CN102068549A - Quality control method for Chinese medicinal preparation heat clearing and blood cooling pills - Google Patents
Quality control method for Chinese medicinal preparation heat clearing and blood cooling pills Download PDFInfo
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Abstract
The invention belongs to the technical field of Chinese patent medicaments, and relates to a quality control method for a Chinese medicinal preparation, namely heat clearing and blood cooling pills prepared from Chinese medicinal materials. The heat clearing and blood cooling pills consist of Chinese medicinal materials, namely scutellaria root and Rehmannia glutinosa. The quality control method comprises the following steps of: taking baicalin and catalpol as reference products, and identifying whether scutellaria root and Rehmannia glutinosa components are contained in the prescription of the heat clearing and blood cooling pills by thin-layer chromatography; and detecting the content of the baicalin in the prescription of the heat clearing and blood cooling pills by high performance liquid chromatography. A quantitative index and an inspection method thereof make the quality standard more perfect. The revised quality standard improves the quality control of medicaments.
Description
Technical field
The invention belongs to the technical field of Chinese patent medicine, relating to the Chinese crude drug is the method for quality control of the Chinese medicine preparation clearing away heat and cooling blood ball made of raw material.
Background technology
The clearing away heat and cooling blood ball is the 9th the 192 page of preparation that records of " the Sanitation Ministry medicine standard " Chinese traditional patent formulation preparation, Ministry of Public Health standard WS3-B-1843-94 record prescription and quality standard:
Prescription: Radix Scutellariae 500g Radix Rehmanniae 500g
Method for making: above two flavors, be ground into fine powder, sieve, mixing, the water pill, drying, promptly.
Differentiate: get this product 1g, grind, add methanol 20ml, reflux 2 hours is put coldly, filters, and filtrate is as need testing solution.Other gets the baicalin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (57 pages of appendix), draw each 10 μ l of need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water (10: 7: 2: 2) be developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
But there are the following problems for above-mentioned standard: after discrimination method point sample lamellae launches to dry, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, the bronzing speckle is arranged, no fluorescence speckle discriminating means existing problems; The assay item that does not reflect the index components of medicine inherent quality in addition for quality control standard, still is short of to some extent, for improving the product quality of Chinese medicine, need improve target level of product quality.
Summary of the invention
The objective of the invention is to the objective of the invention is to overcome the clearing away heat and cooling blood ball standard weak point of prior art, a kind of method of quality control of clearing away heat and cooling blood ball that can the qualitative and quantitative analysis ingredient is provided.
For the technical scheme that reaches purpose employing of the present invention is: a kind of method of quality control of Chinese medicine preparation clearing away heat and cooling blood ball, wherein said pharmaceutical formulation is by Chinese crude drug: Radix Scutellariae 500g Radix Rehmanniae 500g forms, more than two the flavor, be ground into fine powder, sieve, mixing, the water pill, drying promptly, is characterized in that: the step of its method is:
(1) be reference substance with baicalin, catalpol, thin layer chromatography differentiates in the clearing away heat and cooling blood ball prescription whether contain Radix Scutellariae, Radix Rehmanniae composition;
(2) with the baicalin be reference substance, high performance liquid chromatography detects content of baicalin in the clearing away heat and cooling blood ball prescription.
The method of quality control of described Chinese medicine preparation clearing away heat and cooling blood ball is characterized in that: described thin layer chromatography differentiates that the method that does not contain Radix Scutellariae in the clearing away heat and cooling blood ball prescription is: get this product 1g, grind, add methanol 20ml, reflux 2 hours is put cold, filter, filtrate is as need testing solution; Other gets the baicalin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to the thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with ethyl acetate-butanone-formic acid-water, ethyl acetate; Butanone: formic acid: water=10: 7: 2: 2, launch, take out, to dry, spray is with 1% ferric chloride alcoholic solution, and 105 ℃ to be heated to the speckle colour developing clear; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Described thin layer chromatography differentiates that the method that whether contains the Radix Rehmanniae composition in the clearing away heat and cooling blood ball prescription is: get this product powder 2g, add methanol 20ml, reflux 1 hour is put coldly, filters, the filtrate evaporate to dryness, residue adds ethyl acetate 20ml supersound process 30 minutes, filters the filtrate evaporate to dryness, residue adds methanol 5ml, as need testing solution; Other gets the catalpol reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same high-efficient silica gel G lamellae, be developing solvent with chloroform-methanol-water, chloroform: methanol: water=14: 6: 1, launch, take out, dry, spray is with the anisaldehyde test solution, and 105 ℃ to be heated to speckle colour developing clear; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
The method of quality control of described Chinese medicine preparation clearing away heat and cooling blood ball is characterized in that: be reference substance with the baicalin, the method that liquid chromatography detects content of baicalin in the clearing away heat and cooling blood ball prescription is:
(1) chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Methanol: water: phosphoric acid=47: 53: 0.2 is mobile phase; The detection wavelength is 280nm; Number of theoretical plate calculates by the baicalin peak should be not less than 2000;
(2) preparation of reference substance solution: it is an amount of to get the baicalin reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 0.1mg, promptly;
(3) preparation of need testing solution: sample thief 2g, porphyrize is got powder 0.2g, the accurate title, decide, and puts in the tool plug conical flask, and precision is measured 70% ethanol 100ml, claim to decide weight, reflux 30 minutes is put cold, claim to decide weight, supply the weight that subtracts mistake with 70% ethanol, shake up, filter, get subsequent filtrate, promptly;
(4) algoscopy: inaccurate reference substance solution and each 5 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly; The every gram of this product contains baicalin must not be less than 24mg.
Being provided with baicalin, catalpol in the clearing away heat and cooling blood ball quality standard of the present invention is reference substance, and thin layer chromatography differentiates in the clearing away heat and cooling blood ball prescription whether contain Radix Scutellariae, Radix Rehmanniae composition; High performance liquid chromatography detects content of baicalin in the clearing away heat and cooling blood ball prescription, the every gram of this product contains the quantitative target and the method for inspection that baicalin must not be less than 24mg, make quality standard comparatively perfect, the quality of strict control medicine, guarantee to improve the quality of products, revised quality standard has improved the quality control of medicine.
Advantage of the present invention and good effect are:
1. thin layer chromatography differentiates that the employing spray is with 1% ferric chloride alcoholic solution in the baicalin colour developing in this method of quality control, it is clear to be heated to speckle colour developing at 105 ℃, increase the thin layer speckle greatly and detect effect, be convenient to observe and differentiate, ensured the accuracy of identification result.
2. increase thin layer chromatography in this method of quality control and differentiated Radix Rehmanniae active component catalpol step, can check out counterfeit drug and substandard drug more exactly, improved the safety in using.
3. increase high-efficient liquid phase technique in this method of quality control and measured the content of baicalin step, improved the controllability of clearing away heat and cooling blood ball quality standard, further guarantee product inherent quality and curative effect, and to promoting production marketing, increase the competitiveness of product in market, guaranteeing that patient's drug safety is significant
4. method of quality control of the present invention is simple, easy to operate, has eliminated the uncertainty that original baicalin is differentiated, is a kind of revised quality standard of discrimination method that can differentiate Chinese medicine preparation clearing away heat and cooling blood ball more comprehensively, accurately, has improved the quality control of medicine.
Description of drawings
Fig. 1 is that the thin layer of including in the former ministry standard of clearing away heat and cooling blood ball is differentiated the figure that inspects under the ultra-violet lamp of Radix Scutellariae.
Fig. 2 is the thin-layer chromatogram of the discriminating Radix Scutellariae of clearing away heat and cooling blood ball of the present invention.
Fig. 3 is the thin-layer chromatogram of the discriminating Radix Rehmanniae of clearing away heat and cooling blood ball of the present invention.
Fig. 4 is the liquid chromatogram for test agent solution of clearing away heat and cooling blood ball of the present invention.
Fig. 5 is the liquid chromatogram of the baicalin standard solution of clearing away heat and cooling blood ball of the present invention.
Fig. 6 is the liquid chromatogram of the blank product solution of clearing away heat and cooling blood ball of the present invention.
Fig. 7 is the linear curve chart of investigating of the assay of clearing away heat and cooling blood ball of the present invention.
The specific embodiment
The present invention has increased the thin layer discriminating of Radix Rehmanniae and the assay of Radix Scutellariae to Chinese medicine preparation clearing away heat and cooling blood ball method of quality control; Simultaneously, to Radix Scutellariae discrimination method in the primary standard, revise again, below in conjunction with embodiment, the present invention is further described, the clearing away heat and cooling blood ball quality after embodiment 1 improves
Standard: prescription: Radix Scutellariae 500g Radix Rehmanniae 500g
Method for making: above two flavors, be ground into fine powder, sieve, mixing, the water pill, drying, promptly.
Character: this product is the yellowish-brown watered pill to pitchy; Sweet in the mouth, hardship.
Differentiate: (1) gets this product 1g, grinds, and adds methanol 20ml, and reflux 2 hours is put coldly, filters, and filtrate is as need testing solution.Other gets the baicalin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water (10: 7: 2: 2) be developing solvent, launch, take out, dry, spray is with 1% ferric chloride alcoholic solution, and 105 ℃ to be heated to the speckle colour developing clear.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(2) get this product powder 2g, add methanol 20ml, reflux 1 hour is put coldly, filters, and filtrate evaporate to dryness, residue add ethyl acetate 20ml supersound process 30 minutes, filter, and filtrate evaporate to dryness, residue add methanol 5ml, as need testing solution.Other gets the catalpol reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same high-efficient silica gel G lamellae, with chloroform-methanol-water (14: 6: 1) is developing solvent, launch, take out, dry, spray is with the anisaldehyde test solution, and 105 ℃ to be heated to the speckle colour developing clear.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Check: should meet every regulation relevant under the pill item (" appendix IA of Chinese pharmacopoeia version in 2005).
Assay: the photograph high performance liquid chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 D) measure.
Chromatographic condition and system suitability test octadecylsilane chemically bonded silica are filler; Methanol-water-phosphoric acid (47: 53: 0.2) is a mobile phase; The detection wavelength is 280nm.Number of theoretical plate calculates by the baicalin peak should be not less than 2000.
It is an amount of that the baicalin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 0.1mg, promptly.
The preparation sample thief 2g of need testing solution, porphyrize is got powder 0.2g, and accurate the title, decide, and puts in the tool plug conical flask, precision is measured 70% ethanol 100ml, claims decide weight, and reflux 30 minutes is put coldly, and weight decided in title, supply the weight that subtracts mistake with 70% ethanol, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each the 5 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
The every gram of this product contains baicalin must not be less than 24mg.
Function with cure mainly: YIN nourishing, heat clearing away, removing heat from blood.Be used for anemia of pregnant woman's part of the body cavity above the diaphragm housing the heart and lungs fire and contain, have a dizzy spell, aphtha of the mouth and tongue, tinnitus toothache, anemia of pregnant woman's heat in blood restlessness during pregnancy.
Usage and consumption: oral, a 6g, 1～2 time on the one.
Attention: the restlessness during pregnancy person of the phlegm-damp stagnation of QI avoids clothes.Specification: every bottled 6g storage: airtight, protection against the tide.
There is Radix Scutellariae to differentiate in the clearing away heat and cooling blood ball proper mass standard, no assay item, this time the raising standard has increased the thin layer discriminating of Radix Rehmanniae and the assay of Radix Scutellariae; Simultaneously, to Radix Scutellariae discrimination method in the primary standard, revise again.
1. the discriminating of Radix Scutellariae
1.1 material and reagent
Methanol, ethyl acetate, butanone, formic acid: analytical pure
Baicalin reference substance: Nat'l Pharmaceutical ﹠ Biological Products Control Institute, lot number: 110715-200514
Clearing away heat and cooling blood ball sample: Lerentang Pharmaceutical Factory, Zhongxin Pharmaceutical Group Co., Ltd., Tianj produces;
Lot number: D081001
Silica gel G plate: Qingdao Haiyang chemical industry subsidiary factory
1.2 the preparation of need testing solution
Get this product 1.0g, add methanol 20ml, reflux 2 hours is put coldly, filters, and filtrate is as need testing solution.
1.3 the preparation of reference substance solution
Get the baicalin reference substance, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution.
1.4 the preparation of blank product solution
By prescription, technology, except that Radix Scutellariae, prepare the blank product, again the blank product are ground into fine powder, prepare blank product solution according to the need testing solution preparation method.
1.5 experimental technique
Method 1: with reference to the Radix Scutellariae thin layer discrimination method of including in the former ministry standard of clearing away heat and cooling blood ball.
Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 10 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water (10: 7: 2: 2) be developing solvent, launch, take out, dry, put under the ultra-violet lamp (254nm) and inspect.
The result: in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, no fluorescence speckle has the bronzing speckle.The results are shown in Figure 1.Among Fig. 11: test sample 2: reference substance 3: blank product
The Radix Scutellariae thin layer discrimination method of including in the former ministry standard of clearing away heat and cooling blood ball is made amendment, changes coloration method:
Method 2: according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, draw each 10 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water (10: 7: 2: 2) be developing solvent, launch, take out, dry, spray is with 1% ferric chloride alcoholic solution, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color, blank product chromatograph is noiseless.The results are shown in Figure 2.
Among Fig. 21: test sample 2: reference substance 3: blank product
1.6 determine Radix Scutellariae thin layer discrimination method be:
Get this product 1g, grind, add methanol 20ml, reflux 2 hours is put coldly, filters, and filtrate is as need testing solution.Other gets the baicalin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water (10: 7: 2: 2) be developing solvent, launch, take out, dry, spray is with 1% ferric chloride alcoholic solution, and 105 ℃ to be heated to the speckle colour developing clear.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
2. the discriminating of Radix Rehmanniae
2.1 material and reagent
Methanol, ethyl acetate, chloroform: analytical pure
Catalpol reference substance: Nat'l Pharmaceutical ﹠ Biological Products Control Institute, lot number: 110808-200407
Clearing away heat and cooling blood ball sample: Lerentang Pharmaceutical Factory, Zhongxin Pharmaceutical Group Co., Ltd., Tianj produces;
Lot number: D081001
High-efficient silica gel G plate:
2.2 the preparation of need testing solution
Get this product powder 2g, add methanol 20ml, reflux 1 hour is put coldly, filters, and filtrate evaporate to dryness, residue add ethyl acetate 20ml supersound process 30 minutes, filter, and filtrate evaporate to dryness, residue add methanol 5ml, as need testing solution.
2.3 the preparation of reference substance solution
Get the catalpol reference substance, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution.
2.4 the preparation of blank product solution
By prescription, technology, except that Radix Rehmanniae, prepare the blank product, again the blank product are ground into fine powder, prepare blank product solution according to the need testing solution preparation method.
2.5 experimental technique
Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same high-efficient silica gel G lamellae, with chloroform-methanol-water (14: 6: 1) is developing solvent, launch, take out, dry, spray is with the anisaldehyde test solution, and 105 ℃ to be heated to the speckle colour developing clear.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.The blank product are noiseless.The results are shown in Figure 3.Among Fig. 31: test sample 2: reference substance 3: blank product.
2.6 determine the Radix Rehmanniae discrimination method be: get this product powder 2g, add methanol 20ml, reflux 1 hour is put coldly, filters, and filtrate evaporate to dryness, residue added the ethyl acetate supersound process 30 minutes, filtered, and filtrate evaporate to dryness, residue add methanol 5ml, as need testing solution.Other gets the catalpol reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same high-efficient silica gel G lamellae, with chloroform-methanol-water (14: 6: 1) is developing solvent, launch, take out, dry, spray is with the anisaldehyde test solution, and 105 ℃ to be heated to the speckle colour developing clear.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Two. content of baicalin is measured
1. instrument and material
Instrument: Waters 2695 high performance liquid chromatographs; Detector: Waters2487; Sartorius CP224S. electronic balance.
Material: chromatographic column: Diamonsil C18,5 μ, 250 * 4.6mm; Baicalin reference substance: lot number: 110715-200514 is produced by Chinese pharmaceutical biological product check; Methanol: chromatographically pure, Tianjin Concord Technology Co., Ltd. produces; Glacial acetic acid, phosphoric acid: analytical pure;
Clearing away heat and cooling blood ball sample: Lerentang Pharmaceutical Factory, Zhongxin Pharmaceutical Group Co., Ltd., Tianj produces;
Lot number: D081001
2. experimental technique
2.1 the preparation of reference substance solution: it is an amount of to get the baicalin reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 0.1mg, promptly.See Fig. 4
2.2 the selection of mobile phase: with reference to " mobile phase in radix scutellariae medicinal materials content assaying method of Chinese pharmacopoeia version in 2005: methanol-water-phosphoric acid (50: 50: 0.2).
Chromatographic condition: 30 ℃ of column temperatures, detect wavelength: 280nm, flow velocity: 0.8ml/min
2.3 the selection of extracting method
The result: employing method 2 baicalins extract fully, determine that employing method 2 is need testing solution extraction solvent.
2.4 the selection of extraction time
With this product porphyrize, it is fixed to get the accurate title of fine powder 0.2g, puts in the tool plug Erlenmeyer flask, and precision is measured 70% ethanol 100ml, weighs, and the time that heating and refluxing extraction is different, it is heavy to put cold-patch, filters, and injects high performance liquid chromatograph and measures.Result such as table 2
The result: employing method 1 baicalin extracts fully, determines that employing method 1 is need testing solution extraction time.
The selection of table 1 extracting method
The selection of table 2 extraction time
2.5 determine the need testing solution preparation method
Sample thief 2g, porphyrize is got powder 0.2g, accurate claims surely, puts in the tool plug conical flask, and precision is measured 70% ethanol 100ml, claims decide weight, and reflux 30 minutes is put coldly, claims to decide weight, supplies the weight that subtracts mistake with 70% ethanol, shakes up, and filtration is got subsequent filtrate, promptly.See Fig. 5
3. blank product formulations prepared from solutions
Except that Radix Scutellariae, prepare the blank product, prepare blank product solution by the need testing solution preparation method by formulation and technology.See Fig. 6
4. methodology checking
4.1 linear the investigation
Get baicalin reference substance solution (concentration 340.8 μ g/ml) and be diluted to the reference substance solution that concentration is 34.08 μ g/ml, 68.16 μ g/ml, 136.32 μ g/ml, 204.48 μ g/ml, 272.64 μ g/ml, 340.8 μ g/ml respectively, draw 5 μ l respectively and inject high performance liquid chromatograph, the record chromatogram is done linear regression with peak area to content.Result such as table 3.
Table 3 is linear to be investigated
Getting regression equation by data is: y=A+Bx=19255.25x-55946.54, r=0.9999
The result shows that baicalin is good in 0.1704～1.704 μ g scope internal linear relation.
4.2 precision is got same need testing solution, continuous sample introduction 6 times is measured relative standard deviation RSD=0.3%, shows that precision is good.Result such as table 4
4.3 repeatability
The fixed 6 parts of same batch sample powder of accurate title, according to the preparation method preparation of need testing solution, the RSD that measures content of baicalin is 0.7%, shows that repeatability is good.Result such as table 5.
The experiment of table 4 precision
The experiment of table 5 repeatability
4.4 stability experiment
Get same need testing solution, test for 1 time every 2 hours sample introductions, continuous sample introduction 6 times, RSD=0.2% shows that this product is basicly stable in 10h.Result such as table 6.
Table 6 stability experiment
4.5 response rate experiment
Get with a collection of known content (content: 6 parts in sample 58.7mg/g), every part of 0.1g accurate claims surely, adds the baicalin reference substance respectively, according to the preparation method preparation of need testing solution, calculating average recovery rate is 95.78%, RSD=0.7% again.The show sample response rate is good as a result.Result such as table 7.
The experiment of table 7 response rate
5.6 sample size is measured
Get five batch samples, be prepared according to the need testing solution preparation method respectively, measure content of baicalin, the results are shown in Table 8.
Table 8 five batch sample assay results
30.2×80％＝24mg/g
According to above five batches testing result, determine that content of baicalin must not be lower than 24mg/g in the clearing away heat and cooling blood ball.
Claims (3)
1. the method for quality control of a Chinese medicine preparation clearing away heat and cooling blood ball, wherein said pharmaceutical formulation are by Chinese crude drug: Radix Scutellariae 500g Radix Rehmanniae 500g forms, more than two flavors, be ground into fine powder, sieve mixing, water pill, drying promptly, is characterized in that: the step of its method is:
(1) be reference substance with baicalin, catalpol, thin layer chromatography differentiates in the clearing away heat and cooling blood ball prescription whether contain Radix Scutellariae, Radix Rehmanniae composition;
(2) with the baicalin be reference substance, high performance liquid chromatography detects content of baicalin in the clearing away heat and cooling blood ball prescription.
2. the method for quality control of Chinese medicine preparation clearing away heat and cooling blood ball according to claim 1, it is characterized in that: described thin layer chromatography differentiates that the method that does not contain Radix Scutellariae in the clearing away heat and cooling blood ball prescription is: get this product 1g, grind, add methanol 20ml, reflux 2 hours, put coldly, filter, filtrate is as need testing solution; Other gets the baicalin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water is developing solvent, ethyl acetate: butanone: formic acid: water=10: 7: 2: 2, launch, take out, dry, spray is with 1% ferric chloride alcoholic solution, and 105 ℃ to be heated to speckle colour developing clear; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Described thin layer chromatography differentiates that the method that whether contains the Radix Rehmanniae composition in the clearing away heat and cooling blood ball prescription is: get this product powder 2g, add methanol 20ml, reflux 1 hour is put coldly, filters, the filtrate evaporate to dryness, residue adds ethyl acetate 20ml supersound process 30 minutes, filters the filtrate evaporate to dryness, residue adds methanol 5ml, as need testing solution; Other gets the catalpol reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same high-efficient silica gel G lamellae, be developing solvent with chloroform-methanol-water, chloroform: methanol: water=14: 6: 1, launch, take out, dry, spray is with the anisaldehyde test solution, and 105 ℃ to be heated to speckle colour developing clear; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
3. the method for quality control of Chinese medicine preparation clearing away heat and cooling blood ball according to claim 1 is characterized in that: be reference substance with the baicalin, the method that liquid chromatography detects content of baicalin in the clearing away heat and cooling blood ball prescription is:
(1) chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Methanol: water: phosphoric acid=47: 53: 0.2 is mobile phase; The detection wavelength is 280nm; Number of theoretical plate calculates by the baicalin peak should be not less than 2000;
(2) preparation of reference substance solution: it is an amount of to get the baicalin reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 0.1mg, promptly;
(3) preparation of need testing solution: sample thief 2g, porphyrize is got powder 0.2g, the accurate title, decide, and puts in the tool plug conical flask, and precision is measured 70% ethanol 100ml, claim to decide weight, reflux 30 minutes is put cold, claim to decide weight, supply the weight that subtracts mistake with 70% ethanol, shake up, filter, get subsequent filtrate, promptly;
(4) algoscopy: inaccurate reference substance solution and each 5 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly; The every gram of this product contains baicalin must not be less than 24mg.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102526356A (en) * | 2012-03-14 | 2012-07-04 | 青岛汉河动植物药业有限公司 | Traditional Chinese medicine compound for clearing Ying heat and cooling blood of poultry |
| CN103070971A (en) * | 2013-02-28 | 2013-05-01 | 吕忠绪 | Traditional Chinese medicament composition for treating hemodia, odontoseisis and toothache |
| CN110646521A (en) * | 2018-06-26 | 2020-01-03 | 北京紫云腾中药饮片有限公司 | Detection method of prepared rehmannia root decoction pieces |
| CN115166128A (en) * | 2022-06-22 | 2022-10-11 | 四川逢春制药有限公司 | Method for identifying Scutellaria Yunnanensis and Scutellaria baicalensis |
| CN115420816A (en) * | 2022-07-21 | 2022-12-02 | 广东万年青制药股份有限公司 | Content determination method of traditional Chinese medicine composition for nourishing yin and cooling blood |
-
2009
- 2009-11-19 CN CN200910228359A patent/CN102068549B/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102526356A (en) * | 2012-03-14 | 2012-07-04 | 青岛汉河动植物药业有限公司 | Traditional Chinese medicine compound for clearing Ying heat and cooling blood of poultry |
| CN102526356B (en) * | 2012-03-14 | 2013-11-27 | 青岛汉河动植物药业有限公司 | Traditional Chinese medicine compound for clearing Ying heat and cooling blood of poultry |
| CN103070971A (en) * | 2013-02-28 | 2013-05-01 | 吕忠绪 | Traditional Chinese medicament composition for treating hemodia, odontoseisis and toothache |
| CN110646521A (en) * | 2018-06-26 | 2020-01-03 | 北京紫云腾中药饮片有限公司 | Detection method of prepared rehmannia root decoction pieces |
| CN115166128A (en) * | 2022-06-22 | 2022-10-11 | 四川逢春制药有限公司 | Method for identifying Scutellaria Yunnanensis and Scutellaria baicalensis |
| CN115420816A (en) * | 2022-07-21 | 2022-12-02 | 广东万年青制药股份有限公司 | Content determination method of traditional Chinese medicine composition for nourishing yin and cooling blood |
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| Publication number | Publication date |
|---|---|
| CN102068549B (en) | 2012-09-05 |
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Address after: 300380 Yumen Road, Xiqing District, Tianjin Patentee after: Lerentang Pharmaceutical Factory of Jinyao Darentang Group Co.,Ltd. Address before: 300380 Yumen Road, Xiqing District, Tianjin Patentee before: Letrentang pharmaceutical factory of Tianjin Zhongxin Pharmaceutical Group Co.,Ltd. |