CN101474274B - Quality control method of Shensu Chinese medicine preparation - Google Patents
Quality control method of Shensu Chinese medicine preparation Download PDFInfo
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Abstract
The invention relates to a quality control method for Shensu Chinese herbal preparation, belonging to the technical field of medicine. The Shensu Chinese herbal preparation is composed of dangshen, dried orange peel, kudzuvine root, and the like, and is suitable for people suffering from the symptoms such as cold caused by weakness, chillness and fever, headaches and stuffy nose, cough and much sputum, and chest distress and vomiting and regurgitation, etc. The quality control method of the invention provides a test index, method, technologies and the like for relevant production and test institutions, so that the quality control of Chinese herbal preparation is bettered, the safety of the medicine use is guaranteed, the guidance for production is improved, the production process control is stricter and more reasonable and the invention can lead the consumers to comprehensively understand the product quality.
Description
Technical field:
The present invention relates to a kind of method of quality control that is used to join Soviet Union's Chinese medicine preparation, belong to technical field of medicaments.
Background technology:
Ginseng Soviet Union Chinese medicine preparation is to form with medical materials such as Radix Puerariae, Pericarpium Citri Reticulatae, Radix Codonopsis, has the effect of expelling wind and cold, expelling phlegm for arresting cough.Be used for weak anemofrigid cold, fever with aversion to cold, headache nasal obstruction, cough with copious phlegm, vomiting uncomfortable in chest.Pharmaceutical preparation must be on the basis that guarantees the constant product quality controllable safety; Constantly more new development in order better to control the quality of this Chinese medicine preparation, guarantees the safety of medication; Better instruct and produce; Make technology controlling and process rationally strict more, make consumer's ability full appreciation product quality, need research, control this Chinese medicine preparation method for quality.Though done number of research projects on the preparation technology of many pharmacy worker's products; But it is the quality of reactor product comprehensively at all; Be become a full member the 31st of standard of new drug for the capsular method of quality control of ginseng Soviet Union at present, just adopted Hesperidin, adopted puerarin simultaneously as differentiating and containing the survey index as differentiating as differentiating; The discriminating of this method and contain survey and all adopt thin layer chromatography to carry out; Tlc determination content poor reproducibility, it is inaccurate to measure the result, is not very rationally with this quality that is used for controlling this Chinese medicine preparation only; If the index with other is controlled,, relatively be difficult to implement owing to do not have ready-made detection scheme, testing conditions etc.
Summary of the invention
The objective of the invention is to: be provided for joining the method for quality control of Soviet Union's Chinese medicine preparation, this method provides means, technical method of the index that detects, detection or the like to relevant production, testing agency; So that better control the quality of this Chinese medicine preparation, guarantee the safety of medication, can better instruct production, make controlling of production process rationally strict more, make consumer's ability full appreciation product quality.
The present invention relates to the method for quality control of the Chinese medicine preparation that Pericarpium Citri Reticulatae medical material or its extract, codonopsis pilosula or its extract etc. process according to certain ratio prescription; Mainly comprise projects such as discriminating, assay, it be just lobetyolin, glucose, platycodin, puerarin, naringin, Hesperidin, praeruptorin A, Praeruptorin B, constuslactone, enoxolone, Radix Codonopsis control medicinal material, Radix Puerariae medical material, Pericarpium Citri Reticulatae control medicinal material, Radix Aucklandiae control medicinal material, in all or part of kind as the detection index of the quality control of this Chinese medicine preparation.
A kind of method of quality control that is used to join Soviet Union's Chinese medicine preparation of the present invention, it is as the discrimination method of this Chinese medicine preparation, the detection index of content assaying method with all or part of kind in puerarin, glucose, Hesperidin, Radix Codonopsis control medicinal material, Pericarpium Citri Reticulatae control medicinal material, naringin, the Radix Aucklandiae control medicinal material.
A kind of method of quality control that is used to join Soviet Union's Chinese medicine preparation of the present invention, it is to adopt all or part of method as discriminating in the following method:
Discriminating for Radix Codonopsis: get the content 5g of these article, water-wet is extracted 3 times with petroleum ether (60～90 ℃) jolting, and each 20ml merges petroleum ether, volatilizes, and residue adds petroleum ether (60～90 ℃) 1ml makes dissolving, as need testing solution.Other gets Radix Codonopsis control medicinal material 2g, and decocte with water 1 hour is concentrated into 25ml, puts coldly, extracts 3 times with petroleum ether (60～90 ℃) jolting, and each 20ml shines medical material solution in pairs with legal system.Draw above-mentioned need testing solution 15 μ l, control medicinal material solution 10 μ l put respectively on same silica gel g thin-layer plate, are developing solvent with petroleum ether (60～90 ℃)-ethyl acetate-formic acid (40: 10: 0.1); Launch, take out, dry; Spray is with 10% ethanol solution of sulfuric acid, and putting 105 ℃, to be heated to the speckle colour developing clear, puts 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 the fluorescence speckle of same color.
Discriminating for Pericarpium Citri Reticulatae: get Pericarpium Citri Reticulatae control medicinal material 2g, decocte with water 1 hour filters, and the filtrating evaporate to dryness adds methanol 5ml and makes dissolving, filters, as control medicinal material solution.Other gets these article content 2g, adds methanol 25ml ultrasonic 15 minutes, filters, and the filtrating evaporate to dryness adds methanol 2ml and makes dissolving, filters, and filtrating is as need testing solution.Draw each 1 μ l of above-mentioned need testing solution and control medicinal material solution, reference substance solution 5 μ l put respectively on same silica GF254 lamellae; With normal hexane-ethyl acetate-methanol-formic acid-ammonia (2: 3: 2: 0.04: 0.4) is developing solvent, launches, and takes out; Dry, spray is put under ultra-violet lamp (365nm) and the wavelength 254nm and is inspected with the aluminum chloride test solution; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
Discriminating for the Radix Aucklandiae: get the content 10g of these article, the 30ml that adds diethyl ether, supersound process 10 minutes filters, and filtrating volatilizes, and residue adds ethanol 0.5ml makes dissolving, as need testing solution.Other gets Radix Aucklandiae control medicinal material 0.2g, and the 5ml that adds diethyl ether shines medical material solution in pairs with legal system; Perhaps getting the constuslactone reference substance again adds methanol and processes saturated solution; Draw above-mentioned need testing solution 5～10 μ l, control medicinal material solution 2～4 μ l perhaps get reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate; With normal hexane-benzene-ethyl acetate (14: 3: 3) is developing solvent, launches, and takes out; Dry, spray is with 1% vanillin sulfuric acid solution, put 105 ℃ dry by the fire to speckle colour developing clear; In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the speckle of same color.
A kind of method of quality control that is used to join Soviet Union's Chinese medicine preparation of the present invention is characterized in that: adopt all or part of method as assay in the following method:
Method 1: adopt content of puerarin in these article of high effective liquid chromatography for measuring; Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filler; Methanol-water-36% acetic acid (20: 75: 5) is mobile phase; Detect wavelength 305nm, number of theoretical plate calculates by puerarin peak should be not less than 1000.Precision takes by weighing puerarin reference substance 5mg, puts in the 50ml measuring bottle, adds water and makes dissolving in right amount and be diluted to scale, shakes up, and promptly gets (containing puerarin 100 μ g among every 1ml), as reference substance solution.The content that other gets under these article content uniformity item is an amount of, and porphyrize takes by weighing about 1g, and accurate the title decides, and puts in the 50ml measuring bottle; Add methanol 30ml, supersound process 30 minutes adds methanol and is diluted to scale, shakes up, and filters; Discard filtrating just, precision is measured subsequent filtrate 25ml, puts evaporate to dryness in the water-bath, and residue adds water makes dissolving; Put in the 25ml measuring bottle, and be diluted to scale, shake up, as need testing solution.Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and these article puerarin content must not be less than 5.5mg/g.
Method 2: adopt HPLC coupling method to measure Determination of Hesperidin Content in these article; Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filler; Methanol-water-36% acetic acid (35: 61: 4) is mobile phase; Detect wavelength 300nm, number of theoretical plate calculates by puerarin peak should be not less than 2000.Precision takes by weighing Hesperidin reference substance 5mg, puts in the 50ml measuring bottle, adds methanol and makes dissolving in right amount and be diluted to scale, shakes up, and promptly gets (containing puerarin 100 μ g among every 1ml), as reference substance solution.The content that other gets under these article content uniformity item is an amount of, and porphyrize takes by weighing about 1g, and accurate the title decides, and puts in the 50ml measuring bottle; Add methanol 30ml, supersound process 30 minutes adds methanol and is diluted to scale, shakes up, and filters; Discard filtrating just, precision is measured subsequent filtrate 25ml, puts evaporate to dryness in the water-bath, and residue adds water makes dissolving; Put in the 25ml measuring bottle, and be diluted to scale, shake up, as need testing solution.Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and these article puerarin content must not be less than 3.5mg/g.
Compared with prior art, method of quality control provided by the invention can better be controlled a kind of product quality with ginseng Soviet Union Chinese medicine preparation of expelling wind and cold, expelling phlegm for arresting cough, guarantees the safety of medication.The present invention selects for use the Pericarpium Citri Reticulatae medical material as reference substance; Because Fructus Aurantii and Pericarpium Citri Reticulatae are equal plant; With containing Hesperidin; So existing standard selects for use Hesperidin not have specificity as reference substance, there is more advantage in the more existing Hesperidin thin layer of the present invention discrimination method: the unstability of not only avoiding the alkali plate; Simultaneously also avoid secondary unfolded loaded down with trivial details, this method can be used for the discriminating of Pericarpium Citri Reticulatae medical material or relevant Pericarpium Citri Reticulatae preparation.Radix Codonopsis also has and differentiates that specificity is strong in this invention once more; Owing to contain the equal Platycodon grandiflouorum of Radix Codonopsis in the 'Shensu '; Pharmacopeia is reference substance with the lobetyolin to the differentiating fluid of Radix Codonopsis; So the present invention has better specificity inspection as 'Shensu ', thereby more effective quality that guarantees product.Make the production technology of ginseng Soviet Union Chinese medicine preparation that guarantee arranged, the preparation that obtains is more reliable, has reached the purpose of invention.
Utilize method of quality control provided by the invention for proof and can better control the product quality of seed ginseng Soviet Union Chinese medicine preparation, the medicine that obtains has effective effect, and the applicant has carried out a series of experiments;
Test Example 1 content of hesperidin method for measuring is investigated
1.1 instrument condition: Tianjin, island high performance liquid chromatograph, LC-2010AHT.
1.2 reagent: methanol (chromatographically pure, analytical pure), acetonitrile (chromatographically pure), chloroform (analytical pure), water are high purity water; Hesperidin reference substance (Nat'l Pharmaceutical & Biological Products Control Institute provides, and supplies assay to use), sample ginseng Soviet Union capsule (pharmaceutical Co. Ltd of Guizhou letter nation, lot number: 20080101).
2.3 chromatographic condition: chromatographic column: enlightening agate ODS C18 post; Mobile phase: methanol-water-36% acetic acid (35: 61: 4); Flow velocity: 1.0ml/min; Column temperature: 30 ℃; Sample size: 10ul; Detect wavelength 3000nm.
1.3 system suitability test
Get the Hesperidin reference substance respectively; Ginseng Soviet Union capsule need testing solution lacks the negative blank solution injecting chromatograph of Pericarpium Citri Reticulatae, Fructus Aurantii medical material; In the chromatogram of record, see that the retention time of Hesperidin is 12 minutes, negative blank chromatogram is Wu Feng in the Hesperidin position; Other peak separating degrees complete (separating degree＞2.0) that Hesperidin is close with it, promptly Hesperidin separates with other components fully under this experiment condition.Theoretical cam curve in the Hesperidin peak more than 4000.
1.4 linear relationship is investigated
1.4.1 supply the preparation of examination solution
Get 10 of ginseng Soviet Union capsule capsules, inclining content, and mixing takes by weighing about 1g, and accurate the title decides; Put in the 50ml measuring bottle, add methanol 30ml, supersound process 30 minutes adds methanol and is diluted to scale, shakes up; Filter, discard filtrating just, precision is measured subsequent filtrate 25ml, puts evaporate to dryness in the water-bath, and residue adds water makes dissolving; Put in the 25ml measuring bottle, and be diluted to scale, shake up, as need testing solution
1.4.2 the preparation of standard solution
Precision takes by weighing Hesperidin reference substance 5mg, puts in the 50ml measuring bottle, adds methanol and makes dissolving in right amount and be diluted to scale, shakes up, and promptly gets (containing Hesperidin 100 μ g among every 1ml), as reference substance solution
1.4.3 the drafting of standard curve
The above-mentioned Hesperidin reference substance solution 2ul of accurate respectively absorption, 4ul, 8ul, 10ul 12ul, 16ul, 20ul injects liquid chromatograph, measures peak area.With the peak area is vertical coordinate, and sample size (ul) is an abscissa drawing standard curve, and regression equation is A=269158.5625C+13014.65, coefficient R=0.9999, and Hesperidin is good linear relationship in 0.4～4ug scope.
1.5 precision test
Get the capsular sample of ginseng Soviet Union and prepare need testing solution by the 1.4.1 method, draw 10ul, repeat sample introduction 6 times, Determination of Hesperidin Content is seen table six in the working sample, and RSD is 1.8%, and assay method precision is good.
The precision test that table one content of hesperidin is measured
1.6 stability test
Get ginseng Soviet Union's capsule 's content, prepare test liquid by the method for preparing of test liquid under the 1.4.1 item, respectively at 0h, 1h, 2h, 4h, 8h hour sample introduction 10ul, the RSD that measures peak area is that 2.2 explanation need testing solutions are good at the 8h internal stability.
1.7 replica test
Get ginseng Soviet Union capsule 's content, the same 1.4.1 of method for preparing, 5 parts of test liquids of parallel preparation, difference sample introduction 10 μ l, sample introduction is measured content.The average content of result of calculation Hesperidin is 0.30mg/g, and RSD is 1.3%, and assay method repeatability is good, and the result sees table two.
The replica test that table two content of hesperidin is measured
1.8 recovery test
Get the ginseng Soviet Union capsule 's content of known content, precision takes by weighing about 0.4g, 5 parts; Add reference substance solution 1.5mL respectively, press preparation need testing solution under the 1.4.1 item, draw need testing solution and Hesperidin reference substance solution 10ul respectively and inject chromatograph of liquid; The record peak area is 98.8% with the average recovery rate of external standard counter point calculation sample, and RSD is 0.7%; This law average recovery is good, and the result sees table three.
Hesperidin determination of recovery rates result in the table three ginseng Soviet Union capsule
1.9 sample determination
Prepare test liquid and contrast solution by preceding method, difference sample introduction 10 μ l, the record chromatogram is measured peak area, calculates content by external standard method, and content of hesperidin mensuration result sees table four in 10 lot sample article.
Content of hesperidin is measured the result in the table four 10 lot sample article
Test Example 2 Hesperidins are differentiated the specificity investigation
2.1 the preparation of standard solution
2.1.1 get Pericarpium Citri Reticulatae medical material 2g, decocte with water 1 hour filters, the filtrating evaporate to dryness adds methanol 5ml and makes dissolving, filters, and filtrating is as supplying examination solution.
Add methanol and process saturated solution 2.1.2 get the Hesperidin reference substance, as reference substance solution.
2.2 the preparation of negative sample
2.2.1 the preparation of Pericarpium Citri Reticulatae negative sample: the Folium Perillae, the Radix Aucklandiae, Rhizoma Zingiberis Recens of getting recipe quantity extract volatile oil, and medicinal liquid volatile oil is subsequent use, and medicinal residues add twice of other medical material water extraction of recipe quantity; Merge said extracted liquid, concentrate, receive cream; The system granule adds volatile oil, promptly gets.
2.2.2 the preparation of Pericarpium Citri Reticulatae, Fructus Aurantii jack to jack adapter property sample: Folium Perillae, the Radix Aucklandiae, the Rhizoma Zingiberis Recens of getting recipe quantity extract volatile oil, and medicinal liquid volatile oil is subsequent use, twice of medicinal residues adding other recipe quantity medical material water extraction except that Fructus Aurantii; Merge said extracted liquid, concentrate, receive cream; The system granule adds volatile oil, promptly gets.
2.3 these article content 2g is got in the preparation of test sample, adds methanol 25ml ultrasonic 15 minutes, filters, the filtrating evaporate to dryness adds methanol 2ml and makes dissolving, filters, and filtrating is as supplying examination solution.
2.4 differentiate and draw each 1 μ l of above-mentioned standard solution, test sample and negative sample solution, reference substance solution 5 μ l put respectively on same silica GF254 lamellae; With normal hexane-ethyl acetate-methanol-formic acid-ammonia (2: 3: 2: 0.04: 0.4) is developing solvent; Launch, take out, dry; Spray is put under ultra-violet lamp (365nm) and the wavelength 254nm and is inspected with the aluminum chloride test solution.
2.5 on test sample and control medicinal material and the corresponding position of reference substance chromatograph, show the fluorescence speckle of same color as a result; Simultaneously on test sample and the corresponding position of Pericarpium Citri Reticulatae list feminine gender chromatograph identical color fluorescence speckle is arranged also, but test sample there is not the fluorescence speckle of corresponding color on Pericarpium Citri Reticulatae, the corresponding position of Fructus Aurantii jack to jack adapter property chromatograph.Explain and select for use the Pericarpium Citri Reticulatae medical material to have specificity, avoid its equal medical material Fructus Aurantii for the interference of differentiating as reference substance.
Specific embodiment
Embodiment is used to join the method for quality control of Soviet Union's Chinese medicine preparation for 1 one kinds, mainly comprises projects such as discriminating, assay.
1, prescription: Folium Perillae 234g, Pericarpium Citri Reticulatae 156g, Radix Aucklandiae 156g, Rhizoma Zingiberis Recens 94g, Radix Codonopsis 234g, Poria 234g, Radix Puerariae 234g, Rhizoma Pinelliae (processed) 234g, Radix Peucedani 234g, Radix Glycyrrhizae 156g, Fructus Aurantii 156g, Radix Platycodonis 156g, Fructus Jujubae 94g
2, method for making: Folium Perillae, Pericarpium Citri Reticulatae, the Radix Aucklandiae, Rhizoma Zingiberis Recens four flavors are extracted volatile oil, and medicinal liquid is subsequent use, and medicinal residues add other medical materials of residue and drop in the multi-function extractor; The decocte with water secondary; The water that adds for the first time 12 times of amounts of medical material soaks into after 2 hours earlier, is heated to and boils, and decocts 2 hours; Filter filtrate for later use; Add for the second time the water of 10 times of amounts of medical material, be heated to and boil, decocted 1.5 hours, filter merging filtrate.Filter, filtrating merges with above-mentioned aqueous solution, 75～85 ℃ of temperature, vacuum-0.04～-the 0.075MPa condition under, filtrate decompression is condensed into thick paste, subsequent use.Above-mentioned thick paste is added appropriate amount of auxiliary materials, and mix homogeneously is granulated, and the drying cartridge capsule is processed 1000, promptly gets.
3, differentiate:
(1) get the content 5g of these article, water-wet is extracted 3 times with petroleum ether (60～90 ℃) jolting, and each 20ml merges petroleum ether, volatilizes, and residue adds petroleum ether (60～90 ℃) 1ml makes dissolving, as need testing solution.Other gets Radix Codonopsis control medicinal material 2g, and decocte with water 1 hour is concentrated into 25ml, puts coldly, extracts 3 times with petroleum ether (60～90 ℃) jolting, and each 20ml shines medical material solution in pairs with legal system.Draw above-mentioned need testing solution 15 μ l, control medicinal material solution 10 μ l put respectively on same silica gel g thin-layer plate, are developing solvent with petroleum ether (60～90 ℃)-ethyl acetate-formic acid (40: 10: 0.1); Launch, take out, dry; Spray is with 10% ethanol solution of sulfuric acid, and putting 105 ℃, to be heated to the speckle colour developing clear, puts 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 the fluorescence speckle of same color.
Get Pericarpium Citri Reticulatae control medicinal material 2g, decocte with water 1 hour filters, and the filtrating evaporate to dryness adds methanol 5ml and makes dissolving, filters, as control medicinal material solution.Other gets these article content 2g, adds methanol 25ml ultrasonic 15 minutes, filters, and the filtrating evaporate to dryness adds methanol 2ml and makes dissolving, filters, and filtrating is as need testing solution.Draw each 1 μ l of above-mentioned need testing solution and control medicinal material solution, reference substance solution 5 μ l put respectively on same silica GF254 lamellae; With normal hexane-ethyl acetate-methanol-formic acid-ammonia (2: 3: 2: 0.04: 0.4) is developing solvent, launches, and takes out; Dry, spray is put under ultra-violet lamp (365nm) and the wavelength 254nm and is inspected with the aluminum chloride test solution; In the test sample chromatograph, on test sample and control medicinal material and the corresponding position of reference substance chromatograph, show the fluorescence speckle of same color.
The content 10g of these article of getting, the 30ml that adds diethyl ether, supersound process 10 minutes filters, and filtrating volatilizes, and residue adds ethanol 0.5ml makes dissolving, as need testing solution.Other gets Radix Aucklandiae control medicinal material 0.2g, and the 5ml that adds diethyl ether shines medical material solution in pairs with legal system; Perhaps getting the constuslactone reference substance again adds methanol and processes saturated solution; Draw above-mentioned need testing solution 5～10 μ l, control medicinal material solution 2～4 μ l perhaps get reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate; With normal hexane-benzene-ethyl acetate (14: 3: 3) is developing solvent, launches, and takes out; Dry, spray is with 1% vanillin sulfuric acid solution, put 105 ℃ dry by the fire to speckle colour developing clear; In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the speckle of same color.
4. assay
(1) test of chromatographic condition and system suitability uses octadecylsilane chemically bonded silica to be filler, and methanol-water-36% acetic acid (20: 75: 5) is mobile phase, detects wavelength 305nm, and number of theoretical plate calculates by puerarin peak should be not less than 1000.
The preparation precision of reference substance solution takes by weighing puerarin reference substance 5mg, puts in the 50ml measuring bottle, adds water and makes dissolving in right amount and be diluted to scale, shakes up, and promptly gets (containing puerarin 100 μ g among every 1ml), as reference substance solution.
The content that the preparation of need testing solution is got under these article content uniformity item is an amount of, and porphyrize takes by weighing about 1g, and accurate the title decides, and puts in the 50ml measuring bottle; Add methanol 30ml, supersound process 30 minutes adds methanol and is diluted to scale, shakes up, and filters; Discard filtrating just, precision is measured subsequent filtrate 25ml, puts evaporate to dryness in the water-bath, and residue adds water makes dissolving; Put in the 25ml measuring bottle, and be diluted to scale, shake up, as need testing solution.Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure.
These article puerarin content must not be less than 5.5mg/g.
(2) test of chromatographic condition and system suitability uses octadecylsilane chemically bonded silica to be filler, and methanol-water-36% acetic acid (35: 61: 4) is mobile phase, detects wavelength 300nm, and number of theoretical plate calculates by puerarin peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing Hesperidin reference substance 5mg, puts in the 50ml measuring bottle, adds methanol and makes dissolving in right amount and be diluted to scale, shakes up, and promptly gets (containing puerarin 100 μ g among every 1ml), as reference substance solution.
The content that the preparation of need testing solution is got under these article content uniformity item is an amount of, and porphyrize takes by weighing about 1g, and accurate the title decides, and puts in the 50ml measuring bottle; Add methanol 30ml, supersound process 30 minutes adds methanol and is diluted to scale, shakes up, and filters; Discard filtrating just, precision is measured subsequent filtrate 25ml, puts evaporate to dryness in the water-bath, and residue adds water makes dissolving; Put in the 25ml measuring bottle, and be diluted to scale, shake up, as need testing solution.Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure.These article content of hesperidin must not be less than 2.0mg/g.
Claims (1)
1. the detection method of seed ginseng Soviet Union Chinese medicine preparation; It is characterized in that: described ginseng Soviet Union Chinese medicine preparation is by following method preparation: Folium Perillae 234g, Pericarpium Citri Reticulatae 156g, Radix Aucklandiae 156g, Rhizoma Zingiberis Recens 94g four flavors extract volatile oil, and medicinal liquid is subsequent use, in medicinal residues and Radix Codonopsis 234g, Poria 234g, Radix Puerariae 234g, Rhizoma Pinelliae Preparata 234g, Radix Peucedani 234g, Radix Glycyrrhizae 156g, Fructus Aurantii 156g, Radix Platycodonis 156g, the Fructus Jujubae 94g input multi-function extractor; The decocte with water secondary; The water that adds for the first time 12 times of amounts of medical material soaks into after 2 hours earlier, is heated to and boils, and decocts 2 hours; Filter filtrate for later use; Add for the second time the water of 10 times of amounts of medical material, be heated to and boil, decocted 1.5 hours, filter, merging filtrate filters, filtrating and above-mentioned combining medicine, 75～85 ℃ of temperature, vacuum-0.04～-the 0.075MPa condition under, filtrate decompression is condensed into thick paste, subsequent use; Above-mentioned thick paste is added appropriate amount of auxiliary materials, and mix homogeneously is granulated, and drying cartridge 1000 capsules promptly get,
The discriminating of Radix Codonopsis: get the content 5g of these article, water-wet is extracted 3 times with the petroleum ether jolting of 60～90 ℃ of boiling ranges, and each 20ml merges petroleum ether, volatilizes, and the petroleum ether 1ml that residue adds 60～90 ℃ of boiling ranges makes dissolving, as need testing solution; Other gets Radix Codonopsis control medicinal material 2g, and decocte with water 1 hour is concentrated into 25ml, puts coldly, extracts 3 times with the petroleum ether jolting of 60～90 ℃ of boiling ranges, and each 20ml shines medical material solution in pairs with legal system; Draw above-mentioned need testing solution 15 μ l, control medicinal material solution 10 μ l put respectively on same silica gel g thin-layer plate, with the petroleum ether-ethyl acetate-formic acid ratio of 60～90 ℃ of boiling ranges be 40: 10: 0.1 be developing solvent; Launch, take out, dry; Spray is with 10% ethanol solution of sulfuric acid, and putting 105 ℃, to be heated to the speckle colour developing clear, puts 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 the fluorescence speckle of same color;
The discriminating of Pericarpium Citri Reticulatae: get Pericarpium Citri Reticulatae control medicinal material 2g, decocte with water 1 hour filters, and the filtrating evaporate to dryness adds methanol 5ml and makes dissolving, filters, as control medicinal material solution; Other gets these article content 2g, adds methanol 25ml ultrasonic 15 minutes, filters, and the filtrating evaporate to dryness adds methanol 2ml and makes dissolving, filters, and filtrating is as need testing solution; Draw each 1 μ l of above-mentioned need testing solution and control medicinal material solution, put respectively on same silica GF254 lamellae, be 2: 3: 2 with normal hexane-ethyl acetate-methanol-formic acid-ammonia ratio: be developing solvent at 0.04: 0.4; Launch, take out, dry; Spray is put under ultra-violet lamp 365nm and the wavelength 254nm and is inspected, in the test sample chromatograph with the aluminum chloride test solution; On test sample and the corresponding position of control medicinal material chromatograph, show the fluorescence speckle of same color;
The discriminating of the Radix Aucklandiae: get the content 10g of these article, the 30ml that adds diethyl ether, supersound process 10 minutes filters, and filtrating volatilizes, and residue adds ethanol 0.5ml makes dissolving, as need testing solution; Other gets Radix Aucklandiae control medicinal material 0.2g, and the 5ml that adds diethyl ether shines medical material solution in pairs with legal system; Perhaps getting the constuslactone reference substance again adds methanol and processes saturated solution; Draw above-mentioned need testing solution 5～10 μ l, control medicinal material solution 2～4 μ l perhaps get reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate; With normal hexane-benzene-ethyl acetate ratio be 14: 3: 3 be developing solvent, launch, take out; Dry, spray is with 1% vanillin sulfuric acid solution, put 105 ℃ dry by the fire to speckle colour developing clear; In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the speckle of same color;
Content of puerarin is measured
Adopt content of puerarin in these article of high effective liquid chromatography for measuring; Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filler; Methanol-water-36% acetic acid ratio be 20: 75: 5 for mobile phase; Detect wavelength 305nm, number of theoretical plate calculates by puerarin peak should be not less than 1000; Precision takes by weighing puerarin reference substance 5mg, puts in the 50ml measuring bottle, adds water and makes dissolving in right amount and be diluted to scale, shakes up, and promptly gets to contain puerarin 100 μ g among every 1ml, as reference substance solution; The content that other gets under these article content uniformity item is an amount of, and porphyrize takes by weighing 1g, and accurate the title decides, and puts in the 50ml measuring bottle; Add methanol 30ml, supersound process 30 minutes adds methanol and is diluted to scale, shakes up, and filters; Discard filtrating just, precision is measured subsequent filtrate 25ml, puts evaporate to dryness in the water-bath, and residue adds water makes dissolving; Put in the 25ml measuring bottle, and be diluted to scale, shake up, as need testing solution; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and these article puerarin content must not be less than 5.5mg/g;
Determination of Hesperidin Content is measured
Adopt HPLC coupling method to measure Determination of Hesperidin Content in these article; Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filler; Methanol-water-36% acetic acid ratio be 35: 61: 4 for mobile phase; Detect wavelength 300nm, number of theoretical plate calculates by puerarin peak should be not less than 2000; Precision takes by weighing Hesperidin reference substance 5mg, puts in the 50ml measuring bottle, adds methanol and makes dissolving in right amount and be diluted to scale, shakes up, and promptly gets to contain Hesperidin 100 μ g among every 1ml, as reference substance solution; The content that other gets under these article content uniformity item is an amount of, and porphyrize takes by weighing 1g, and accurate the title decides, and puts in the 50ml measuring bottle; Add methanol 30ml, supersound process 30 minutes adds methanol and is diluted to scale, shakes up, and filters; Discard filtrating just, precision is measured subsequent filtrate 25ml, puts evaporate to dryness in the water-bath, and residue adds water makes dissolving; Put in the 25ml measuring bottle, and be diluted to scale, shake up, as need testing solution; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and these article content of hesperidin must not be less than 2.0mg/g.
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| CN102614378B (en) * | 2012-04-26 | 2014-01-15 | 陕西方舟制药有限公司 | Yin nourishing and blood sugar lowering Chinese medicinal composition and preparation method as well as detection method thereof |
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| 师永清.HPLC法测定参苏丸中橙皮苷的含量.《中国药房》.2007,第18卷(第18期),第1402-1403页. * |
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Address after: 550014 Luodian County, Qiannan Buyei and Miao Autonomous Prefecture, Jiefang Road Province Ping Town, No., No. 96 Patentee after: Xinbang Pharmacy Co., Ltd., Guizhou Address before: 227 No. 550014 Guizhou Guiyang Xinbang Baiyun Road Economic Development Zone Patentee before: Xinbang Pharmacy Co., Ltd., Guizhou |
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Granted publication date: 20120627 Termination date: 20201224 |