacuum drying.The result adds 6 times of amount solvents, and ginsenoside Re+Rg1 extracted amount, dried cream yield are respectively 766.37mg, 54.76%, adds 9 times of amount solvents and is respectively 957.22mg, 60.18%, adds 12 times of amount solvents and is respectively 960.38mg, 65.34%.So can think and can carry most effective ingredient when adding 9 times of amounts of solvent, increase extraction time and solvent amount again, can only increase the proposition of invalid components such as starch.From energy savings, reduce production costs and reduce dose and consider, preferred Radix Ginseng Rubra reflux, extract, technology is: red ginseng powder is broken into coarse powder, adds 9 times of amount 20% alcohol dipping after 8 hours, reflux, extract, secondary, each 2 hours.
(2) Herba Epimedii, Radix Angelicae Sinensis, Fructus Cnidii, Rhizoma Chuanxiong, Fructus Foeniculi five kinds of Chinese medicine percolation technology are investigated
With dried cream yield, icariin extracted amount is evaluation index, and the percolation technology of five kinds of Chinese medicine such as Herba Epimedii is investigated, and takes by weighing three parts of five tastes 212.1g such as Herba Epimedii by the amount of former renal aid syrup prescription, pulverize separately becomes coarse powder, makes solvent with 70% ethanol, floods after 48 hours, with the speed of per minute 1～3ml percolation slowly, by testing program, collect percolate 1000ml (4.7 times of amounts), 1500ml (7 times of amounts), 2000ml (9.4 times of amounts) respectively, reclaim ethanol, concentrating under reduced pressure, vacuum drying.Collection percolate 1000ml icariin extracted amount, dried cream yield are respectively 598mg, 7.34%, and percolate 1500ml is respectively 650mg, 9.29%, collect percolate 2000ml and are respectively 667mg, 10.27%.So can think that percolate 1500ml can carry most effective ingredient, increase extraction time and solvent amount again, can only increase the proposition of invalid components such as starch.From energy savings, reduce production costs and reduce dose and consider, 5 flavor percolation extraction processes such as preferred Herba Epimedii are that ground spice such as Herba Epimedii is broken into coarse powder, make solvent with 70% ethanol, flood after 48 hours, with the speed of per minute 1～3ml percolation slowly, collect 7 times of amounts of percolate.
(3) ten Six-element liquid medicine such as Radix Polygoni Multiflori Preparata are put forward technology
With dried cream yield, the stilbene glucoside extracted amount is an evaluation index, ten Six-element liquid medicine such as Radix Polygoni Multiflori Preparata are put forward technology to be investigated, measure 16 flavors such as taking by weighing Radix Polygoni Multiflori Preparata by 1/2 of former renal aid syrup prescription and add Radix Ginseng Rubra through three parts of the common 413.15g of the medicinal residues of alcohol extraction, by testing program, add not commensurability water respectively, soaked 1 hour, and decocted secondary, each 2 hours, collecting decoction, filter, the filtrate filtrate decompression is concentrated into the clear paste that relative density is 1.16 (80 ℃ of heat are surveyed), adds ethanol and makes that to contain the alcohol amount be 65%, left standstill 48 hours, get the supernatant decompression recycling ethanol, concentrating under reduced pressure, vacuum drying.The result adds 8 times of water gaging stilbene glucoside extracted amounts, dried cream yield is respectively 652mg, 12.46%, add 10 times of water gaging stilbene glucoside extracted amounts, dried cream yield is respectively 725mg, 14.13%, add 12 times of water gaging stilbene glucoside extracted amounts, dried cream yield is respectively 729mg, 15.62%, so can think when amount of water is 10 times, can carry most effective ingredient substantially, increase the solvent amount again, can only increase the proposition of invalid components such as starch, phlegmatic temperament.From energy savings, reduce cost and reduce dose and consider, 16 flavor extraction processes such as preferred Radix Polygoni Multiflori Preparata are: 16 flavors such as Radix Polygoni Multiflori Preparata add the medicinal residues of Radix Ginseng Rubra through alcohol extraction, adding 10 times of water gagings soaked 1 hour, decoct secondary, each 2 hours, collecting decoction, filter, the filtrate filtrate decompression is concentrated into relative density be 1.16 clear paste of (80 ℃ of heat are surveyed), adds ethanol and makes that to contain the alcohol amount be 65%, leaves standstill 48 hours.
(4) drying process
The prescription Chinese crude drug is evaporated to thick paste through extracting, and when carrying out drying, is subjected to heat damage for a long time for preventing effective ingredient, can adopt drying meanss such as vacuum drying, spray drying or lyophilization according to the situation of actual production equipment.With the contained active component with kidney tonifying effect 2 in contained active component icariin of Herba Epimedii and the Radix Polygoni Multiflori Preparata, 3,5, the extracted amount of 4-tetrahydroxystilbene-2-O-b-D-glucoside is an evaluation index, influence to vacuum drying centering pharmaceutically active ingredient is investigated, and finds that vacuum/spray drying front and back icariin extracted amount, stilbene glucoside extracted amount all do not have significant difference.
(5) moulding process
The dried cream powder of gained is made various solid preparations according to a conventional method, as tablet, sugar coated tablet, film coated tablet, chewable tablet, effervescent tablet, dispersible tablet, capsule, hard capsule, soft capsule, pellt capsule, suck agent, electuary, granule, effervescent granule, pill, drop pill, pellet etc.Following Study on Forming is an example with tablet, chewable tablet, granule, capsule.
A. tablet
This product dried cream powder viscosity is stronger, test is the effect of 75% ethanol, 85 ethanol % and 95% alcohol granulation relatively, get extractum powder 50g, add 15g starch, mixing, spray into above-mentioned wetting agent, phenomenon occurs cohering when 75% ethanol, 85% alcohol granulation as a result, 95% alcohol granulation effect is better, and preparation easily, grain color is even, and is easily dry.
Test intended is selected microcrystalline Cellulose (MCC), hyprolose (HPC), pregelatinized Starch (Pre-starch), micropowder silica gel (SiO for use
2), magnesium stearate (Mg-st) is adjuvant, test method: dried cream powder mixes with adjuvant (except the magnesium stearate), adds ethanol system granule, drying adds magnesium stearate, mixing, tabletting, experimental design and the results are shown in Table 1.
Table 1: compression molding craft screening and result
| The prescription number | Dried cream powder (%) | MCC (％) | HPC (％) | Pre-starc h(％) | SiO 2 (％) | Mg-st (％) | Compressibility | Disintegration time (min) |
| 1 2 3 | 79.6 84.6 89.6 | 15 0 9 | 5 7 0 | 0 8 0 | 0 0 1 | 0.4 0.4 0.4 | Good, medium (9kg) is good for hardness, and general (7kg) is good for hardness, hardness height (11kg) | 8 10 9 |
| 4 | 94.6 | 0 | 3 | 0 | 2 | 0.4 | Sticking is arranged, hardness general (8kg) | 7 |
By table 1 as seen, the 1 adjuvant ratio of writing out a prescription accounts for 20%, and hardness is medium, because added adjuvant space is little, test is found micropowder silica gel to the hardness influence better, and helps preparation of granules, and is heavy for reducing sheet, and suitable tabletting and subsequent packet film-coat needs, select for use prescription 3 for determining prescription, granulate easily, the tablet appearance is bright and clean, the hardness height, disintegrate is fast.
B. chewable tablet
Heavier bitter taste is arranged in the renal aid extract, only add correctivess such as sucrose, Aspartane, stevioside, mannitol and be difficult to shelter its bitter taste, so attempt adopting in wet extractum and add an amount of betacyclodextrin, the mixing after drying, add sweeting agent etc. again and carry out the method for flavoring, the result shows that this method is respond well.The amount of the betacyclodextrin that adds, the amount that adds aspartame are carried out preferably, when the result adds 30% betacyclodextrin, 1% Aspartane, taste good.
Because dried cream powder viscosity is stronger, so during granulation, do not need to add in addition again binding agent.Being wetting agent with 95% ethanol, 90% ethanol, 80% ethanol respectively, granulating, is evaluation index with granulation difficulty or ease, fine powder amount, and wetting agent is investigated, and the result is better with 90% alcohol granulation effect, is wetting agent so adopt 90% ethanol.
C. granule
A. wet granulation is got dried cream powder 200g, adds an amount of 90% ethanol, mixes, and the system soft material is crossed 14 mesh sieves and granulated.60 ℃ of dryings of wet granular, granule are with 14 mesh sieve granulate, and fine grained and fine powder go with 60 mesh sieves sieve, promptly.
B. dry granulation adopts the dry granulation machine to granulate, and control workshop relative humidity is below 50%.
Two kinds of methods all can be granulated smoothly, and water content, melting are all qualified, but dry granulation does not need guiding humid medium (ethanol), does not need heat drying, and technological process is short, and it is low to consume energy, and equipment is few, so dry granulation is better.
D. capsule
This product dried cream powder flowability is poor slightly, improve its flowability so add an amount of micropowder silica gel, experiment shows that the micropowder silica gel of adding 1% can effectively improve its flowability, control workshop relative humidity is below 50%, carry out the capsule trial assembly, add the dried cream powder fill smoothly of 1% micropowder silica gel, the capsule of being adorned is carried out inspections such as content uniformity, moisture, the result is all up to specification.
Experimental example 2: Shenbao preparation assay research
(1) in the Shenbao preparation 2,3,5,4 '-tetrahydroxystilbene-2-O-b-D-glycoside assay
A. the chromatographic condition octadecylsilane chemically bonded silica is a filler; Second eyeball-water (25: 75) is mobile phase; The detection wavelength is 320nm.Number of theoretical plate is by 2,3,5, and 4 '-tetrahydroxystilbene-2-O-b-D-glucoside peak calculates should be not less than 2000.
B. the preparation precision of the preparation reference substance solution of reference substance, test sample, negative control product solution takes by weighing 2,3,5, and 4 '-tetrahydroxystilbene-2-O-b-D-glucoside reference substance adds Diluted Alcohol and makes the solution that every 1ml contains 20ug, promptly.
Renal aid agreement that contracts a film or TV play to an actor or actress 0.15g is got in the preparation of need testing solution respectively, renal aid is chewed agreement that contracts a film or TV play to an actor or actress 0.3g, the about 1.5g of granule for strengthening kidney, the about 0.15g of kidney capsule content, and accurate the title decides, and puts in the conical flask respectively, the accurate Diluted Alcohol 50ml that adds, claim to decide weight, reflux 30 minutes is put cold, claim to decide weight, supply the weight that subtracts mistake with Diluted Alcohol, shake up, filter, get subsequent filtrate, promptly.
Scarce Radix Polygoni Multiflori Preparata negative control 0.15g is got in the preparation that lacks the Radix Polygoni Multiflori Preparata negative control solution, operates with method according to " preparation of need testing solution ", promptly gets to lack the Radix Polygoni Multiflori Preparata negative control solution.
C. measure accurate respectively reference substance solution, need testing solution, scarce each 20ml of Radix Polygoni Multiflori Preparata negative control solution of drawing, inject chromatograph of liquid, measure, promptly.
As seen in the test sample 2,3,5, separating degree＞1.5 of 4 '-tetrahydroxystilbene-2-O-b-D-glucoside, 2,3,5,4 '-tetrahydroxystilbene-2-O-b-D-glucoside reaches better with other component and separates, and feminine gender does not have interference, and interference component is not measured.Theoretical cam curve is with 2,3,5, and 4 '-tetrahydroxystilbene-2-O-b-D-glucoside peak calculates and is not less than 2000.Mobile phase employing methanol-acetonitrile-water (5: 1: 9) should.
D. this method is carried out methodological study, as a result 2,3,5,4 '-tetrahydroxystilbene-2-O-b-D-glucoside becomes the good linear relation in 15 μ g/ml～120 μ g/ml scopes, and the response rate is 98.99%, and precision, repeatability are all good.
(2) icariin Determination on content in the Shenbao preparation
A. the chromatographic condition octadecylsilane chemically bonded silica is a filler; Second eyeball-water (30: 70) is mobile phase; The detection wavelength is 270nm.Number of theoretical plate calculates by the icariin peak should be not less than 2000.
B. the preparation of reference substance, test sample, negative control product solution
The preparation precision of reference substance solution takes by weighing the icariin reference substance, adds methanol and makes the solution that every 1ml contains 40ug, promptly.
Renal aid agreement that contracts a film or TV play to an actor or actress 0.25g is got in the preparation of need testing solution respectively, renal aid is chewed agreement that contracts a film or TV play to an actor or actress 0.3g, the about 1.5g of granule for strengthening kidney, the about 0.25g of kidney capsule content, the accurate title, decide, and adds water 10ml respectively, puts in the tool plug separatory funnel, with ethyl acetate extraction 4 times, each 10ml, combined ethyl acetate layer, evaporate to dryness, residue adds dissolve with methanol and is transferred in the 25ml measuring bottle, add methanol to scale, shake up, promptly.
Scarce Herba Epimedii negative control 0.18g is got in the preparation that lacks the Herba Epimedii negative control solution, operates with method according to " preparation of need testing solution ", promptly gets to lack the negative negative control solution of Herba Epimedii.
C. measure: get reference substance solution, need testing solution, lack Herba Epimedii negative control solution and each 20 μ l of blank solution (mobile phase), inject chromatograph of liquid, measure.
As seen the separating degree of icariin＞1.5 in the test sample, icariin reaches better with other component and separates, and feminine gender does not have interference, interference component is measured.Theoretical cam curve is calculated greater than 2000 with the icariin peak.Mobile phase adopts methanol-water-glacial acetic acid (60: 40: 0.5) also can.
D. this method is carried out methodological study, icariin becomes the good linear relation in 20 μ g/ml～80 μ g/m1 scopes as a result, and the response rate is 99.98%, and precision, repeatability are all good.Show that this law can be used for measuring the content Determination of Icariin of Shenbao preparation.
(3) osthole Determination on content in the Shenbao preparation
A. the test of chromatographic condition and system suitability is a filler with octadecylsilane chemically bonded silica; Methanol-water (67: 33) is a mobile phase; The detection wavelength is 249nm.Number of theoretical plate calculates by the osthole peak should be not less than 2000.
B. the preparation of reference substance, test sample, negative control product solution
The preparation precision of reference substance solution takes by weighing the osthole reference substance, adds methanol and makes the solution that every 1ml contains 50ug, promptly.
Renal aid agreement that contracts a film or TV play to an actor or actress 0.25g is got in the preparation of need testing solution respectively, renal aid is chewed agreement that contracts a film or TV play to an actor or actress 0.3g, the about 1.5g of granule for strengthening kidney, the about 0.25g of kidney capsule content, the accurate title, decide, and puts respectively in the tool plug conical flask, the accurate ethanol 50ml that adds, close plug, claim to decide weight, supersound process 1 hour claims to decide weight, supply the weight that subtracts mistake with ethanol, shake up, filter, get subsequent filtrate promptly.
Scarce Fructus Cnidii negative control 0.25g is got in the preparation that lacks the Fructus Cnidii negative control solution, operates with method according to " preparation of need testing solution ", promptly gets to lack the negative negative control solution of Fructus Cnidii.
C. measure accurate respectively draw reference substance solution and need testing solution 20ml, inject chromatograph of liquid, measure, promptly.
As seen the separating degree of osthole＞1.5 in the test sample, osthole reaches better with other component and separates, and feminine gender does not have interference, interference component is measured.Theoretical cam curve is calculated greater than 2000 with the osthole peak.Mobile phase adopts methanol-water (67: 33), methanol-water-oxolane (53: 42: 5) also can.
D. this method is carried out methodological study, osthole becomes the good linear relation in 10 μ g/ml～100 μ g/ml scopes as a result, and the response rate is 99.35%, and precision, repeatability are all good.Show that this law can be used for measuring the content of the osthole of Shenbao preparation.
(4) schisandrin Determination on content in the Shenbao preparation
A. the chromatographic condition octadecylsilane chemically bonded silica is a filler; Methanol-water (13: 7) is a mobile phase; The detection wavelength is 250nm.Number of theoretical plate calculates by the schisandrin peak should be not less than 2000.
B. the preparation of reference substance, test sample, negative control product solution
The preparation precision of reference substance solution takes by weighing the schisandrin reference substance, adds methanol and makes the solution that every 1ml contains 30ug.
Renal aid agreement that contracts a film or TV play to an actor or actress 0.3g is got in the preparation of need testing solution respectively, renal aid is chewed agreement that contracts a film or TV play to an actor or actress 0.5g, the about 2.0g of granule for strengthening kidney, the about 0.3g of kidney capsule content, and accurate the title decides, and puts respectively in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, supersound process 20 minutes, claim to decide weight again, supply the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate, promptly.
Scarce Fructus Schisandrae Chinensis negative control 0.25g is got in the preparation that lacks the Fructus Schisandrae Chinensis negative control solution, operates with method according to " preparation of need testing solution ", promptly gets to lack the negative negative control solution of Fructus Schisandrae Chinensis.
C. measure accurate respectively draw reference substance solution and need testing solution 20ml, inject chromatograph of liquid, measure, promptly.
As seen the separating degree of schisandrin＞1.5 in the test sample, schisandrin reaches better with other component and separates, and feminine gender does not have interference, interference component is measured.Theoretical cam curve is calculated greater than 2000 with the schisandrin peak.Mobile phase adopts methanol-water (13: 7) also can.
D. this method is carried out methodological study, schisandrin becomes the good linear relation in 10 μ g/ml～80 μ g/ml scopes as a result, and the response rate is 99.52%, and precision, repeatability are all good.Show that this law can be used for measuring the content of the osthole of Shenbao preparation.
Experimental example 3: Shenbao preparation qualitative identification research
(1) thin layer chromatography of Radix Angelicae Sinensis and Rhizoma Chuanxiong is differentiated, with reference to " discriminating of Rhizoma Chuanxiong under item of Chinese pharmacopoeia version in 2000. because of the speckle basically identical of Radix Angelicae Sinensis and Rhizoma Chuanxiong control medicinal material, so this experiment is contrast with Radix Angelicae Sinensis and two kinds of control medicinal materials of Rhizoma Chuanxiong, negative sample also adopts and lacks Radix Angelicae Sinensis, Rhizoma Chuanxiong two flavors simultaneously.With normal hexane-ethyl acetate (9: 1) is developing solvent, and Rf value is suitable as a result, and clear spot lacks Radix Angelicae Sinensis, the Rhizoma Chuanxiong sample is noiseless.Developing solvent adopts petroleum ether (60-90 ℃)-ethyl acetate (9: 2), cyclohexane extraction-ethyl acetate (17: 3) also can.
(2) thin layer chromatography of Fructus Cnidii is differentiated, this experiment is to be reference substance with the osthole, and cyclohexane extraction-ethyl acetate (7: 2) is developing solvent, and Rf value is suitable as a result, clear spot, and it is noiseless to lack the Fructus Cnidii sample.Developing solvent adopts normal hexane-ethyl acetate (85: 15), benzene-ethyl acetate (30: 1) also can.
(3) thin layer chromatography of Radix Polygoni Multiflori Preparata is differentiated, ethyl acetate extraction is used earlier in the test sample preparation, extract with 5% sodium carbonate liquor again, composition such as emodin is dissolved in the alkali liquor, again the acidify ethyl acetate extraction, compare medical material with Radix Polygoni Multiflori, emodin compares product, and petroleum ether (30～60 ℃)-Ethyl formate-formic acid (15: 5: 1) is developing solvent, chromatograph clear spot as a result, Rf value is suitable, and it is noiseless to lack the Radix Polygoni Multiflori Preparata sample.Developing solvent adopts chloroform-methanol (8: 2), petroleum ether (30～60 ℃)-ethyl acetate-glacial acetic acid (9: 1: 0.1) also can.
(4) be the thin layer chromatography discriminating of Herba Epimedii, with reference to the method under the black positive reinforcing the heart syrup of National Drug Administration of People's Republic of China (PRC) standard (trying) [WS-10585 (ZD-0585) 2002] the discriminating item.Because of the prescription in the Herba Epimedii amount more, after n-butanol extraction is adopted in test, the need testing solution preparation method of reuse alkali liquid washing, with the icariin is reference substance, (10: 1: 1: 1) be developing solvent, be developer with 10% ethanol solution of sulfuric acid to ethyl acetate-butanone-formic acid-water, as a result the chromatograph clear spot, Rf value is suitable, and it is noiseless to lack the Herba Epimedii sample.
(5) be the liquid chromatograph discriminating of Fructus Psoraleae.With reference to the method under National Drug Administration of People's Republic of China (PRC) standard (trying) tonifying kidneys and nourishing brain ball [WS-10555 (ZD-0555) 2002] the discriminating item.The mixing reference substance solution of getting psoralen and isopsoralen earlier is in 200-400nm place scanning ultra-violet absorption spectrum, and the result is presented at 246nm wavelength place absorption maximum, so select 246nm for measuring wavelength.Three batch samples sample introduction after methanol is ultrasonic, in the test sample chromatograph, with mix the corresponding position of reference substance chromatographic peak all arranged, lack the Fructus Psoraleae negative sample with the method preparation, in the negative sample chromatograph,, illustrate that negative sample is noiseless to it not having chromatographic peak with the corresponding position of reference substance.Mobile phase adopts methanol-water (60: 40) also can.
Embodiment 4: the comparison of active constituent content in the Shenbao preparation (is example with SHENBAO HEJI, renal aid sheet, renal aid chewable tablet, granule for strengthening kidney)
(1) 2,3,5,4 '-tetrahydroxystilbene-2-O-b-D-glucoside content relatively
Relatively in the Shenbao preparation 2,3,5, the content of 4 '-tetrahydroxystilbene-2-O-b-D-glucoside, the result is as follows: SHENBAO HEJI (mg/10ml) 1.3,2.1,6.4; Renal aid sheet (mg/ sheet) 5.07,5.11,5.09; Renal aid chewable tablet (mg/ sheet) 7.26,7.32,7.21; Granule for strengthening kidney (mg/ bag) 6.39,6.51,6.61; Kidney capsule (mg/ grain) 3.82,3.87,3.91.The amount that 3 of SHENBAO HEJI 10ml and renal aid sheets, 2 of renal aid chewable tablet, granule for strengthening kidney 1 bag, kidney capsule are 4 is suitable.Find in the SHENBAO GUTI ZHIJI 2,3,5,4 '-tetrahydroxystilbene-2-O-b-D-glucoside content is higher, shows that SHENBAO GUTI ZHIJI has bigger advantage at aspects such as preparation stabilities.
(2) icariin content relatively
Compare content Determination of Icariin in the Shenbao preparation, the result is as follows: SHENBAO HEJI (mg/10ml) 1.0,4.0,3.6; Renal aid sheet (mg/ sheet) 2.02,2.09,2.06; Renal aid chewable tablet (mg/ sheet) 3.31,3.17,3.10; Granule for strengthening kidney (mg/ bag) 4.52,4.12,4.37; Kidney capsule (mg/ grain) 1.55,1.58,1.62.The amount that 3 of SHENBAO HEJI 10ml and renal aid sheets, 2 of renal aid chewable tablet, granule for strengthening kidney 1 bag, kidney capsule are 4 is suitable.Find that icariin content is higher in the SHENBAO GUTI ZHIJI, show that SHENBAO GUTI ZHIJI has bigger advantage at aspects such as preparation stabilities.
(3) osthole content relatively
Compare the content of osthole in the Shenbao preparation, the result is as follows: SHENBAO HEJI (mg/10ml) 0.8,2.4,1.9; Renal aid sheet (mg/ sheet) 0.92,1.05,1.06; Renal aid chewable tablet (mg/ sheet) 1.51,1.44,1.60; Granule for strengthening kidney (mg/ bag) 3.14,3.26,3.10; Kidney capsule (mg/ grain) 0.86,0.92,0.95.The amount that 3 of SHENBAO HEJI 10ml and renal aid sheets, 2 of renal aid chewable tablet, granule for strengthening kidney 1 bag, kidney capsule are 4 is suitable.Find that osthole content is higher in the SHENBAO GUTI ZHIJI, show that SHENBAO GUTI ZHIJI has bigger advantage at aspects such as preparation stabilities.
(4) schisandrin content relatively
Compare the content of schisandrin in the Shenbao preparation, the result is as follows: SHENBAO HEJI (mg/10m1) 0.64,0.45,1.32; Renal aid sheet (mg/ sheet) 0.78,0.62,0.83; Renal aid chewable tablet (mg/ sheet) 1.07,1.02,0.94; Granule for strengthening kidney (mg/ bag) 2.01,2.14,2.07; Kidney capsule (mg/ grain) 0.47,0.41,0.55.The amount that 3 of SHENBAO HEJI 10ml and renal aid sheets, 2 of renal aid chewable tablet, granule for strengthening kidney 1 bag, kidney capsule are 4 is suitable.Find that schisandrin content is higher in the SHENBAO GUTI ZHIJI, show that SHENBAO GUTI ZHIJI has bigger advantage at aspects such as preparation stabilities.
Experimental example 5: content limit determines in the Shenbao preparation assay
(1) 2,3,5,4 '-tetrahydroxystilbene-2-O-b-D-glucoside content limit is determined
Contain the about 0.744g of Radix Polygoni Multiflori Preparata medical material in the once minimum dose of Shenbao preparation, in a regulation of Chinese Pharmacopoeia version in 2005 the Radix Polygoni Multiflori Preparata medical material 2,3,5, the content of 4 '-tetrahydroxystilbene-2-O-b-D-glucoside must not be lower than 0.7%.With in the Radix Polygoni Multiflori Preparata medical material 2,3,5,4 '-tetrahydroxystilbene-2-O-b-D-glucoside content is 0.7%, when the rate of transform is 35%, contains 2,3,5 in the once minimum dose, and 4 '-tetrahydroxystilbene-2-O-b-D-glucoside is 1.82mg.In conjunction with in the SHENBAO HEJI 2,3,5, in 4 '-tetrahydroxystilbene-2-O-b-D-glucoside content and the renal aid sheet of being developed, renal aid chewable tablet, granule for strengthening kidney, the kidney capsule 2,3,5,4 '-tetrahydroxystilbene-2-O-b-D-glucoside the rate of transform is considered the factors such as loss in the big production link, with this product 2,3,5,4 '-tetrahydroxystilbene-2-O-b-D-glucoside content limit is decided to be: contain Radix Polygoni Multiflori Preparata with 2,3 in the once minimum dose, 5,4 '-tetrahydroxystilbene-2-0-b-D-glucoside (C
20H
22O
9) meter, must not be less than 1.3mg.
(2) the Herba Epimedii content limit is determined
Contain the about 0.946g of epimedium herb in the once minimum dose of Shenbao preparation, content Determination of Icariin must not be lower than 0.5% in regulation epimedium herb of Chinese Pharmacopoeia version in 2005.In Herba Epimedii content in the epimedium herb is 0.5%, and when the rate of transform was 35%, containing icariin in the once minimum dose was 1.6mg.In conjunction with the icariin rate of transform in icariin content in the SHENBAO HEJI and the renal aid sheet developed, renal aid chewable tablet, granule for strengthening kidney, the kidney capsule, consider the factors such as loss in the big production link, this product icariin content limit is decided to be: contain Herba Epimedii with icariin (C in the once minimum dose
33H
40O
15) meter, must not be less than 1.4mg.
(3) the osthole content limit is determined
Contain the about 0.28g of Fructus Cnidii medical material in the once minimum dose of Shenbao preparation, the content of osthole must not be lower than 1.0% in a regulation Fructus Cnidii of Chinese Pharmacopoeia version in 2005 medical material.In osthole content in the Fructus Cnidii medical material is 1.0%, and when the rate of transform was 35%, containing osthole in the once minimum dose was 0.98mg.In conjunction with the osthole rate of transform in osthole content in the SHENBAO HEJI and the renal aid sheet developed, renal aid chewable tablet, granule for strengthening kidney, the kidney capsule, consider the factors such as loss in the big production link, this product osthole content limit is decided to be: contain Fructus Cnidii with osthole (C in the once minimum dose
15H
16O
3) meter, must not be less than 0.8mg.
(4) the schisandrin content limit is determined
Contain the about 0.36g of schisandra chinensis medicinal material in the once minimum dose of Shenbao preparation, the content of schisandrin must not be lower than 0.40% in 2005 editions regulation schisandra chinensis medicinal materials of Chinese Pharmacopoeia.In schisandrin content in the schisandra chinensis medicinal material is 0.40%, and when the rate of transform was 35%, containing schisandrin in the once minimum dose was 0.504mg.In conjunction with the schisandrin rate of transform in schisandrin content in the SHENBAO HEJI and the renal aid sheet developed, renal aid chewable tablet, granule for strengthening kidney, the kidney capsule, consider the factors such as loss in the big production link, this product schisandrin content limit is decided to be: contain Fructus Schisandrae Chinensis with schisandrin (C in the once minimum dose
24H
32O
7) meter, must not be less than 0.4mg.
The specific embodiment
Further specify the present invention by the following examples, but do not limit range of application of the present invention therefrom.
Embodiment 1: the preparation of tablet
Fructus Cnidii 93.3g Rhizoma Chuanxiong 94.3g Semen Cuscutae 220g
Fructus Psoraleae 95g Poria 100g Radix Ginseng Rubra 66.7g
Fructus Foeniculi 48g Fructus Schisandrae Chinensis 120g Fructus Rosae Laevigatae 315.3g
Rhizoma Atractylodis Macrocephalae 47.3g Radix Angelicae Sinensis 156g Fructus Rubi 109.7g
Radix Polygoni Multiflori Preparata 248g Semen Plantaginis 55g Radix Rehmanniae Preparata 313.3g
Fructus Lycii 220g Rhizoma Dioscoreae 154.3g Herba Epimedii 315.3g
Semen Trigonellae 313.3g Radix Astragali 171.3g Herba Cistanches 157.7g
Radix Glycyrrhizae Preparata 47.3g
More than 22 the flavor, Fructus Cnidii, Herba Epimedii, Radix Angelicae Sinensis, Rhizoma Chuanxiong, Fructus Foeniculi are ground into coarse powder, make solvent with 70% ethanol, flood after 48 hours,, collect the about 5000ml of percolate with the speed of per minute 1～3ml percolation slowly, reclaim ethanol, being evaporated to relative density is the clear paste of 1.10 (80 ℃ of heat are surveyed), filters filtrate for later use; Red ginseng powder is broken into coarse powder, adds 9 times of amount 20% alcohol dipping after 8 hours, the reflux, extract, secondary, and each 2 hours, merge extractive liquid, filtered, and filtrate recycling ethanol is concentrated into relative density and is the clear paste of 1.10 (80 ℃ of heat are surveyed), and is standby; Ten Six-elements such as all the other Fructus Rubies with the medicinal residues of Radix Ginseng Rubra through alcohol extraction, add 10 times of water gagings and soaked 1 hour, decoct secondary, each 2 hours, collecting decoction, filter, filtrate is concentrated into the clear paste that relative concentration is 1.16 (80 ℃ of heat are surveyed), adds ethanol and makes that to contain the alcohol amount be 65%, left standstill 48 hours, and got supernatant and reclaim ethanol, being concentrated into relative density is the clear paste of 1.10 (80 ℃ of heat are surveyed), add extracting solution and red ginseng extracts such as above-mentioned Fructus Cnidii, mixing, vacuum drying, pulverize, add microcrystalline Cellulose 51g, micropowder silica gel 6g, mixing is made granule, dry, add magnesium stearate 2.5g, mixing is pressed into 1000, coating promptly gets the renal aid sheet.
Embodiment 2: the preparation of chewable tablet
Fructus Cnidii 140g Rhizoma Chuanxiong 141.5g Semen Cuscutae 330g
Fructus Psoraleae 142.5g Poria 150g Radix Ginseng Rubra 100g
Fructus Foeniculi 72g Fructus Schisandrae Chinensis 180g Fructus Rosae Laevigatae 473g
Rhizoma Atractylodis Macrocephalae 71g Radix Angelicae Sinensis 234g Fructus Rubi 164.5g
Radix Polygoni Multiflori Preparata 372g Semen Plantaginis 82.5g Radix Rehmanniae Preparata 470g
Fructus Lycii 330g Rhizoma Dioscoreae 231.5g Herba Epimedii 473g
Semen Trigonellae 470g Radix Astragali 257g Herba Cistanches 236.5g
Radix Glycyrrhizae Preparata 71g
More than 22 the flavor, Fructus Cnidii, Herba Epimedii, Radix Angelicae Sinensis, Rhizoma Chuanxiong, Fructus Foeniculi are ground into coarse powder, make solvent with 70% ethanol, flood after 48 hours,, collect the about 7500ml of percolate with the speed of per minute 1～3ml percolation slowly, reclaim ethanol, being evaporated to relative density is the clear paste of 1.10 (80 ℃ of heat are surveyed), filters filtrate for later use; Red ginseng powder is broken into coarse powder, adds 9 times of amount 20% alcohol dipping after 8 hours, the reflux, extract, secondary, and each 2 hours, merge extractive liquid, filtered, and filtrate recycling ethanol is concentrated into relative density and is the clear paste of 1.10 (80 ℃ of heat are surveyed), and is standby; Ten Six-elements such as all the other Fructus Rubies with the medicinal residues of Radix Ginseng Rubra through alcohol extraction, add 10 times of water gagings and soaked 1 hour, decoct secondary, each 2 hours, collecting decoction, filter, filtrate is concentrated into relative concentration be 1.16 clear paste of (80 ℃ of heat are surveyed), adds ethanol and makes that to contain the alcohol amount be 65%, leaves standstill 48 hours, get supernatant and reclaim ethanol, being concentrated into relative density is the clear paste of 1.10 (80 ℃ of heat are surveyed), adds extracting solution and red ginseng extracts such as above-mentioned Fructus Cnidii, mixing, add betacyclodextrin 318g, mixing, vacuum drying is pulverized, add Aspartane 10g, mixing is made granule, drying in right amount with 90% ethanol; Add magnesium stearate 3g, mixing is pressed into 1000, and the bag film-coat promptly gets the renal aid chewable tablet.
Embodiment 3: the preparation of granule
Fructus Cnidii 93.3g Rhizoma Chuanxiong 94.3g Semen Cuscutae 220g
Fructus Psoraleae 95g Poria 100g Radix Ginseng Rubra 66.7g
Fructus Foeniculi 48g Fructus Schisandrae Chinensis 120g Fructus Rosae Laevigatae 315.3g
Rhizoma Atractylodis Macrocephalae 47.3g Radix Angelicae Sinensis 156g Fructus Rubi 109.7g
Radix Polygoni Multiflori Preparata 248g Semen Plantaginis 55g Radix Rehmanniae Preparata 313.3g
Fructus Lycii 220g Rhizoma Dioscoreae 154.3g Herba Epimedii 315.3g
Semen Trigonellae 313.3g Radix Astragali 171.3g Herba Cistanches 157.7g
Radix Glycyrrhizae Preparata 47.3g
More than 22 the flavor, Fructus Cnidii, Herba Epimedii, Radix Angelicae Sinensis, Rhizoma Chuanxiong, Fructus Foeniculi are ground into coarse powder, make solvent with 70% ethanol, flood after 48 hours,, collect the about 7000ml of percolate with the speed of per minute 1～3ml percolation slowly, reclaim ethanol, being evaporated to relative density is the clear paste of 1.05 (heat is surveyed), filters filtrate for later use; Red ginseng powder is broken into coarse powder, adds 9 times of amount 20% alcohol dipping after 8 hours, the reflux, extract, secondary, and each 2 hours, merge extractive liquid, filtered, and filtrate recycling ethanol is concentrated into relative density and is the clear paste of 1.05 (heat is surveyed), and is standby; Ten Six-elements such as all the other Fructus Rubies, with the medicinal residues of Radix Ginseng Rubra through alcohol extraction, adding 10 times of water gagings soaked 1 hour, decoct secondary, each 2 hours, collecting decoction, filter, filtrate is concentrated into relative concentration be 1.10 clear paste of (heat is surveyed), adds ethanol and makes and contain the alcohol amount and reach 65%, leaves standstill 48 hours, get supernatant and reclaim ethanol, being concentrated into relative density is the clear paste of 1.05 (heat is surveyed), adds extracting solution and red ginseng extracts such as above-mentioned Fructus Cnidii, mixing, add dextrin 500g, spray drying, dry granulation is made granule 1000 grams altogether.
Embodiment 4: the preparation of capsule
Fructus Cnidii 70g Rhizoma Chuanxiong 70.75g Semen Cuscutae 165g
Fructus Psoraleae 71.25g Poria 75g Radix Ginseng Rubra 50g
Fructus Foeniculi 36g Fructus Schisandrae Chinensis 90g Fructus Rosae Laevigatae 236.5g
Rhizoma Atractylodis Macrocephalae 35.5g Radix Angelicae Sinensis 117g Fructus Rubi 82.25g
Radix Polygoni Multiflori Preparata 186g Semen Plantaginis 41.25g Radix Rehmanniae Preparata 235g
Fructus Lycii 165g Rhizoma Dioscoreae 115.75g Herba Epimedii 236.5g
Semen Trigonellae 235g Radix Astragali 128.5g Herba Cistanches 118.25g
Radix Glycyrrhizae Preparata 35.5g
More than 22 the flavor, Fructus Cnidii, Herba Epimedii, Radix Angelicae Sinensis, Rhizoma Chuanxiong, Fructus Foeniculi are ground into coarse powder, make solvent with 70% ethanol, flood after 48 hours,, collect the about 3750ml of percolate with the speed of per minute 1～3ml percolation slowly, reclaim ethanol, being evaporated to relative density is the clear paste of 1.10 (80 ℃ of heat are surveyed), filters filtrate for later use; Red ginseng powder is broken into coarse powder, adds 9 times of amount 20% alcohol dipping after 8 hours, the reflux, extract, secondary, and each 2 hours, merge extractive liquid, filtered, and filtrate recycling ethanol is concentrated into relative density and is the clear paste of 1.10 (80 ℃ of heat are surveyed), and is standby; Ten Six-elements such as all the other Fructus Rubies with the medicinal residues of Radix Ginseng Rubra through alcohol extraction, add 10 times of water gagings and soaked 1 hour, decoct secondary, each 2 hours, collecting decoction filtered, filtrate is concentrated into the clear paste that relative concentration is 1.16 (80 ℃ of heat are surveyed), add ethanol and make that to contain alcohol amount be 65%, left standstill 48 hours, get supernatant and reclaim ethanol, being concentrated into relative density is the clear paste of 1.10 (80 ℃ of heat are surveyed), add extracting solution and red ginseng extracts such as above-mentioned Fructus Cnidii, mixing, vacuum drying, pulverize, add micropowder silica gel 4g, mixing incapsulates, make 1000, promptly.
Embodiment 5: the discriminating of renal aid sheet and assay (can comprise following all or part of)
1. differentiate
(1) get 6 of this product, porphyrize, the 20ml that adds diethyl ether, reflux 1 hour filters. and filtrate volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Other gets Radix Angelicae Sinensis and each 0.5g of Rhizoma Chuanxiong control medicinal material, shines medical material solution in pairs with legal system.Drawing above-mentioned need testing solution and control medicinal material solution 2 μ l, put respectively on same silica gel g thin-layer plate, is developing solvent with normal hexane-ethyl acetate (9: 1), launches, and takes out, and dries, and puts under the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
(2) get the osthole reference substance, add ethanol and make the solution that every 1ml contains 1mg, in contrast product solution.Drawing above-mentioned reference substance solution and [discriminating] (1) item each 1 μ l of need testing solution down, put respectively on same silica gel g thin-layer plate, is developing solvent with cyclohexane extraction-ethyl acetate (7: 2), launches, and taking-up is dried, and puts under the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(3) get 12 of this product, porphyrize adds ethyl acetate 30ml, reflux 1 hour is put coldly, filters, filtrate is extracted 3 times with 5% sodium carbonate liquor jolting, and each 20ml merges sodium carbonate extraction liquid, with hydrochloric acid adjust pH to 2～3, the jolting of reuse ethyl acetate is extracted 2 times, each 30ml, combined ethyl acetate extracting solution, be concentrated into 1ml, as need testing solution.Other gets Radix Polygoni Multiflori control medicinal material 0.3g, shines medical material solution in pairs with legal system.Get the emodin reference substance again, add methanol and make the solution that every 1ml contains 0.2mg, in contrast product solution.Draw above-mentioned need testing solution 10 μ l, each 2 μ l of control medicinal material and reference substance solution, put respectively on same silica gel g thin-layer plate, upper solution with petroleum ether (30～60 ℃)-Ethyl formate-formic acid (15: 5: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show identical orange-yellow fluorescence speckle.Put in the ammonia steam smoked after, inspect under the daylight, speckle becomes redness.
(4) get 10 of this product, porphyrize adds n-butyl alcohol 30ml, and supersound process 30 minutes filters, and filtrate adds ammonia solution washing 2 times, and each 30ml discards ammonia solution, and n-butyl alcohol liquid evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets the icariin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Draw each 5 μ 1 of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (10: 1: 1: 1) be developing solvent, expansion was taken out with ethyl acetate-butanone-formic acid-water, dry, spray is put 105 ℃ of bakings several minutes, in the test sample chromatograph with 10% ethanol solution of sulfuric acid, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(5) get 1 of this product, porphyrize adds methanol 20ml, and ultrasonic 30 minutes, put coldly, filter, filtrate is as need testing solution.Other gets psoralen and the isopsoralen reference substance is an amount of, adds methanol and makes the mixed solution that every 1ml contains 4 μ g, in contrast product solution.With the octadecylsilane chemically bonded silica is filler; Methanol-water (40: 60) is a mobile phase, and the detection wavelength is 246nm.Accurate respectively reference substance solution and each 20ul of need testing solution of drawing injects chromatograph of liquid, measures.The retention time of main peak should be consistent with reference substance in the test sample chromatogram.
2. assay
(1) 2,3,5,4 '-tetrahydroxystilbene-2-O-b-D-glucoside lucifuge operation.
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Second eyeball-water (25: 75) is mobile phase; The detection wavelength is 320nm.Number of theoretical plate is by 2,3,5, and 4 '-tetrahydroxystilbene-2-O-b-D-glucoside peak calculates should be not less than 2000.
The preparation precision of reference substance solution takes by weighing 2,3,5, and 4 '-tetrahydroxystilbene-2-O-b-D-glucoside reference substance adds Diluted Alcohol and makes the solution that every 1ml contains 20ug, promptly.
This product under the weight differential item, porphyrize, mixing are got in the preparation of need testing solution, get about 0.25g, the accurate title, decide, and puts in the conical flask, the accurate Diluted Alcohol 50ml that adds claims to decide weight, reflux 30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with Diluted Alcohol, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each 20ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures promptly.
Every of this product contains Radix Polygoni Multiflori Preparata with 2,3,5,4 '-tetrahydroxystilbene-2-O-b-D-glucoside (C
20H
22O
9) meter, must not be less than 0.6mg.
(2) icariin
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Second eyeball-water (30: 70) is mobile phase; The detection wavelength is 270nm.Number of theoretical plate calculates by the icariin peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the icariin reference substance, adds methanol and makes the solution that every 1ml contains 40ug, promptly.
This product under the weight differential item, porphyrize, mixing are got in the preparation of need testing solution, get about 0.25g, the accurate title, decide, and adds water 10ml, put in the tool plug separatory funnel, use ethyl acetate extraction 4 times, each 10ml, the combined ethyl acetate layer, evaporate to dryness, residue add dissolve with methanol and are transferred in the 25ml measuring bottle, add methanol to scale, shake up, promptly.
Accurate respectively reference substance solution and each 20ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures promptly.
Every of this product contains Herba Epimedii with icariin (C
33H
40O
15) meter, must not be less than 0.5mg.
(3) osthole
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (67: 33) is a mobile phase; The detection wavelength is 249nm.Number of theoretical plate calculates by the osthole peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the osthole reference substance, adds methanol and makes the solution that every 1ml contains 50ug, promptly.
The renal aid sheet is got in the preparation of need testing solution, porphyrize, and mixing is got about 0.25g, and accurate the title, decide, and puts in the tool plug conical flask, the accurate ethanol 50ml that adds, close plug claims to decide weight, and supersound process 1 hour claims to decide weight again, supply the weight that subtracts mistake with ethanol, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and the need testing solution 20ml of drawing of algoscopy injects chromatograph of liquid, measures, promptly.
Every of this product contains Fructus Cnidii with osthole (C
15H
16O
3) meter, must not be less than 0.25mg;
(4) schisandrin
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (13: 7) is a mobile phase; The detection wavelength is 250nm.Number of theoretical plate calculates by the schisandrin peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the schisandrin reference substance, adds methanol and makes the solution that every 1ml contains 30ug, promptly.
The renal aid sheet is got in the preparation of need testing solution, porphyrize, and mixing is got about 0.3g, and accurate the title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, and supersound process 20 minutes claims to decide weight again, supply the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each 20ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures promptly.
Every of this product contains Fructus Schisandrae Chinensis with schisandrin (C
24H
32O
7) meter, must not be less than 0.15mg;
Embodiment 6: the discriminating of renal aid chewable tablet and assay (can comprise following all or part of)
1. differentiate
(1) get 4 of this product, porphyrize, the 30ml that adds diethyl ether, reflux 1 hour filters. and filtrate volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Other gets Radix Angelicae Sinensis and each 0.5g of Rhizoma Chuanxiong control medicinal material, shines medical material solution in pairs with legal system.Drawing above-mentioned need testing solution and control medicinal material solution 2 μ l, put respectively on same silica gel g thin-layer plate, is developing solvent with normal hexane-ethyl acetate (9: 1), launches, and takes out, and dries, and puts under the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
(2) get the osthole reference substance, add ethanol and make the solution that every 1ml contains 1mg, in contrast product solution.Drawing above-mentioned reference substance solution and [discriminating] (1) item each 1 μ l of need testing solution down, put respectively on same silica gel g thin-layer plate, is developing solvent with cyclohexane extraction-ethyl acetate (7: 2), launches, and taking-up is dried, and puts under the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(3) get 8 of this product, porphyrize adds ethyl acetate 30ml, reflux 1 hour is put coldly, filters, filtrate is extracted 3 times with 5% sodium carbonate liquor jolting, and each 20ml merges sodium carbonate extraction liquid, with hydrochloric acid adjust pH to 2～3, the jolting of reuse ethyl acetate is extracted 2 times, each 30ml, combined ethyl acetate extracting solution, be concentrated into 1ml, as need testing solution.Other gets Radix Polygoni Multiflori control medicinal material 0.3g, shines medical material solution in pairs with legal system.Get the emodin reference substance again, add methanol and make the solution that every 1ml contains 0.2mg, in contrast product solution.Draw above-mentioned need testing solution 10 μ l, each 2 μ l of control medicinal material and reference substance solution, put respectively on same silica gel g thin-layer plate, upper solution with petroleum ether (30～60 ℃)-Ethyl formate-formic acid (15: 5: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show identical orange-yellow fluorescence speckle.Put in the ammonia steam smoked after, inspect under the daylight, speckle becomes redness.
(4) get 5 of this product, porphyrize adds n-butyl alcohol 30ml, and supersound process 30 minutes filters, and filtrate adds ammonia solution washing 2 times, and each 30ml discards ammonia solution, and n-butyl alcohol liquid evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets the icariin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (10: 1: 1: 1) be developing solvent, expansion was taken out with ethyl acetate-butanone-formic acid-water, dry, spray is put 105 ℃ of bakings several minutes, in the test sample chromatograph with 10% ethanol solution of sulfuric acid, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(5) get 1 of this product, porphyrize adds methanol 40ml, and ultrasonic 30 minutes, put coldly, filter, filtrate is as need testing solution.Other gets psoralen and the isopsoralen reference substance is an amount of, adds methanol and makes the mixed solution that every 1ml contains 4 μ g, in contrast product solution.With the octadecylsilane chemically bonded silica is filler; Methanol-water (40: 60) is a mobile phase, and the detection wavelength is 246nm.Accurate respectively reference substance solution and each 20ul of need testing solution of drawing injects chromatograph of liquid, measures.The retention time of main peak should be consistent with reference substance in the test sample chromatogram.
2. assay
(1) 2,3,5,4 '-tetrahydroxystilbene-2-O-b-D-glucoside lucifuge operation.Measure according to high performance liquid chromatography (Chinese Pharmacopoeia version appendix in 2005 VID).
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Second eyeball-water (25: 75) is mobile phase; The detection wavelength is 320nm.Number of theoretical plate is by 2,3,5, and 4 '-tetrahydroxystilbene-2-O-b-D-glucoside peak calculates should be not less than 2000.
The preparation precision of reference substance solution takes by weighing 2,3,5, and 4 '-tetrahydroxystilbene-2-O-b-D-glucoside reference substance adds Diluted Alcohol and makes the solution that every 1ml contains 20ug, promptly.
This product under the weight differential item, porphyrize, mixing are got in the preparation of need testing solution, get about 0.3g, the accurate title, decide, and puts in the conical flask, the accurate Diluted Alcohol 50ml that adds claims to decide weight, reflux 30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with Diluted Alcohol, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each 20ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures promptly.
Every of this product contains Radix Polygoni Multiflori Preparata with 2,3,5,4 '-tetrahydroxystilbene-2-O-b-D-glucoside (C
20H
22O
9) meter, must not be less than 0.9mg.
(2) icariin
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Second eyeball-water (30: 70) is mobile phase; The detection wavelength is 270nm.Number of theoretical plate calculates by the icariin peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the icariin reference substance, adds methanol and makes the solution that every 1ml contains 40ug, promptly.
This product under the weight differential item, porphyrize, mixing are got in the preparation of need testing solution, get about 0.3g, the accurate title, decide, and dissolves with suitable quantity of water, put in the tool plug separatory funnel, use ethyl acetate extraction 4 times, each 10ml, the combined ethyl acetate layer, evaporate to dryness, residue add dissolve with methanol and are transferred in the 25ml measuring bottle, add methanol to scale, shake up, promptly.
Accurate respectively reference substance solution and each 20ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures promptly.
Every of this product contains Herba Epimedii with icariin (C
33H
40O
15) meter, must not be less than 0.75mg.
(3) osthole
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (67: 33) is a mobile phase; The detection wavelength is 249nm.Number of theoretical plate calculates by the osthole peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the osthole reference substance, adds methanol and makes the solution that every 1ml contains 50ug, promptly.
The renal aid chewable tablet is got in the preparation of need testing solution, porphyrize, and mixing is got about 0.3g, and accurate the title, decide, and puts in the tool plug conical flask, the accurate ethanol 50ml that adds, close plug claims to decide weight, and supersound process 1 hour claims to decide weight again, supply the weight that subtracts mistake with ethanol, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and the need testing solution 20ml of drawing of algoscopy injects chromatograph of liquid, measures, promptly.
Every of this product contains Fructus Cnidii with osthole (C
15H
16O
3) meter, must not be less than 0.4mg.
(4) schisandrin
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (13: 7) is a mobile phase; The detection wavelength is 250nm.Number of theoretical plate calculates by the schisandrin peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the schisandrin reference substance, adds methanol and makes the solution that every 1ml contains 30ug, promptly.
The renal aid chewable tablet is got in the preparation of need testing solution, porphyrize, and mixing is got about 0.5g, and accurate the title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, and supersound process 20 minutes claims to decide weight again, supply the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each 20ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures promptly.
Every of this product contains Fructus Schisandrae Chinensis with schisandrin (C
24H
32O
7) meter, must not be less than 0.2mg;
Embodiment 7: the discriminating of granule for strengthening kidney and assay (can comprise following all or part of)
1. differentiate
(1) get this product 6g, porphyrize, the 30ml that adds diethyl ether soaked 15 minutes, and supersound process is 15 minutes again, puts coldly, filters, and filtrate volatilizes solvent, and residue adds ethanol 1ml makes dissolving, as need testing solution.Other gets Radix Angelicae Sinensis and each 0.2g of Rhizoma Chuanxiong control medicinal material, shines medical material solution in pairs with legal system.Draw above-mentioned need testing solution 15 μ l, control medicinal material solution 2 μ l put respectively on same silica gel g thin-layer plate, are developing solvent with normal hexane-ethyl acetate (9: 1), launch, and take out, and dry, and put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
(2) get the osthole reference substance, add ethanol and make the solution that every 1ml contains 1mg, in contrast product solution.Drawing each the 1 μ l of need testing solution under the item of above-mentioned reference substance solution and [discriminating] (1), put respectively on same silica gel g thin-layer plate, is developing solvent with cyclohexane extraction-ethyl acetate (7: 2), launches, and takes out, and dries, and puts under the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(3) get this product 6g, porphyrize adds ethyl acetate 30ml, reflux 1 hour is put coldly, filters, filtrate is extracted 3 times with 5% sodium carbonate liquor jolting, and each 20ml merges sodium carbonate extraction liquid, with hydrochloric acid adjust pH to 2～3, the jolting of reuse ethyl acetate is extracted 2 times, and each 30ml merges ethyl acetate extraction liquid, be concentrated into 1ml, as need testing solution.Other gets Radix Polygoni Multiflori control medicinal material 0.3g, shines medical material solution in pairs with legal system.Get the emodin reference substance again, add methanol and make the solution that every 1ml contains 0.2mg, in contrast product solution.Draw above-mentioned need testing solution 10 μ l, each 2 μ l of control medicinal material and reference substance solution, put respectively on same silica gel g thin-layer plate, upper solution with petroleum ether (30～60 ℃)-Ethyl formate-formic acid (15: 5: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show identical orange-yellow fluorescence speckle.Put in the ammonia steam smoked after, inspect under the daylight, speckle becomes redness.
(4) get this product 6g, porphyrize adds n-butyl alcohol 30ml, and supersound process 30 minutes filters, and filtrate adds ammonia solution washing 2 times, and each 30ml discards ammonia solution, and n-butyl alcohol liquid evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets the icariin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (10: 1: 1: 1) be developing solvent, expansion was taken out with ethyl acetate-butanone-formic acid-water, dry, spray is put 105 ℃ of bakings several minutes, in the test sample chromatograph with 10% ethanol solution of sulfuric acid, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(5) get this product 1g, porphyrize adds methanol 20ml, and ultrasonic 30 minutes, put coldly, filter, filtrate is as need testing solution.Other gets psoralen and the isopsoralen reference substance is an amount of, adds methanol and makes the mixed solution that every 1ml contains 3 μ g, in contrast product solution.With the octadecylsilane chemically bonded silica is filler; Methanol-water (40: 60) is a mobile phase, and the detection wavelength is 246nm.Accurate respectively reference substance solution and each 10ul of need testing solution of drawing injects chromatograph of liquid, measures.The retention time of main peak should be consistent with reference substance in the test sample chromatogram.
2. assay
(1) 2,3,5,4 '-tetrahydroxystilbene-2-O-b-D-glucoside lucifuge operation.
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Second eyeball-water (25: 75) is mobile phase; The detection wavelength is 320nm.Number of theoretical plate is by 2,3,5, and 4 '-tetrahydroxystilbene-2-O-b-D-glucoside peak calculates should be not less than 2000.
The preparation precision of reference substance solution takes by weighing 2,3,5, and 4 '-tetrahydroxystilbene-2-O-b-D-glucoside reference substance adds Diluted Alcohol and makes the solution that every 1ml contains 60ug, promptly.
The about 1.5g of this product is got in the preparation of need testing solution, accurate claims surely, puts in the conical flask, and the accurate Diluted Alcohol 50ml that adds claims decide weight, and reflux 30 minutes is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with Diluted Alcohol, shakes up, and gets the supernatant filtration, promptly.
Accurate respectively reference substance solution and each 10ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures promptly.
This product contains 2,3,5 for every bag, 4 '-tetrahydroxystilbene-2-O-b-D-glucoside (C
20H
22O
9) must not be less than 1.3mg.
(2) icariin
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Second eyeball-water (30: 70) is mobile phase; The detection wavelength is 270nm.Number of theoretical plate calculates by the icariin peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the icariin reference substance, adds methanol and makes the solution that every 1ml contains 40ug, promptly.
The about 0.6g of this product is got in the preparation of need testing solution, and accurate the title decides, and with the suitable quantity of water dissolving, puts in the tool plug separatory funnel, uses ethyl acetate extraction 4 times, and each 10ml merges the ethyl acetate layer.Evaporate to dryness, residue 10ml dissolve with methanol filters promptly.
Accurate respectively reference substance solution and each 10ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures promptly.
This product contains icariin (C for every bag
33H
40O
15) must not be less than 1.5mg.
(3) osthole
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (67: 33) is a mobile phase; The detection wavelength is 249nm.Number of theoretical plate calculates by the osthole peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the osthole reference substance, adds methanol and makes the solution that every 1ml contains 50ug, promptly.
Granule for strengthening kidney is got in the preparation of need testing solution, porphyrize, and mixing is got about 1.5g, and accurate the title, decide, and puts in the tool plug conical flask, the accurate ethanol 50ml that adds, close plug claims to decide weight, and supersound process 1 hour claims to decide weight again, supply the weight that subtracts mistake with ethanol, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and the need testing solution 20ml of drawing of algoscopy injects chromatograph of liquid, measures, promptly.
This product contains osthole (C for every bag
15H
16O
3) must not be less than 0.8mg.
(4) schisandrin
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (13: 7) is a mobile phase; The detection wavelength is 250nm.Number of theoretical plate calculates by the schisandrin peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the schisandrin reference substance, adds methanol and makes the solution that every 1ml contains 30ug, promptly.
Granule for strengthening kidney is got in the preparation of need testing solution, porphyrize, and mixing is got about 2.0g, and accurate the title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, and supersound process 20 minutes claims to decide weight again, supply the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each 20ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures promptly.
This product contains schisandrin (C for every bag
24H
32O
7) must not be less than 0.4mg.
Embodiment 8: the discriminating of kidney capsule and assay
1. differentiate
(1) get 8 of this product, the 20ml that adds diethyl ether, reflux 1 hour filters. and filtrate volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Other gets Radix Angelicae Sinensis and each 0.5g of Rhizoma Chuanxiong control medicinal material, shines medical material solution in pairs with legal system.Drawing above-mentioned need testing solution and control medicinal material solution 2 μ l, put respectively on same silica gel g thin-layer plate, is developing solvent with normal hexane-ethyl acetate (9: 1), launches, and takes out, and dries, and puts under the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
(2) get the osthole reference substance, add ethanol and make the solution that every 1ml contains 1mg, in contrast product solution.Drawing above-mentioned reference substance solution and [discriminating] (1) item each 1 μ l of need testing solution down, put respectively on same silica gel g thin-layer plate, is developing solvent with cyclohexane extraction-ethyl acetate (7: 2), launches, and taking-up is dried, and puts under the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(3) get 15 of this product, porphyrize adds ethyl acetate 30ml, reflux 1 hour is put coldly, filters, filtrate is extracted 3 times with 5% sodium carbonate liquor jolting, and each 20ml merges sodium carbonate extraction liquid, with hydrochloric acid adjust pH to 2～3, the jolting of reuse ethyl acetate is extracted 2 times, each 30ml, combined ethyl acetate extracting solution, be concentrated into 1ml, as need testing solution.Other gets Radix Polygoni Multiflori control medicinal material 0.3g, shines medical material solution in pairs with legal system.Get the emodin reference substance again, add methanol and make the solution that every 1ml contains 0.2mg, in contrast product solution.Draw above-mentioned need testing solution 10 μ l, each 2 μ l of control medicinal material and reference substance solution, put respectively on same silica gel g thin-layer plate, upper solution with petroleum ether (30～60 ℃)-Ethyl formate-formic acid (15: 5: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show identical orange-yellow fluorescence speckle.Put in the ammonia steam smoked after, inspect under the daylight, speckle becomes redness.
(4) get 12 of this product, porphyrize adds n-butyl alcohol 30ml, and supersound process 30 minutes filters, and filtrate adds ammonia solution washing 2 times, and each 30ml discards ammonia solution, and n-butyl alcohol liquid evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets the icariin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (10: 1: 1: 1) be developing solvent, expansion was taken out with ethyl acetate-butanone-formic acid-water, dry, spray is put 105 ℃ of bakings several minutes, in the test sample chromatograph with 10% ethanol solution of sulfuric acid, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(5) get 2 of this product, porphyrize adds methanol 20ml, and ultrasonic 30 minutes, put coldly, filter, filtrate is as need testing solution.Other gets psoralen and the isopsoralen reference substance is an amount of, adds methanol and makes the mixed solution that every 1ml contains 4 μ g, in contrast product solution.With the octadecylsilane chemically bonded silica is filler; Methanol-water (40: 60) is a mobile phase, and the detection wavelength is 246nm.Accurate respectively reference substance solution and each 20ul of need testing solution of drawing injects chromatograph of liquid, measures.The retention time of main peak should be consistent with reference substance in the test sample chromatogram.
2. assay
(1) 2,3,5,4 '-tetrahydroxystilbene-2-O-b-D-glucoside lucifuge operation.
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Second eyeball-water (25: 75) is mobile phase; The detection wavelength is 320nm.Number of theoretical plate is by 2,3,5, and 4 '-tetrahydroxystilbene-2-O-b-D-glucoside peak calculates should be not less than 2000.
The preparation precision of reference substance solution takes by weighing 2,3,5, and 4 '-tetrahydroxystilbene-2-O-b-D-glucoside reference substance adds Diluted Alcohol and makes the solution that every 1ml contains 20ug, promptly.
This product under the weight differential item, porphyrize, mixing are got in the preparation of need testing solution, get about 0.25g, the accurate title, decide, and puts in the conical flask, the accurate Diluted Alcohol 50ml that adds claims to decide weight, reflux 30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with Diluted Alcohol, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each 20ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures promptly.
Every of this product contains Radix Polygoni Multiflori Preparata with 2,3,5,4 '-tetrahydroxystilbene-2-O-b-D-glucoside (C
20H
22O
9) meter, must not be less than 0.4mg.
(2) icariin
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Second eyeball-water (30: 70) is mobile phase; The detection wavelength is 270nm.Number of theoretical plate calculates by the icariin peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the icariin reference substance, adds methanol and makes the solution that every 1ml contains 40ug, promptly.
This product under the weight differential item, porphyrize, mixing are got in the preparation of need testing solution, get about 0.25g, the accurate title, decide, and adds water 10ml, put in the tool plug separatory funnel, use ethyl acetate extraction 4 times, each 10ml, the combined ethyl acetate layer, evaporate to dryness, residue add dissolve with methanol and are transferred in the 25ml measuring bottle, add methanol to scale, shake up, promptly.
Accurate respectively reference substance solution and each 20ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures promptly.
Every of this product contains Herba Epimedii with icariin (C
33H
40O
15) meter, must not be less than 0.35mg
(3) osthole
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (67: 33) is a mobile phase; The detection wavelength is 249nm.Number of theoretical plate calculates by the osthole peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the osthole reference substance, adds methanol and makes the solution that every 1ml contains 50ug, promptly.
This product content is got in the preparation of need testing solution, porphyrize, and mixing is got about 0.25g, and accurate the title, decide, and puts in the tool plug conical flask, the accurate ethanol 50ml that adds, close plug claims to decide weight, and supersound process 1 hour claims to decide weight again, supply the weight that subtracts mistake with ethanol, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and the need testing solution 20ml of drawing of algoscopy injects chromatograph of liquid, measures, promptly.
Every of this product contains Fructus Cnidii with osthole (C
15H
16O
3) meter, must not be less than 0.2mg
(4) schisandrin
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (13: 7) is a mobile phase; The detection wavelength is 250nm.Number of theoretical plate calculates by the schisandrin peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the schisandrin reference substance, adds methanol and makes the solution that every 1ml contains 30ug, promptly.
This product content is got in the preparation of need testing solution, porphyrize, and mixing is got about 0.3g, and accurate the title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, and supersound process 20 minutes claims to decide weight again, supply the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each 20ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures promptly.
Every of this product contains Fructus Schisandrae Chinensis with schisandrin (C
24H
32O
7) meter, must not be less than 0.1mg.
Claims (10)
1. Shenbao preparation, this Chinese medicine is the solid preparation of Chinese medicine of being made by following Chinese medicinal raw materials, following proportioning can change in proportion,
Fructus Cnidii 28 weight portion Rhizoma Chuanxiongs 28.3 weight portion Semen Cuscutae 66 weight portions
Fructus Psoraleae 28.5 weight portion Poria 30 weight portion Radix Ginseng Rubra 20 weight portions
Fructus Foeniculi 14.4 weight portion Fructus Schisandrae Chinensis 36 weight portion Fructus Rosae Laevigatae 94.6 weight portions
The Rhizoma Atractylodis Macrocephalae 14.2 weight portion Radix Angelicae Sinensis 46.8 weight portion Fructus Rubies 32.9 weight portions
Radix Polygoni Multiflori Preparata 74.4 weight portion Semen Plantaginiss 16.5 weight portion Radix Rehmanniae Preparata 94 weight portions
Fructus Lycii 66 weight portion Rhizoma Dioscoreaes 46.3 weight portion Herba Epimedii 94.6 weight portions
The Semen Trigonellae 94 weight portion Radixs Astragali 51.4 weight portion Herba Cistanches 47.3 weight portions
Radix Glycyrrhizae Preparata 14.2 weight portions
It is characterized in that its preparation method process following steps:
(1) ethanol percolation or the reflux, extract, of Fructus Cnidii, Herba Epimedii, Radix Angelicae Sinensis, Rhizoma Chuanxiong, Fructus Foeniculi usefulness 50-80% in the prescription;
(2) ethanol percolation or the reflux, extract, of Radix Ginseng Rubra usefulness 10-50% in the prescription, medicinal residues are standby;
(3) all the other ten Six-elements such as Fructus Rubi are with above-mentioned Radix Ginseng Rubra medicinal residues in the prescription, and water is carried or water extract-alcohol precipitation;
(4) extracting solution of above-mentioned (1), (2), (3) gained is concentrated in right amount, mixing after mixing/adding appropriate amount of auxiliary materials, vacuum drying/spray drying/lyophilization;
(5) the dry thing of above-mentioned (4) gained is made various solid preparations according to a conventional method.
2. according to the Shenbao preparation of claim 1, it is characterized in that, it is a solid preparation, the various solid dosage formss that comprise renal aid are as tablet, sugar coated tablet, film coated tablet, chewable tablet, effervescent tablet, dispersible tablet, capsule, hard capsule, soft capsule, pellt capsule, suck agent, electuary, granule, effervescent granule, pill, drop pill, pellet.
3. according to the preparation method of claim 1, it is characterized in that the preparation method of making concrete a certain preparation is as follows:
(1) makes the preparation method of 1000 tablets of tablets
Fructus Cnidii 93.3g Rhizoma Chuanxiong 94.3g Semen Cuscutae 220g
Fructus Psoraleae 95g Poria 100g joins 66.7g
Fructus Foeniculi 48g Fructus Schisandrae Chinensis 120g Fructus Rosae Laevigatae 315.3g
Rhizoma Atractylodis Macrocephalae 47.3g Radix Angelicae Sinensis 156g Fructus Rubi 109.7g
Radix Polygoni Multiflori Preparata 248g Semen Plantaginis 55g Radix Rehmanniae Preparata 313.3g
Fructus Lycii 220g Rhizoma Dioscoreae 154.3g Herba Epimedii 315.3g
Semen Trigonellae 313.3g Radix Astragali 171.3g Herba Cistanches 157.7g
Radix Glycyrrhizae Preparata 47.3g
More than 22 the flavor, Fructus Cnidii, Herba Epimedii, Radix Angelicae Sinensis, Rhizoma Chuanxiong, Fructus Foeniculi are ground into coarse powder, make solvent with 70% ethanol, flood after 48 hours,, collect the about 5000ml of percolate with the speed of per minute 1～3ml percolation slowly, reclaim ethanol, being evaporated to relative density is the clear paste of 1.10 (80 ℃ of heat are surveyed), filters filtrate for later use; Red ginseng powder is broken into coarse powder, adds 9 times of amount 20% alcohol dipping after 8 hours, the reflux, extract, secondary, and each 2 hours, merge extractive liquid, filtered, and filtrate recycling ethanol is concentrated into relative density and is the clear paste of 1.10 (80 ℃ of heat are surveyed), and is standby; Ten Six-elements such as all the other Fructus Rubies with the medicinal residues of Radix Ginseng Rubra through alcohol extraction, add 10 times of water gagings and soaked 1 hour, decoct secondary, each 2 hours, collecting decoction, filter, filtrate is concentrated into the clear paste that relative concentration is 1.16 (80 ℃ of heat are surveyed), adds ethanol and makes that to contain the alcohol amount be 65%, left standstill 48 hours, and got supernatant and reclaim ethanol, being concentrated into relative density is the clear paste of 1.10 (80 ℃ of heat are surveyed), add extracting solution and red ginseng extracts such as above-mentioned Fructus Cnidii, mixing, vacuum drying, pulverize, add microcrystalline Cellulose 51g, micropowder silica gel 6g, mixing is made granule, dry, add magnesium stearate 2.5g, mixing is pressed into 1000, coating promptly gets the renal aid sheet.
(2) make the preparation method of 1000 tablet chewable tablets
Fructus Cnidii 140g Rhizoma Chuanxiong 141.5g Semen Cuscutae 330g
Fructus Psoraleae 142.5g Poria 150g Radix Ginseng Rubra 100g
Fructus Foeniculi 72g Fructus Schisandrae Chinensis 180g Fructus Rosae Laevigatae 473g
Rhizoma Atractylodis Macrocephalae 71g Radix Angelicae Sinensis 234g Fructus Rubi 164.5g
Radix Polygoni Multiflori Preparata 372g Semen Plantaginis 82.5g Radix Rehmanniae Preparata 470g
Fructus Lycii 330g Rhizoma Dioscoreae 231.5g Herba Epimedii 473g
Semen Trigonellae 470g Radix Astragali 257g Herba Cistanches 236.5g
Radix Glycyrrhizae Preparata 71g
More than 22 the flavor, Fructus Cnidii, Herba Epimedii, Radix Angelicae Sinensis, Rhizoma Chuanxiong, Fructus Foeniculi are ground into coarse powder, make solvent with 70% ethanol, flood after 48 hours,, collect the about 7500ml of percolate with the speed of per minute 1～3ml percolation slowly, reclaim ethanol, being evaporated to relative density is the clear paste of 1.10 (80 ℃ of heat are surveyed), filters filtrate for later use; Red ginseng powder is broken into coarse powder, adds 9 times of amount 20% alcohol dipping after 8 hours, the reflux, extract, secondary, and each 2 hours, merge extractive liquid, filtered, and filtrate recycling ethanol is concentrated into relative density and is the clear paste of 1.10 (80 ℃ of heat are surveyed), and is standby; Ten Six-elements such as all the other Fructus Rubies with the medicinal residues of Radix Ginseng Rubra through alcohol extraction, add 10 times of water gagings and soaked 1 hour, decoct secondary, each 2 hours, collecting decoction, filter, filtrate is concentrated into relative concentration be 1.16 clear paste of (80 ℃ of heat are surveyed), adds ethanol and makes that to contain the alcohol amount be 65%, leaves standstill 48 hours, get supernatant and reclaim ethanol, being concentrated into relative density is the clear paste of 1.10 (80 ℃ of heat are surveyed), adds extracting solution and red ginseng extracts such as above-mentioned Fructus Cnidii, mixing, add betacyclodextrin 318g, mixing, vacuum drying is pulverized, add Aspartane 10g, mixing is made granule, drying in right amount with 90% ethanol; Add magnesium stearate 3g, mixing is pressed into 1000, and the bag film-coat promptly gets the renal aid chewable tablet.
(3) it is as follows to make the particulate preparation method of 1000g:
Fructus Cnidii 93.3g Rhizoma Chuanxiong 94.3g Semen Cuscutae 220g
Fructus Psoraleae 95g Poria 100g Radix Ginseng Rubra 66.7g
Fructus Foeniculi 48g Fructus Schisandrae Chinensis 120g Fructus Rosae Laevigatae 315.3g
Rhizoma Atractylodis Macrocephalae 47.3g Radix Angelicae Sinensis 156g Fructus Rubi 109.7g
Radix Polygoni Multiflori Preparata 248g Semen Plantaginis 55g Radix Rehmanniae Preparata 313.3g
Fructus Lycii 220g Rhizoma Dioscoreae 154.3g Herba Epimedii 315.3g
Semen Trigonellae 313.3g Radix Astragali 171.3g Herba Cistanches 157.7g
Radix Glycyrrhizae Preparata 47.3g
More than 22 the flavor, Fructus Cnidii, Herba Epimedii, Radix Angelicae Sinensis, Rhizoma Chuanxiong, Fructus Foeniculi are ground into coarse powder, make solvent with 70% ethanol, flood after 48 hours,, collect the about 7000ml of percolate with the speed of per minute 1～3ml percolation slowly, reclaim ethanol, being evaporated to relative density is the clear paste of 1.05 (heat is surveyed), filters filtrate for later use; Red ginseng powder is broken into coarse powder, adds 9 times of amount 20% alcohol dipping after 8 hours, the reflux, extract, secondary, and each 2 hours, merge extractive liquid, filtered, and filtrate recycling ethanol is concentrated into relative density and is the clear paste of 1.05 (heat is surveyed), and is standby; Ten Six-elements such as all the other Fructus Rubies, with the medicinal residues of Radix Ginseng Rubra through alcohol extraction, add 10 times of water gagings and soaked 1 hour, decoct secondary, each 2 hours, collecting decoction, filter, filtrate is concentrated into the clear paste that relative concentration is 1.10 (heat is surveyed), adds ethanol and makes and contain the alcohol amount and reach 65%, left standstill 48 hours, get supernatant and reclaim ethanol, being concentrated into relative density is the clear paste of 1.05 (heat is surveyed), adds extracting solution and red ginseng extracts such as above-mentioned Fructus Cnidii, mixing, add dextrin 500g, spray drying, dry granulation, make granule 1000 grams altogether, promptly get granule for strengthening kidney.
(4) make the preparation method of 1000 capsules
Fructus Cnidii 70g Rhizoma Chuanxiong 70.75g Semen Cuscutae 165g
Fructus Psoraleae 71.25g Poria 75g Radix Ginseng Rubra 50g
Fructus Foeniculi 36g Fructus Schisandrae Chinensis 90g Fructus Rosae Laevigatae 236.5g
Rhizoma Atractylodis Macrocephalae 35.5g Radix Angelicae Sinensis 117g Fructus Rubi 82.25g
Radix Polygoni Multiflori Preparata 186g Semen Plantaginis 41.25g Radix Rehmanniae Preparata 235g
Fructus Lycii 165g Rhizoma Dioscoreae 115.75g Herba Epimedii 236.5g
Semen Trigonellae 235g Radix Astragali 128.5g Herba Cistanches 118.25g
Radix Glycyrrhizae Preparata 35.5g
More than 22 the flavor, Fructus Cnidii, Herba Epimedii, Radix Angelicae Sinensis, Rhizoma Chuanxiong, Fructus Foeniculi are ground into coarse powder, make solvent with 70% ethanol, flood after 48 hours,, collect the about 3750ml of percolate with the speed of per minute 1～3ml percolation slowly, reclaim ethanol, being evaporated to relative density is the clear paste of 1.10 (80 ℃ of heat are surveyed), filters filtrate for later use; Red ginseng powder is broken into coarse powder, adds 9 times of amount 20% alcohol dipping after 8 hours, the reflux, extract, secondary, and each 2 hours, merge extractive liquid, filtered, and filtrate recycling ethanol is concentrated into relative density and is the clear paste of 1.10 (80 ℃ of heat are surveyed), and is standby; Ten Six-elements such as all the other Fructus Rubies with the medicinal residues of Radix Ginseng Rubra through alcohol extraction, add 10 times of water gagings and soaked 1 hour, decoct secondary, each 2 hours, collecting decoction filtered, filtrate is concentrated into the clear paste that relative concentration is 1.16 (80 ℃ of heat are surveyed), add ethanol and make that to contain alcohol amount be 65%, left standstill 48 hours, get supernatant and reclaim ethanol, being concentrated into relative density is the clear paste of 1.10 (80 ℃ of heat are surveyed), add extracting solution and red ginseng extracts such as above-mentioned Fructus Cnidii, mixing, vacuum drying, pulverize, add micropowder silica gel 4g, mixing incapsulates, make 1000, promptly.
4. the method for quality control of a Shenbao preparation is characterized in that, contains in following assay and the qualitative identification one or more:
(1) assay
A. measure in the Shenbao preparation 2,3,5 with high-efficient liquid phase technique, the content of 4 '-tetrahydroxystilbene-2-O-b-D-glucoside;
B. measure content Determination of Icariin in the Shenbao preparation with high-efficient liquid phase technique;
C. measure the content of osthole in the Shenbao preparation with high-efficient liquid phase technique;
D. measure the content of schisandrin in the Shenbao preparation with high-efficient liquid phase technique.
(2) qualitative identification
A. differentiate Radix Angelicae Sinensis and Rhizoma Chuanxiong in the Shenbao preparation with thin layer chromatography;
B. differentiate Fructus Cnidii in the Shenbao preparation with thin layer chromatography;
C. differentiate Radix Polygoni Multiflori Preparata in the Shenbao preparation with thin layer chromatography;
D. differentiate Herba Epimedii in the Shenbao preparation with thin layer chromatography;
E. differentiate Fructus Psoraleae in the Shenbao preparation with high-efficient liquid phase technique.
5. the method for quality control of a Shenbao preparation is characterized in that, contains in following assay and the qualitative identification one or more:
(1) assay
A. high-efficient liquid phase technique measures in the Shenbao preparation 2,3,5, the content of 4 '-tetrahydroxystilbene-2-O-b-D-glucoside
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels; Second eyeball-water (5-70: 95-30) be mobile phase; UV-detector or diode array detector.Number of theoretical plate is by 2,3,5, and 4 '-tetrahydroxystilbene-2-O-b-D-glucoside peak calculates should be not less than 2000.
The preparation precision of reference substance solution takes by weighing 2,3,5, and 4 '-tetrahydroxystilbene-2-O-b-D-glucoside reference substance adds ethanol or Diluted Alcohol or other The suitable solvent and makes the solution of determining concentration, product solution in contrast.
The preparation precision of need testing solution takes by weighing product or the product content thing is an amount of, with the methanol/ethanol extraction of suitable concentration, as need testing solution.
Accurate respectively reference substance solution and an amount of volume of need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly.
B. high-efficient liquid phase technique is measured icariin content in the Shenbao preparation
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels; Second eyeball-water (5-70: 95-30) be mobile phase; UV-detector or diode array detector.Number of theoretical plate calculates by the icariin peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the icariin reference substance, adds methanol or other The suitable solvent and makes the solution of determining concentration, product solution in contrast.
The preparation precision of need testing solution takes by weighing product or the product content thing is an amount of, adds the suitable quantity of water dissolving, extract with ethyl acetate or other The suitable solvent, and the extracting solution evaporate to dryness, residue dissolves with The suitable solvent, as need testing solution.
Accurate respectively reference substance solution and an amount of volume of need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly.
C. high-efficient liquid phase technique is measured osthole content in the Shenbao preparation
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels; Methanol-water (40-85: 60-15) be mobile phase; UV-detector or diode array detector.Number of theoretical plate calculates by the osthole peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the osthole reference substance, adds methanol or other The suitable solvent and makes the solution of determining concentration, product solution in contrast.
The preparation precision of need testing solution takes by weighing product or the product content thing is an amount of, with the methanol/ethanol extraction of suitable concentration, as need testing solution.
Accurate respectively reference substance solution and an amount of volume of need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly.
D. high-efficient liquid phase technique is measured schisandrin content in the Shenbao preparation
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels; Methanol-water (5-30: 2-15) be mobile phase; UV-detector or diode array detector.Number of theoretical plate calculates by the schisandrin peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the schisandrin reference substance, adds methanol or other The suitable solvent and makes the solution of determining concentration, product solution in contrast.
The preparation precision of need testing solution takes by weighing product or the product content thing is an amount of, with the methanol/ethanol extraction of suitable concentration, as need testing solution.
Accurate respectively reference substance solution and an amount of volume of need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly.
(2) qualitative identification
A. thin layer chromatography is differentiated Radix Angelicae Sinensis and Rhizoma Chuanxiong in the Shenbao preparation
Get product or the product content thing is an amount of, add diethyl ether or other The suitable solvent is extracted, extracting solution is as need testing solution, or extracting solution steams/volatilize, and residue adds The suitable solvent makes dissolving, as need testing solution.Other gets Radix Angelicae Sinensis and the Rhizoma Chuanxiong control medicinal material is an amount of, makes control medicinal material solution after the extraction.Each is an amount of to draw above-mentioned need testing solution and control medicinal material solution, puts respectively on same silica gel G or silica gel H lamellae, with normal hexane-ethyl acetate (3-30: 0.3-3) be developing solvent, launch, take out, dry, put under the ultra-violet lamp and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
B. thin layer chromatography is differentiated Fructus Cnidii in the Shenbao preparation
Get product or the product content thing is an amount of, add diethyl ether or other The suitable solvent is extracted, extracting solution is as need testing solution, or extracting solution steams/volatilize, and residue adds The suitable solvent makes dissolving, as need testing solution.It is an amount of that other gets the osthole reference substance, and solubilizer is made reference substance solution in right amount.Each is an amount of to draw above-mentioned need testing solution and reference substance solution, puts respectively on same silica gel G or silica gel H lamellae, with benzene-ethyl acetate (10-50: 0.3-2) be developing solvent, launch, take out, dry, put under the ultra-violet lamp and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
C. thin layer chromatography is differentiated Radix Polygoni Multiflori Preparata in the Shenbao preparation
Get product or the product content thing is an amount of, adding ethyl acetate or other The suitable solvent extracts, extracting solution extracts with the sodium carbonate liquor of suitable concentration, sodium carbonate extraction liquid hydrochloric acid adjust pH to 1～4, reuse ethyl acetate or the extraction of other The suitable solvent, extract is as need testing solution, or extract steams/volatilizes, residue adds The suitable solvent makes dissolving, as need testing solution.It is an amount of that other gets the Radix Polygoni Multiflori control medicinal material, makes control medicinal material solution after the extraction.It is an amount of to get the emodin reference substance again, and solubilizer is made reference substance solution in right amount.Each is an amount of to draw above-mentioned need testing solution, control medicinal material and reference substance solution, put respectively on same silica gel G or silica gel H lamellae, (5-25: 2-8: upper solution 0.4-2) is developing solvent with petroleum ether (30～60 ℃)-Ethyl formate-formic acid, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show identical orange-yellow fluorescence speckle.Put in the ammonia steam smoked after, inspect under the daylight, speckle becomes redness.
D. thin layer chromatography is differentiated Herba Epimedii in the Shenbao preparation
Get product or the product content thing is an amount of, add n-butyl alcohol or other The suitable solvent and extract, extracting solution washs with ammonia solution, discards ammonia solution, and extracting solution is as need testing solution, or extracting solution steams/volatilize, and residue adds The suitable solvent makes dissolving, as need testing solution.Other gets the icariin reference substance, and solubilizer is made reference substance solution in right amount.Each is an amount of to draw above-mentioned two kinds of solution, put respectively on same silica gel G or silica gel H lamellae, with ethyl acetate-butanone-formic acid-water (3-30: 0.4-4: 0.4-4: 0.4-4) be developing solvent, launch, take out, dry, spray is heated to colour developing with 10% ethanol solution of sulfuric acid, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
E. high-efficient liquid phase technique is differentiated Fructus Psoraleae in the Shenbao preparation
Get product or the product content thing is an amount of, add methanol or other The suitable solvent and extract, extracting solution is as need testing solution.Other gets psoralen and the isopsoralen reference substance is an amount of, and solubilizer is made reference substance solution in right amount.With the octadecylsilane chemically bonded silica is filler; Methanol-water (20-80: 80-20) be mobile phase, UV-detector or diode array detector.Accurate respectively reference substance solution and each an amount of volume of need testing solution drawn injects chromatograph of liquid, measures.The retention time of main peak should be consistent with reference substance in the test sample chromatogram.
6. according to the method for quality control of the Shenbao preparation of claim 5, it is characterized in that:
(1) described extraction can be adopted conventional methods such as supersound process, reflux, extract,, microwave extraction, vibration extraction;
(2) 2,3,5, the mobile phase of the assay of 4 '-tetrahydroxystilbene-2-O-b-D-glucoside can also be methanol-acetonitrile-water (2-10: 0.5-2: 4-20), methanol-water (5-70: 95-30) or other suitable mobile phase;
(3) mobile phase measured of content Determination of Icariin can also be methanol-water-glacial acetic acid (40-80: 20-60: 0.2-1), methanol-water (5-70: 95-30) or other suitable mobile phase;
(4) mobile phase of the assay of osthole can also be methanol-water-oxolane (30-75: 20-60: 2-10), acetonitrile-water (5-70: 95-30) or other suitable mobile phase;
(5) mobile phase of the assay of schisandrin can also be acetonitrile-water (5-70: 95-30) or other suitable mobile phase;
(6) developing solvent differentiated of the thin layer chromatography of Radix Angelicae Sinensis and Rhizoma Chuanxiong can also be petroleum ether (60-90 ℃)-ethyl acetate (5-25: 0.5-5), cyclohexane extraction-ethyl acetate (5-25: 0.5-5) or other suitable developing solvent;
(7) developing solvent differentiated of the thin layer chromatography of Fructus Cnidii can also be cyclohexane extraction-ethyl acetate (3-20: 0.5-5), normal hexane-ethyl acetate (4-20: 0.4-4) or other suitable developing solvent;
(8) developing solvent differentiated of the thin layer chromatography of Radix Polygoni Multiflori Preparata can also be chloroform-methanol (5-15: 0.5-5), petroleum ether (30-60 ℃)-ethyl acetate-glacial acetic acid (50-150: 5-50: 0.5-5) or other suitable developing solvent;
(9) both can adopt reference substance among qualitative identification a, b, c, the d, and also can adopt control medicinal material to compare, or both all adopt; Both can adopt two kinds of reference substances among the qualitative identification e, also can only adopt wherein a kind of reference substance in contrast.
7. the method for quality control of a Shenbao preparation is characterized in that, contains in following assay and the qualitative identification one or more:
(1) assay
A. high-efficient liquid phase technique measures in the Shenbao preparation 2,3,5, the content of 4 '-tetrahydroxystilbene-2-O-b-D-glucoside
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Second eyeball-water (25: 75) is mobile phase; The detection wavelength is 320nm.Number of theoretical plate is by 2,3,5, and 4 '-tetrahydroxystilbene-2-O-b-D-glucoside peak calculates should be not less than 2000.
The preparation precision of reference substance solution takes by weighing 2,3,5, and 4 '-tetrahydroxystilbene-2-O-b-D-glucoside reference substance adds Diluted Alcohol and makes the solution that every 1ml contains 20ug, promptly.
Product is got in the preparation of need testing solution or the product content thing is an amount of, puts in the conical flask, and the accurate Diluted Alcohol 50ml that adds claims decide weight, and reflux 30 minutes is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with Diluted Alcohol, shakes up, and filtration is got subsequent filtrate, promptly.
Accurate respectively reference substance solution and each 20ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures, promptly.
B. high-efficient liquid phase technique is measured icariin content in the Shenbao preparation
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Second eyeball-water (30: 70) is mobile phase; The detection wavelength is 270nm.Number of theoretical plate calculates by the icariin peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the icariin reference substance, adds methanol and makes the solution that every 1ml contains 40ug, promptly.
Product is got in the preparation of need testing solution or the product content thing is an amount of, adds water 10ml, puts in the tool plug separatory funnel, uses ethyl acetate extraction 4 times, each 10ml, combined ethyl acetate layer, evaporate to dryness, residue add dissolve with methanol and are transferred in the 25ml measuring bottle, add methanol to scale, shake up, promptly.
Accurate respectively reference substance solution and the need testing solution 20ml of drawing of algoscopy injects chromatograph of liquid, measures, promptly.
C. high-efficient liquid phase technique is measured osthole content in the Shenbao preparation
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (67: 33) is a mobile phase; The detection wavelength is 249nm.Number of theoretical plate calculates by the osthole peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the osthole reference substance, adds methanol and makes the solution that every 1ml contains 50ug, promptly.
Product is got in the preparation of need testing solution or the product content thing is an amount of, puts in the tool plug conical flask, the accurate ethanol 50ml that adds, and close plug claims to decide weight, and supersound process 1 hour claims to decide weight again, supplies the weight that subtracts mistake with ethanol, shakes up, and filters, and gets subsequent filtrate, promptly.
Accurate respectively reference substance solution and the need testing solution 20ml of drawing of algoscopy injects chromatograph of liquid, measures, promptly.
D. high-efficient liquid phase technique is measured schisandrin content in the Shenbao preparation
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (13: 7) is a mobile phase; The detection wavelength is 250nm.Number of theoretical plate calculates by the schisandrin peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the schisandrin reference substance, adds methanol and makes the solution that every 1ml contains 30ug, promptly.
Product is got in the preparation of need testing solution or the product content thing is an amount of, puts in the tool plug conical flask, the accurate methanol 50ml that adds, and close plug claims to decide weight, and supersound process 20 minutes claims to decide weight again, supplies the weight that subtracts mistake with methanol, shakes up, and filters, and gets subsequent filtrate, promptly.
Accurate respectively reference substance solution and each 20ml of need testing solution of drawing of algoscopy injects chromatograph of liquid, measures, promptly.
(2) qualitative identification
A. thin layer chromatography is differentiated Radix Angelicae Sinensis and Rhizoma Chuanxiong in the Shenbao preparation
Get product or the product content thing is an amount of, the 30ml that adds diethyl ether, reflux 1 hour filters. and filtrate volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Other gets Radix Angelicae Sinensis and each 0.5g of Rhizoma Chuanxiong control medicinal material, shines medical material solution in pairs with legal system.Drawing above-mentioned need testing solution and control medicinal material solution 2 μ l, put respectively on same silica gel g thin-layer plate, is developing solvent with normal hexane-ethyl acetate (9: 1), launches, and takes out, and dries, and puts under the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
B. thin layer chromatography is differentiated Fructus Cnidii in the Shenbao preparation
Get product or the product content thing is an amount of, the 30ml that adds diethyl ether, reflux 1 hour filters. and filtrate volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Get the osthole reference substance, add ethanol and make the solution that every 1ml contains 1mg, in contrast product solution.Drawing each 1 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with benzene-ethyl acetate (30: 1) or cyclohexane extraction-ethyl acetate (7: 2), launches, and takes out, and dries, and puts under the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
C. thin layer chromatography is differentiated Radix Polygoni Multiflori Preparata in the Shenbao preparation
Get product or the product content thing is an amount of, the 30ml that adds diethyl ether, reflux 1 hour filters. and filtrate volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Add ethyl acetate 30ml, reflux 1 hour is put cold, filter, filtrate is extracted 3 times with 5% sodium carbonate liquor jolting, and each 20ml merges sodium carbonate extraction liquid, with hydrochloric acid adjust pH to 2～3, the jolting of reuse ethyl acetate is extracted 2 times, each 30ml, combined ethyl acetate extracting solution, be concentrated into 1ml, as need testing solution.Other gets Radix Polygoni Multiflori control medicinal material 0.3g, shines medical material solution in pairs with legal system.Get the emodin reference substance again, add methanol and make the solution that every 1ml contains 0.2mg, in contrast product solution.Draw above-mentioned need testing solution 10 μ l, each 2 μ l of control medicinal material and reference substance solution, put respectively on same silica gel g thin-layer plate, upper solution with petroleum ether (30～60 ℃)-Ethyl formate-formic acid (15: 5: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show identical orange-yellow fluorescence speckle.Put in the ammonia steam smoked after, inspect under the daylight, speckle becomes redness.
D. thin layer chromatography is differentiated Herba Epimedii in the Shenbao preparation
Get product or the product content thing is an amount of, the 30ml that adds diethyl ether, reflux 1 hour filters. and filtrate volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Add n-butyl alcohol 30ml, supersound extraction 30 minutes filters, and filtrate adds ammonia solution washing 2 times, and each 30ml discards ammonia solution, and n-butyl alcohol liquid evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets the icariin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (10: 1: 1: 1) be developing solvent, expansion was taken out with ethyl acetate-butanone-formic acid-water, dry, spray is put 105 ℃ of bakings several minutes, in the test sample chromatograph with 10% ethanol solution of sulfuric acid, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
E. high-efficient liquid phase technique is differentiated Fructus Psoraleae in the Shenbao preparation
Get product or the product content thing is an amount of, add methanol 40ml, supersound extraction 30 minutes is put coldly, filters, and filtrate is as need testing solution.Other gets psoralen and the isopsoralen reference substance is an amount of, adds methanol and makes the mixed solution that every 1ml contains 4 μ g, in contrast product solution.Measure according to high performance liquid chromatography (appendix ID of Chinese Pharmacopoeia version in 2005).With the octadecylsilane chemically bonded silica is filler; Methanol-water (40: 60) is a mobile phase, and the detection wavelength is 246nm.Accurate respectively reference substance solution and each 20ul of need testing solution of drawing injects chromatograph of liquid, measures.The retention time of main peak should be consistent with reference substance in the test sample chromatogram.
8. method according to claim 7, it is characterized in that, the amount of described extraction sample or dissolving extract solvent for use, ultrasonic or time, standardize solution or dissolving back volume, point sample amount or the sample size of reflux, extract,, the concentration of reference substance can be that benchmark changes with described occurrence, or change in proportion; Both can adopt reference substance among described qualitative identification a, b, c, the d, and also can adopt control medicinal material to compare, or both all adopt, both can adopt two kinds of reference substances among the qualitative identification e, also can only adopt wherein a kind of reference substance in contrast; Described supersound process also can adopt conventional extracting method such as reflux, extract,, microwave extraction, vibration extraction, and described reflux, extract, also can adopt conventional extracting method such as supersound process, microwave extraction, vibration extraction.
9. according to claim 4,5,7 described methods, it is characterized in that, can be used to detect any dosage form of the Shenbao preparation that makes by the described preparation method of claim 1 or make by other preparation method, as tablet, sugar coated tablet, film coated tablet, chewable tablet, effervescent tablet, dispersible tablet, capsule, hard capsule, soft capsule, pellt capsule, oral liquid, syrup, suck agent, electuary, granule, effervescent granule, pill, drop pill, pellet.
10. according to claim 4,5,7 described content assaying methods, it is characterized in that, in the Shenbao preparation 2,3,5, the content limit of 4 '-tetrahydroxystilbene-2-O-b-D-glucoside is: contain Radix Polygoni Multiflori Preparata with 2 in the once minimum dose, 3,5,4 '-tetrahydroxystilbene-2-O-b-D-glucoside (C20H22O9) meter must not be less than 1.3mg; The content Determination of Icariin limit is: contain Herba Epimedii in the once minimum dose in icariin (C33H40O15), must not be less than 1.4mg; The content limit of osthole is: contain Fructus Cnidii in the once minimum dose in osthole (C15H16O3), must not be less than 0.8mg; The content limit of schisandrin is: contain Fructus Schisandrae Chinensis in the once minimum dose in schisandrin (C24H32O7), must not be less than 0.4mg; Above-mentioned content limit is the minimum content limit, can improve content limit according to the concrete condition of producing.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102139012B (en) * | 2010-02-03 | 2013-01-09 | 天津中新药业集团股份有限公司隆顺榕制药厂 | Quality control method for kidney tonifying syrup |
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| CN105675741A (en) * | 2015-12-30 | 2016-06-15 | 成都九芝堂金鼎药业有限公司 | Method for determining content of effective components in hair growing pill |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102139012B (en) * | 2010-02-03 | 2013-01-09 | 天津中新药业集团股份有限公司隆顺榕制药厂 | Quality control method for kidney tonifying syrup |
| CN103063793A (en) * | 2013-01-01 | 2013-04-24 | 吉林紫鑫药业股份有限公司 | Method for determining content of cynomorium songaricum kidney-tonifying capsule |
| CN103163271A (en) * | 2013-03-29 | 2013-06-19 | 贵州省烟草科学研究院 | Measuring method for residual amount of cnidium lactone in tobacco leaves |
| CN103163271B (en) * | 2013-03-29 | 2015-04-08 | 贵州省烟草科学研究院 | Measuring method for residual amount of cnidium lactone in tobacco leaves |
| CN104906312A (en) * | 2015-06-15 | 2015-09-16 | 通化万通药业股份有限公司 | Shenbao (Chinese character) mixture and preparation method thereof |
| CN105675741A (en) * | 2015-12-30 | 2016-06-15 | 成都九芝堂金鼎药业有限公司 | Method for determining content of effective components in hair growing pill |
| CN106153813A (en) * | 2016-08-29 | 2016-11-23 | 贵州信邦制药股份有限公司 | The discrimination method of rheum emodin in ostealgia medicated wine |
| CN106248841A (en) * | 2016-08-29 | 2016-12-21 | 贵州信邦制药股份有限公司 | The content assaying method of Radix Polygoni Multiflori Preparata in anti-rheumatism medicated wine |
| CN107179374A (en) * | 2017-06-29 | 2017-09-19 | 江苏海昇药业有限公司 | The detection method of tonic tablet for essence and blood finger-print |
| CN107179374B (en) * | 2017-06-29 | 2019-10-22 | 江苏海昇药业有限公司 | The detection method of tonic tablet for essence and blood finger-print |
| CN114509507A (en) * | 2020-11-16 | 2022-05-17 | 上海新亚药业邗江有限公司 | Quantitative method for simultaneously determining multiple indexes in Huangjingzanyu capsule |
| CN114509507B (en) * | 2020-11-16 | 2024-03-12 | 上海新亚药业邗江有限公司 | Quantitative method for simultaneously measuring multiple indexes in polygonatum sibiricum Zanyu capsules |
| CN113281439A (en) * | 2021-07-25 | 2021-08-20 | 江西汇仁药业股份有限公司 | Quality control detection method of Shenbao tablets |
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