CN101474274A - Quality control method of Shensu Chinese medicine preparation - Google Patents
Quality control method of Shensu Chinese medicine preparation Download PDFInfo
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- CN101474274A CN101474274A CNA2008100690618A CN200810069061A CN101474274A CN 101474274 A CN101474274 A CN 101474274A CN A2008100690618 A CNA2008100690618 A CN A2008100690618A CN 200810069061 A CN200810069061 A CN 200810069061A CN 101474274 A CN101474274 A CN 101474274A
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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, guarantee the safety of medication, better instruct and produce, make technology controlling and process rationally strict more, make consumer's energy 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 as differentiating as differentiating item, adopted puerarin as differentiating and containing the survey index simultaneously, the discriminating of this method and contain survey and all adopt thin layer chromatography to carry out, tlc determination content poor reproducibility, measurement result is inaccurate, is not very reasonable 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 energy 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. make 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 this product, 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, decocts 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, with petroleum ether (60～90 ℃)-ethyl acetate-formic acid (40:10:0.1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, putting 105 ℃, to be heated to 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, decoct with water 1 hour, filter, the filtrate evaporate to dryness adds methanol 5ml and makes dissolving, filters, in contrast medical material solution.Other gets this product content 2g, adds methanol 25ml ultrasonic 15 minutes, filters, and the filtrate evaporate to dryness adds methanol 2ml and makes dissolving, filters, and filtrate 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 1 put respectively on same silica GF254 lamellae, are developing solvent with normal hexane-ethyl acetate-methanol-formic acid-ammonia (2:3:2:0.04:0.4), launch, take out, dry, spray is with the aluminum chloride test solution, put under ultra-violet lamp (365nm) and the wavelength 254nm 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 the Radix Aucklandiae: get the content 10g of this product, the 30ml that adds diethyl ether, supersound process 10 minutes filters, and filtrate 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 makes saturated solution; Draw above-mentioned need testing solution 5～10 μ l, control medicinal material solution 2～4 μ l or get reference substance solution 5 μ l put respectively on same silica gel g thin-layer plate, are developing solvent with normal hexane-benzene-ethyl acetate (14:3:3), 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.
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 high effective liquid chromatography for measuring this product, chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is 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), in contrast product solution.The content that other gets under this product content uniformity item is an amount of, and porphyrize takes by weighing about 1g, the accurate title, decide, and puts in the 50ml measuring bottle, adds methanol 30ml, supersound process 30 minutes adds methanol and is diluted to scale, shakes up, filter, discard filtrate just, precision is measured subsequent filtrate 25ml, put evaporate to dryness in the water-bath, residue adds water makes dissolving, puts 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 this product puerarin content must not be less than 5.5mg/g.
Method 2: adopt high performance liquid chromatography coupling method to measure Determination of Hesperidin Content in this product, chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is 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), in contrast product solution.The content that other gets under this product content uniformity item is an amount of, and porphyrize takes by weighing about 1g, the accurate title, decide, and puts in the 50ml measuring bottle, adds methanol 30ml, supersound process 30 minutes adds methanol and is diluted to scale, shakes up, filter, discard filtrate just, precision is measured subsequent filtrate 25ml, put evaporate to dryness in the water-bath, residue adds water makes dissolving, puts 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 this product 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 Pericarpium Citri Reticulatae medical material product in contrast for use, because Fructus Aurantii and Pericarpium Citri Reticulatae are equal plant, with containing Hesperidin, so existing standard select for use Hesperidin in contrast product do not have specificity, 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 ', thus the 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 uses for assay), sample ginseng Soviet Union capsule (pharmaceutical Co. Ltd of Guizhou letter nation, lot number: 20080101).
2.3 chromatographic condition: chromatographic column: enlightening agate 0DS 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, the retention time of Hesperidin is 12 minutes, negative blank chromatogram is at Hesperidin position Wu Feng, Hesperidin other peak separating degrees close with it are (separating degree〉2.0) fully, and 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 the preparation of test solution
Get 10 of ginseng Soviet Union capsule capsules, inclining content, and mixing takes by weighing about 1g, the accurate title, decide, and puts in the 50ml measuring bottle, adds methanol 30ml, supersound process 30 minutes adds methanol and is diluted to scale, shakes up, filter, discard filtrate just, precision is measured subsequent filtrate 25ml, put evaporate to dryness in the water-bath, residue adds water makes dissolving, puts 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), in contrast product 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 sees 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 preparation method 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 preparation method, 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, the results are shown in 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, the results are shown in 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, sample introduction 10 μ l write down chromatogram respectively, measure peak area, calculate content by external standard method, and the content of hesperidin measurement result sees Table four in 10 batch samples.
Content of hesperidin measurement result in table four 10 batch samples
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, decoct with water 1 hour, filter, the filtrate evaporate to dryness adds methanol 5ml and makes dissolving, filters, and filtrate is as test solution.
Add methanol and make saturated solution 2.1.2 get the Hesperidin reference substance, in contrast product 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 standby, 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.
2.2.2 the preparation of Pericarpium Citri Reticulatae, Fructus Aurantii jack to jack adapter sample: Folium Perillae, the Radix Aucklandiae, the Rhizoma Zingiberis Recens of getting recipe quantity extract volatile oil, medicinal liquid volatile oil is standby, 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, add volatile oil, promptly.
2.3 this product content 2g is got in the preparation of test sample, adds methanol 25ml ultrasonic 15 minutes, filters, the filtrate evaporate to dryness adds methanol 2ml and makes dissolving, filters, and filtrate is as test 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 one ethyl acetate one 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 chromatograph.Illustrate select for use the Pericarpium Citri Reticulatae medical material in contrast product have specificity, avoid its equal medical material Fructus Aurantii for the interference of differentiating.
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, medicinal liquid is standby, medicinal residues add other medical materials of residue and drop in the multi-function extractor, decoct 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, filtrate and the merging of above-mentioned aqueous solution, 75～85 ℃ of temperature, vacuum-0.04～-the 0.075MPa condition under, filtrate decompression is condensed into thick paste, standby.Above-mentioned thick paste is added appropriate amount of auxiliary materials, and mix homogeneously is granulated, and the drying cartridge capsule is made 1000, promptly.
3, differentiate:
(1) get the content 5g of this product, 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, decocts 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, with petroleum ether (60～90 ℃)-ethyl acetate-formic acid (40:10:0.1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, putting 105 ℃, to be heated to 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, decoct with water 1 hour, filter, the filtrate evaporate to dryness adds methanol 5ml and makes dissolving, filters, in contrast medical material solution.Other gets this product content 2g, adds methanol 25ml ultrasonic 15 minutes, filters, and the filtrate evaporate to dryness adds methanol 2ml and makes dissolving, filters, and filtrate 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, are developing solvent with normal hexane-ethyl acetate-methanol-formic acid-ammonia (2:3:2:0.04:0.4), launch, take out, dry, spray is with the aluminum chloride test solution, put under ultra-violet lamp (365nm) and the wavelength 254nm and inspect, 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.
Get the content 10g of this product, the 30ml that adds diethyl ether, supersound process 10 minutes filters, and filtrate 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 makes saturated solution; Draw above-mentioned need testing solution 5～10 μ l, control medicinal material solution 2～4 μ l or get reference substance solution 5 μ l put respectively on same silica gel g thin-layer plate, are developing solvent with normal hexane-benzene-ethyl acetate (14:3:3), 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.
4. assay
(1) test of chromatographic condition and system suitability is a filler with octadecylsilane chemically bonded silica, 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), in contrast product solution.
The content that the preparation of need testing solution is got under this product content uniformity item is an amount of, and porphyrize takes by weighing about 1g, the accurate title, decide, and puts in the 50ml measuring bottle, adds methanol 30ml, supersound process 30 minutes adds methanol and is diluted to scale, shakes up, filter, discard filtrate just, precision is measured subsequent filtrate 25ml, put evaporate to dryness in the water-bath, residue adds water makes dissolving, puts 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.
This product puerarin content must not be less than 5.5mg/g.
(2) test of chromatographic condition and system suitability is a filler with octadecylsilane chemically bonded silica, 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), in contrast product solution.
The content that the preparation of need testing solution is got under this product content uniformity item is an amount of, and porphyrize takes by weighing about 1g, the accurate title, decide, and puts in the 50ml measuring bottle, adds methanol 30ml, supersound process 30 minutes adds methanol and is diluted to scale, shakes up, filter, discard filtrate just, precision is measured subsequent filtrate 25ml, put evaporate to dryness in the water-bath, residue adds water makes dissolving, puts 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.
This product content of hesperidin must not be less than 2.0mg/g.
Claims (4)
1, a kind of method of quality control that is used to join Soviet Union's Chinese medicine preparation, mainly comprise projects such as discriminating, assay, it is characterized in that: it is with the detection index of all or part of kind in lobetyolin, glucose, Platycodin D, puerarin, naringin, Hesperidin, praeruptorin A, Praeruptorin B, constuslactone, enoxolone, Radix Codonopsis control medicinal material, Radix Puerariae medical material, Pericarpium Citri Reticulatae control medicinal material, the Radix Aucklandiae control medicinal material as the quality control of this Chinese medicine preparation.
2, according to the described a kind of method of quality control that is used to join Soviet Union's Chinese medicine preparation of claim 1, it is characterized in that: 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 as the discrimination method of this Chinese medicine preparation, the detection index of content assaying method.
3, according to claim 1 or 2 described a kind of method of quality control that are used to join Soviet Union's Chinese medicine preparation, it is characterized in that: adopt in the following method all or part of as the method for differentiating:
Discriminating for Radix Codonopsis: get the content 5g of this product, 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, decocts 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, with petroleum ether (60～90 ℃)-ethyl acetate-formic acid (40:10:0.1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, putting 105 ℃, to be heated to 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, decoct with water 1 hour, filter, the filtrate evaporate to dryness adds methanol 5ml and makes dissolving, filters, in contrast medical material solution.Other gets this product content 2g, adds methanol 25ml ultrasonic 15 minutes, filters, and the filtrate evaporate to dryness adds methanol 2ml and makes dissolving, filters, and filtrate 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, are developing solvent with normal hexane-ethyl acetate-methanol-formic acid-ammonia (2:3:2:0.04:0.4), launch, take out, dry, spray is with the aluminum chloride test solution, put under ultra-violet lamp (365nm) and the wavelength 254nm and inspect, 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.
Discriminating for the Radix Aucklandiae: get the content 10g of this product, the 30ml that adds diethyl ether, supersound process 10 minutes filters, and filtrate 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 makes saturated solution; Draw above-mentioned need testing solution 5～10 μ l, control medicinal material solution 2～4 μ l or get reference substance solution 5 μ l put respectively on same silica gel g thin-layer plate, are developing solvent with normal hexane-benzene-ethyl acetate (14:3:3), 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.
4, according to claim 1 or 2 described a kind of method of quality control that are used to join Soviet Union's Chinese medicine preparation, it is characterized in that: adopt all or part of method in the following method as assay:
Method 1: adopt content of puerarin in high effective liquid chromatography for measuring this product, chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is 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), in contrast product solution.The content that other gets under this product content uniformity item is an amount of, and porphyrize takes by weighing about 1g, the accurate title, decide, and puts in the 50ml measuring bottle, adds methanol 30ml, supersound process 30 minutes adds methanol and is diluted to scale, shakes up, filter, discard filtrate just, precision is measured subsequent filtrate 25ml, put evaporate to dryness in the water-bath, residue adds water makes dissolving, puts 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.
Method 2: adopt high performance liquid chromatography coupling method to measure Determination of Hesperidin Content in this product, chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is 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), in contrast product solution.The content that other gets under this product content uniformity item is an amount of, and porphyrize takes by weighing about 1g, the accurate title, decide, and puts in the 50ml measuring bottle, adds methanol 30ml, supersound process 30 minutes adds methanol and is diluted to scale, shakes up, filter, discard filtrate just, precision is measured subsequent filtrate 25ml, put evaporate to dryness in the water-bath, residue adds water makes dissolving, puts 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.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102614378A (en) * | 2012-04-26 | 2012-08-01 | 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 |
| CN106645438A (en) * | 2015-10-30 | 2017-05-10 | 湖南康寿制药有限公司 | Detection method of radix ginseng and folium perillae preparation |
| CN106645534A (en) * | 2015-10-30 | 2017-05-10 | 湖南康寿制药有限公司 | A fingerprint detecting method for a Shensu preparation |
| KR101814999B1 (en) | 2012-01-13 | 2018-01-08 | 주식회사 엘지생활건강 | Composition for improving skin wrinkle and enhancing elasticity |
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2008
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101814999B1 (en) | 2012-01-13 | 2018-01-08 | 주식회사 엘지생활건강 | Composition for improving skin wrinkle and enhancing elasticity |
| CN102614378A (en) * | 2012-04-26 | 2012-08-01 | 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 |
| 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 |
| CN106645438A (en) * | 2015-10-30 | 2017-05-10 | 湖南康寿制药有限公司 | Detection method of radix ginseng and folium perillae preparation |
| CN106645534A (en) * | 2015-10-30 | 2017-05-10 | 湖南康寿制药有限公司 | A fingerprint detecting method for a Shensu preparation |
| CN106645534B (en) * | 2015-10-30 | 2018-07-31 | 湖南康寿制药有限公司 | A kind of detection method of 'Shensu ' finger-print |
| CN106645438B (en) * | 2015-10-30 | 2019-08-16 | 湖南康寿制药有限公司 | A kind of detection method of 'Shensu ' |
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