CN101352558A - Quality control method of granular formulation for treating gastricism without aversion to cold - Google Patents
Quality control method of granular formulation for treating gastricism without aversion to cold Download PDFInfo
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- CN101352558A CN101352558A CNA2008100553409A CN200810055340A CN101352558A CN 101352558 A CN101352558 A CN 101352558A CN A2008100553409 A CNA2008100553409 A CN A2008100553409A CN 200810055340 A CN200810055340 A CN 200810055340A CN 101352558 A CN101352558 A CN 101352558A
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Abstract
The invention relates to a quality control method of granules which can treat cold-defying gastritis. The method is characterized in that a thin-layer chromatography is adopted to identify Szechwan lovage rhizome, gamene, inula flower, peach kernel and platyciad semen in the preparation; the thin-layer chromatogram identification of the five medicines adopts same sample solution and is finished on three silica gel thin-layer plates, which is simple, quick and free from pollution. By using a HPLC method and taking acetonitrile-methanol-0.1 percent of phosphoric acid as moving phases and taking 316nm as the detection wavelength, the method fixes the amount of ferulic acid which is an effective ingredient of the preparation; by extracting and removing impurity, interference peak is excluded and the method is accurate and reappeared. The quality control method has the effect that in the seven medicines of the prescription, the thin-layer chromatogram identification of five medicines and the quantitative determination of the effective ingredients of monarch drugs are enlarged, thus forming high-standard medicines quality standards. Compared with the conventional method, the quality control method not only controls the quality of the medicines in all dimensions, but also has the advantages of high detection efficiency, short time, low cost and no pollution.
Description
Technical field
The present invention relates to a kind of method of quality control for the treatment of the frosttenderless gastritis granule.
Background technology
Aspect preventing and curing diseases, traditional Chinese medicine and extraction preparation thereof are in occupation of important position, and its method of quality control all is that thin layer is differentiated and assay.But in all kinds of state quality standards, thin layer is differentiated the discriminating that is mostly single medical material.Disturb for getting rid of, the pre-treatment program of sample is how complicated, loaded down with trivial details, needs with a large amount of toxicity organic reagents purification process repeatedly, require great effort, time-consuming, take reagent, contaminated environment, health risk, sense cycle is long.The previous quality standard that contains 5～6 thin layers discriminatings and binomial assay of order detects to be finished, and will spend 4～5 days time at least, and longer as the retrial spended time, detection speed is seriously restricting modernization of Chinese medicine speed of production.So seek simple, fast detection method, improve detection efficiency, reduce and detect cost, reduce the pollution of toxic agent to environment, become the difficulty that Chinese medicine quality control must break through.
A kind of treatment frosttenderless gastritis granule, be made up of Flos Inulae, Radix Angelicae Sinensis, Herba Lycopi, Radix Rubiae, Radix Curcumae, Semen Persicae, Semen Platycladi seven flavor Chinese medicines, the ratio of weight and number of each Chinese crude drug was during its prescription was formed: respectively 3～5 parts of Flos Inulae, Radix Angelicae Sinensis, Radix Rubiae, Radix Curcumae, Herba Lycopi, Semen Persicae, Semen Platycladi.Finish 5 discriminatings and 1 assay by traditional detection method, take 3～4 day time at least.
The present invention is exactly at above-mentioned difficult point, invented and adopted the ultransonic need testing solution of same methanol, on 3 blocks of lamellaes, easy, differentiate Radix Angelicae Sinensis, Radix Rubiae, Semen Persicae, Semen Platycladi and Flos Inulae five tastes medical material quickly, and also developing solvent also is nontoxic organic reagent.And, directly adopt the aqueous acid dilution method with aqueous alcohol liquid, and carry out abstraction impurity removal, avoid the destruction of evaporate to dryness to composition ferulic acid to be measured, guaranteed the accuracy and the repeatability of assay method.
This invention effectively improves detection speed, reduces and detects cost, reduces environmental pollution, and provides the high level drug standard for comprehensive control drug quality.
Summary of the invention
Adopt thin layer chromatography to 5 flavor Chinese medicines in the prescription, Radix Angelicae Sinensis, Radix Rubiae, Semen Persicae, Semen Platycladi and Flos Inulae are differentiated, the thin layer of five tastes medical material is differentiated and is adopted same need testing solution, on 3 blocks of lamellaes, finish, and control medicinal material also all is the ultransonic supernatant solution of methanol, differentiate methanol 26ml, nontoxic developing solvent 30ml, the 1.0 hours time of only needing for five.Easy, quick, cost is low, pollution-free.
Using high-efficient liquid phase technique, is mobile phase with acetonitrile-methanol-0.1% phosphoric acid; 316nm carries out quantitatively the effective ingredient ferulic acid in the preparation for detecting wavelength.Adopt aqueous acid directly to dilute the method for aqueous methanol solution, avoid the evaporate to dryness operation, again by lower boiling extracted with diethyl ether, the evaporation of limit temperature is got rid of first and is disturbed, and second reduces ferulic acid Yin Gaowen, make the drawback of content reduction, effectively improved accuracy, repeatability and the precision of method.Methodological study shows: the ferulic acid sample size is at 0.00584～1.46 μ g, and sample size and peak area are good linear relationship, and its regression equation is: Y=6801136X-15199.5, Y=0.99998.Adopt application of sample to reclaim experiment, the response rate of ferulic acid is 98.97% (n=9), and RSD is 0.77% (seeing Table 1).
The present invention solves the scheme that its technical problem adopts:
This product 2～3g is got in [discriminating] (1), adds methanol 3～5ml, and supersound process 5～10 minutes filters, and filtrate is as need testing solution.Other gets Radix Angelicae Sinensis, each 0.2～1g of Radix Rubiae control medicinal material powder, add methanol 4～8ml respectively, supersound process 5～10 minutes, the supernatant conduct is control medicinal material solution separately, draw control medicinal material solution 3～5 μ l, need testing solution 6-8 μ l, put respectively in same be the silica gel G F of binding agent with the sodium carboxymethyl cellulose
254On the lamellae, with cyclohexane extraction-ethyl acetate-formic acid (4～8: 1～2: 0.1～0.2) be developing solvent, launch, take out, dry, put as early as possible under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of Radix Rubiae control medicinal material chromatograph on, show the fluorescence speckle of two same colors at least; With the corresponding position of Radix Angelicae Sinensis control medicinal material chromatograph on, show an identical fluorescence principal spot (see figure 1).
(2) get Flos Inulae control medicinal material powder 0.2～0.4g, add methanol 4～6ml respectively, supersound process 5～10 minutes, supernatant is medical material solution in contrast, draw each the 5-8 μ l of need testing solution under control medicinal material solution and the discriminating (1), put respectively in same be the silica gel G F of binding agent with the sodium carboxymethyl cellulose
254On the lamellae, with ethyl acetate-butanone-formic acid-water (12～18: 1～1.2: 0.5～0.6: 0.5～0.6) 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 control medicinal material chromatograph on, show the fluorescence speckle of a same color at least; Put again under the ultra-violet lamp (254nm) and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence quenching speckle (seeing Fig. 2,3) of a same color at least.
(3) get Semen Persicae control medicinal material powder 0.2～0.5g, Semen Platycladi control medicinal material powder 0.05～0.2g, add methanol 3～6ml, supersound process 5～10 minutes, the supernatant conduct is control medicinal material separately, draw each 7～8 μ l of need testing solution under control medicinal material solution 3～5 μ l and discriminating (1) item, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with cyclohexane extraction-ethyl acetate-formic acid (4～8: 1～2: 0.1～0.2) be developing solvent, launch, take out, dry, spray is with 2% phosphomolybdic acid ethanol solution, and it is clear that hot blast blows to the speckle colour developing, in the test sample chromatograph, with Semen Persicae and Semen Platycladi control medicinal material chromatograph relevant position on, show the principal spot (see figure 4) of 1～2 same color respectively.
[assay] measured according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica, acetonitrile-methanol-0.1% phosphoric acid solution (10～16: 2～5: 70～79) be mobile phase; The detection wavelength is 316nm, flow velocity 08～1.0ml/min.Number of theoretical plate is not less than 4000 by the calculating of ferulic acid peak.
Reference substance solution prepares precision, and to take by weighing ferulic acid an amount of, adds 70% methanol and make the solution that every 1ml contains 0.003～0.01mg, promptly.
Need testing solution preparation gets that this product is an amount of, and porphyrize takes by weighing about 1g, and accurate the title puts in the tool plug conical flask calmly, the accurate 60% methanol 25ml that adds, close plug claims to decide weight, and supersound process 10～60 minutes is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up, filter with methanol.Get subsequent filtrate 10～15ml, add 0.5% hydrochloric acid (ml/ml), 10～15ml, shake up, with extracted with diethyl ether 4 times, each 10～15ml merges ether solution, does not distinguish the flavor of to there being ether 40 ℃ of water-bath Back stroke, with 30～70% methanol, residual solution is quantitatively transferred in 5～10ml measuring bottle, and, shaken up to scale, filter, promptly get need testing solution.
Accurate respectively reference substance solution and each 10～20 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Inventive principle:
1. the chemical constitution according to each effective ingredient of Chinese medicine is different with polarity, and along with moving of developing solvent, the absorption on lamellae, desorption ability and different are separated the speckle of each effective ingredient.Again by each effective ingredient under the different conditions of inspecting, present different spot colors, make on the same block of lamellae and can detect several composition speckles simultaneously without interfering with each other.
2. by easy sour water dilution, abstraction impurity removal, the evaporation of limit temperature, and component, ratio, the detection wavelength of adjusting mobile phase, solved because of impurity peaks disturbs, a difficult problem that can't quantitative assay, and improved accuracy, repeatability and the precision of method.Make composition to be measured under selected detection wavelength, peak area that is presented and content are the good linear relation, and are able to quantitative assay.
Innovative point of the present invention and beneficial effect are as follows:
(1) broken through a sample solution, a lamellae, detect a kind of traditional identification method of Chinese medicine, innovated same need testing solution, on 3 blocks of lamellaes, to finish the quick thin layer of 5 flavor Chinese medicines and differentiate new method, Radix Angelicae Sinensis, Radix Rubiae are on a lamellae, Flos Inulae is on a lamellae, and Semen Persicae and Semen Platycladi are on a lamellae.
(2) when preparation thin layer need testing solution and control medicinal material solution, avoided the operating procedure of serious environment pollution such as extraction, evaporate to dryness, extraction and experimenter's health, each sample only is that simple methanol is ultrasonic, can obtain experimental solutions.Differentiate sample 2～3g, methanol 26ml, developing solvent 30ml, the 1.0 hours time of only needing for five; Easy, quick, cost is low, pollution-free.
(3) developing solvent of the present invention system has avoided toxic agent such as benzene, toluene, chloroform, only adopted avirulent cyclohexane extraction, ethyl acetate, butanone, formic acid and water just to finish detection, and clear spot is easily declared.
(4) adopt aqueous acid directly to dilute the method that aqueous methanol is extracted solution, avoid the evaporate to dryness operation, again by lower boiling extracted with diethyl ether, the evaporation of limit temperature, a difficult problem and ferulic acid Yin Gaowen that can't quantitative assay, the drawback that content is reduced have been solved because of impurity peaks disturbs, effectively improved the accuracy of method, repeatability and precision.Make composition to be measured under selected detection wavelength, crest separates good (seeing Fig. 5,6,7).
(5) the present invention compares with traditional method of quality control, improves detection efficiency, saves detection time, reduces and detects cost, reduces environmental pollution, and provides the high level drug standard for comprehensive control drug quality.
Description of drawings
Fig. 1 is that the thin layer of Radix Rubiae and Radix Angelicae Sinensis is differentiated figure
Fig. 2 differentiates (inspecting under the 365nm) figure for the Flos Inulae thin layer
Fig. 3 differentiates (inspecting under the 254nm) figure for the Flos Inulae thin layer
Fig. 4 is that Semen Persicae and Semen Platycladi thin layer are differentiated figure
Fig. 5 ferulic acid reference substance HPLC chromatogram
Fig. 6 treats the HPLC chromatogram of frosttenderless gastritis granule
Fig. 7 does not contain the blank sample chromatogram of Radix Angelicae Sinensis
Among Fig. 1,1 is the Radix Rubiae blank sample, and 2 is the Radix Rubiae control medicinal material, and 3 is the Radix Angelicae Sinensis blank sample, and 4 is the Radix Angelicae Sinensis control medicinal material, and 5.6.7 is a sample.
Fig. 2 and Fig. 3 are same block of lamellae, and Fig. 2 inspects under uviol lamp 365nm, and Fig. 3 inspects under uviol lamp 254nm, and the sample label of Fig. 2 and Fig. 3 is the same, and 1.2.3 is a sample, and 4 is the Flos Inulae control medicinal material, and 5 is the Flos Inulae blank sample.
Among Fig. 4,1 is the Semen Platycladi control medicinal material, and 2 is the Semen Persicae control medicinal material, and 3 is Semen Persicae, Semen Platycladi blank sample, and 4.5.6 is a sample.
Among Fig. 5,1 is ferulic acid reference substance chromatographic peak.
Among Fig. 6,1 is ferulic acid chromatographic peak in the sample.
Among Fig. 7, be the chromatographic peak of blank sample.
The specific embodiment of the invention is as follows:
This product 2～3g is got in [discriminating] (1), adds methanol 3～5ml, and supersound process 5～10 minutes filters, and filtrate is as need testing solution.Other gets Radix Rubiae, each 0.2～1g of Radix Angelicae Sinensis control medicinal material powder, add methanol 4～8ml respectively, supersound process 5～10 minutes, the supernatant conduct is control medicinal material solution separately, draw control medicinal material solution 3～5 μ l, need testing solution 6-8 μ l, put respectively in same be the silica gel G F of binding agent with the sodium carboxymethyl cellulose
254On the lamellae, with cyclohexane extraction-ethyl acetate-formic acid (4～8: 1～2: 0.1～0.2) be developing solvent, launch, take out, dry, put as early as possible under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of Radix Rubiae control medicinal material chromatograph on, show the fluorescence speckle of two same colors at least; With the corresponding position of Radix Angelicae Sinensis control medicinal material chromatograph on, show an identical fluorescence principal spot (see figure 1).
(2) get Flos Inulae control medicinal material powder 0.2～0.4g, add methanol 4～6ml respectively, supersound process 5～10 minutes, supernatant is medical material solution in contrast, draw each the 5-8 μ l of need testing solution under control medicinal material solution and the discriminating (1), put respectively in same be the silica gel G F of binding agent with the sodium carboxymethyl cellulose
254On the lamellae, with ethyl acetate-butanone-formic acid-water (12～18: 1～1.2: 0.5～0.6: 0.5～0.6) 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 control medicinal material chromatograph on, show the fluorescence speckle of a same color at least; Put again under the ultra-violet lamp (254nm) and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence quenching speckle (seeing Fig. 2,3) of a same color at least.
(3) get Semen Persicae control medicinal material powder 0.2～0.5g, Semen Platycladi control medicinal material powder 0.05～0.2g, add methanol 3～6ml, supersound process 5～10 minutes, the supernatant conduct is control medicinal material separately, draw each 7～8 μ l of need testing solution under control medicinal material solution 3～5 μ l and discriminating (1) item, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with cyclohexane extraction-ethyl acetate-formic acid (4～8: 1～2: 0.1～0.2) be developing solvent, launch, take out, dry, spray is with 2% phosphomolybdic acid ethanol solution, and it is clear that hot blast blows to the speckle colour developing, in the test sample chromatograph, with Semen Persicae and Semen Platycladi control medicinal material chromatograph relevant position on, show the principal spot (see figure 4) of 1～2 same color respectively.
[assay] measured according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica, acetonitrile-methanol-0.1% phosphoric acid solution (10～16: 2～5: 70～79) be mobile phase; The detection wavelength is 316nm, flow velocity 08～1.0ml/min.Number of theoretical plate is not less than 4000 by the calculating of ferulic acid peak.
Reference substance solution prepares precision, and to take by weighing ferulic acid an amount of, adds 70% methanol and make the solution that every 1ml contains 0.003～0.01mg, promptly.
Need testing solution preparation gets that this product is an amount of, and porphyrize takes by weighing about 1g, and accurate the title puts in the tool plug conical flask calmly, the accurate 60% methanol 25ml that adds, close plug claims to decide weight, and supersound process 10～60 minutes is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up, filter with methanol.Get subsequent filtrate 10～15ml, add 0.5% hydrochloric acid (ml/ml), 10～15ml, shake up, with extracted with diethyl ether 4 times, each 10～15ml merges ether solution, does not distinguish the flavor of to there being ether 40 ℃ of water-bath Back stroke, with 30～70% methanol, residual solution is quantitatively transferred in 5～10ml measuring bottle, and, shaken up to scale, filter, promptly get need testing solution.
Accurate respectively reference substance solution and each 10～20 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.Measure 4 batch sample content, the results are shown in subordinate list 2.
Ferulaic acid content measurement result in the subordinate list 2 treatment frosttenderless gastritis samples
Claims (2)
1. thin layer is differentiated
A. (4～8: 1～2: being developing solvent 0.1～0.2), is carrier with silica gel, and ultra-violet lamp 365nm has differentiated Radix Angelicae Sinensis, Radix Rubiae for inspecting wavelength simultaneously on same block of lamellae with cyclohexane extraction-ethyl acetate-formic acid.
B. (12～18: 1～1.2: 0.5～0.6: being developing solvent 0.5～0.6), is carrier with silica gel, and ultra-violet lamp 365nm and 254nm have differentiated Flos Inulae for inspecting wavelength with ethyl acetate-butanone-formic acid-water.
C. (4～8: 1～2: being developing solvent 0.1～0.2), is carrier with silica gel, and 1% phosphomolybdic acid ethanol solution is a developer, has differentiated Semen Persicae and Semen Platycladi simultaneously on same block of lamellae with cyclohexane extraction-ethyl acetate-formic acid.
Above-mentioned all discriminatings are adopted with a need testing solution, and all control medicinal materials all are the ultransonic supernatant of methanol, and method is easy, quick, clear spot.
2. assay
A. the test of chromatographic condition and system suitability is a filler with octadecylsilane chemically bonded silica, acetonitrile-methanol-0.1% phosphoric acid solution (10～16: 2～5: 70～79) be mobile phase; The detection wavelength is 316nm, flow velocity 0.8～1.0ml/min.Number of theoretical plate is not less than 4000 by the calculating of ferulic acid peak.
B. reference substance solution prepares precision to take by weighing ferulic acid an amount of, adds 70% methanol and makes the solution that every 1ml contains 0.003～0.01mg, promptly.
C. it is an amount of that this product is got in the need testing solution preparation, and porphyrize takes by weighing about 1g, and accurate the title decides, and puts in the tool plug conical flask, the accurate 60% methanol 25ml that adds, close plug claims to decide weight, and supersound process 10～60 minutes is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up, filter with methanol.Get subsequent filtrate 10～15ml, add 0.5% hydrochloric acid (ml/ml), 10～15ml, shake up, with extracted with diethyl ether 4 times, each 10～15ml merges ether solution, does not distinguish the flavor of to there being ether 40 ℃ of water-bath Back stroke, with 30～70% methanol, residual solution is quantitatively transferred in 5～10ml measuring bottle, and, shaken up to scale, filter, promptly get need testing solution.
D. accurate respectively reference substance solution and each 10～20 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008100553409A CN101352558A (en) | 2008-07-07 | 2008-07-07 | Quality control method of granular formulation for treating gastricism without aversion to cold |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103105447A (en) * | 2011-11-09 | 2013-05-15 | 贵州益佰制药股份有限公司 | Detection method for Cinnamomum migao heart-comforting preparation |
| CN109406707A (en) * | 2018-11-29 | 2019-03-01 | 四川新绿色药业科技发展有限公司 | A kind of TLC Identification of stir-baked SEMEN PERSICAE and its preparation |
-
2008
- 2008-07-07 CN CNA2008100553409A patent/CN101352558A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103105447A (en) * | 2011-11-09 | 2013-05-15 | 贵州益佰制药股份有限公司 | Detection method for Cinnamomum migao heart-comforting preparation |
| CN103105447B (en) * | 2011-11-09 | 2014-09-24 | 贵州益佰制药股份有限公司 | Detection method for Cinnamomum migao heart-comforting preparation |
| CN109406707A (en) * | 2018-11-29 | 2019-03-01 | 四川新绿色药业科技发展有限公司 | A kind of TLC Identification of stir-baked SEMEN PERSICAE and its preparation |
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Open date: 20090128 |