CN101618119A - Quality standard of Sinopanax formosanus pills - Google Patents
Quality standard of Sinopanax formosanus pills Download PDFInfo
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- CN101618119A CN101618119A CN200810053757A CN200810053757A CN101618119A CN 101618119 A CN101618119 A CN 101618119A CN 200810053757 A CN200810053757 A CN 200810053757A CN 200810053757 A CN200810053757 A CN 200810053757A CN 101618119 A CN101618119 A CN 101618119A
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Abstract
The invention relates to a quality standard of Sinopanax formosanus pills. In the quality standard, the physical and chemical distinction with poor specificity in the prior standard is deleted, thin-layer identification of scopoletin is added, a method for determining the content of alkaloid by acid dye colorimetry in the prior standard is cancelled, and the contents of the scopoletin and atropine are determined by liquid chromatography. The method for determining the contents of the atropine and the scopoletin has the advantages that: the operation step is simple; the operation time is shortened compared with the prior art, and the detection time for a batch of products is generally about 2 hours; in the whole operation process, manual operation is less, the error resulted from individual difference is decreased to the lowest degree, and the data is completely viewed and processed by computer software; and the method is accurate, reliable, easy in operation and good in reproduction. The quality standard can be used in the daily quality control of the Sinopanax formosanus pills to further guarantee the inner quality of the products and have great meaning for guaranteeing the safe administration to patients.
Description
Technical field
The present invention relates to technical field of Chinese medicines, particularly relate to the quality standard of the Radix Physochlainae drop pill that Radix Physochlainae paste and substrate (Polyethylene Glycol) makes in right amount
Background technology
The Radix Physochlainae drop pill is the relieving asthma and cough expectorant, since throwing in market, has obtained numerous patients' generally approval with its determined curative effect, advantage such as take effect rapidly.Primary standard is recorded in 1995 editions pharmacopeia 1997 enlarged editions, and in standard, Radix Physochlainae drop pill quality standard is recited as: this product is the drop pill that Radix Physochlainae paste and substrate (Polyethylene Glycol) are made in right amount.
[character] this product is brown drop pill; Mildly bitter flavor.
[discriminating] gets this product 10 balls, adds ethanol 5ml, porphyrize, and warm 10 minutes, filter, filtrate evaporate to dryness, residue add 5% sulfuric acid solution makes dissolving, filters.Get filtrate 1ml, add 1～2 of test solution of mercuric potassium iodide, generate faint yellow precipitation; Other gets filtrate 1ml, adds 1～2 of bismuth potassium iodide test solution, generates reddish brown precipitation.
[inspection] should meet every regulation relevant under the drop pill item (15 pages of 1990 editions appendix of Chinese Pharmacopoeia)
The preparation of [assay] reference substance solution: precision takes by weighing at 1 hour atropine sulfate 30mg of 120 ℃ of dryings, puts in the 25ml measuring bottle, adds water and makes and be dissolved to scale, shakes up.Accurate draw solution 15ml puts in the 100ml measuring bottle, and thin up promptly gets (1ml contains anhydrous slufuric acid atropine 180 μ g) to scale.The preparation of need testing solution: get this product 80 balls, porphyrize, precision takes by weighing in right amount (weight that is equivalent to 12 balls approximately), puts in the 10ml measuring bottle, and it is an amount of to add water, and supersound process 30 minutes is diluted with water to scale.Filter, discard filtrate just, divide and get subsequent filtrate, promptly.
Algoscopy: precision is measured test sample and each 1ml of reference substance solution, puts respectively in the separatory funnel, respectively adds acetic acid-sodium acetate buffer solution (PH:3.7) 5ml, precision adds 0.15% orange N solution 5ml again, shakes up, and each usefulness chloroform 8ml jolting gently extracted 3 minutes, left standstill 30 minutes, divide and get the chloroform layer, filter in the 50ml measuring bottle reuse chloroform extraction 4 times with the moistening filter paper of chloroform, each 8ml, filter is gone in the measuring bottle successively, and the accurate 1% sulphuric acid methanol solution 6ml that adds washs on a small quantity with chloroform, filter paper, washing liquid is incorporated in the measuring bottle, until scale, shakes up, use spectrophotography, wavelength place at 545nm measures trap respectively, calculates, promptly.
This product contains alkaloid with hyoscyamine (C
17H
23NO
3) calculate and should be 90.0～110.0% of labelled amount (0.12mg/ ball).
[function with cure mainly] Dingchuan, cough-relieving is eliminated the phlegm.Be used for chronic bronchitis, asthmatic tracheitis.
[usage and consumption] usual amounts, buccal, a 1-2 ball, 3-6 ball on the one.The maximum dose buccal, one time 4 ball, one day 12 ball.
[specification] every ball contains alkaloid 0.12mg.
[attention] glaucoma patient is avoided usefulness, and anemia of pregnant woman and prostate be the careful usefulness of loose person extremely.
Shady and cool dry place is put in [storage] sealing.
[useful life] 3 years.
Character: this product is the sepia thick paste.
Assay: measure according to assay method (wherein the preparation of need testing solution changes precision into and takes by weighing Radix Physochlainae paste 50mg, puts in the 10ml measuring bottle, and is as follows) under the Radix Physochlainae drop pill item, this product contains alkaloid with hyoscyamine (C
17H
23NO
3) calculate, should be 5.7-7.8%.
Main effective ingredient-alkaloids content the detection method of Radix Physochlainae drop pill is an acid-dye colorimetry in above-mentioned standard, and there is following shortcoming in this detection method:
1, complicated operation relates to numerous steps such as preparation, extraction, colour developing, colorimetric;
2, the operating time tediously long, the detection time of common a collection of product is about 4.5 hours;
3, anthropic factor influence is more in the operating process, and particularly the operation technique of extraction time and separatory funnel has inconsistently slightly in extraction process, can cause the repeatability of final result to occur than big-difference.
Chinese Pharmacopoeia is strict day by day to the quality control requirement of Chinese patent medicine product, tcm product assay item requires the effective ingredient kind is controlled as much as possible, Market competition, quality level to product requires constantly to promote, the quality standard that promotes product is imperative, to increase the competitiveness of product in market.
Summary of the invention
The objective of the invention is one of physicochemical identification in the primary standard is deleted, reason is that the specificity of precipitation is poor in the compound preparation, can not say something.
Another object of the present invention is that the thin layer that has increased scopoletin in the standard is differentiated.
Another object of the present invention is to have cancelled the method for acid-dye colorimetry mensuration alkaloid in the primary standard, adopt liquid chromatography for measuring Anisodamine and atropinic content, improve Radix Physochlainae drop pill active constituent content measuring method, improve the technical merit that its quality improves its quality standard.
For reach purpose of the present invention we through inspection information, alkaloid in the Radix Physochlainae drop pill is mainly tropane constituents (mainly comprising compositions such as atropine, scopolamine, Anisodamine), for improving the quality control level of product, make the extensive patients medication safer, reasonable, enterprise's decision is revised standard in former 1995 editions pharmacopeia 1997 enlarged editions, provide a kind of quality standard of Radix Physochlainae drop pill, the drop pill that Radix Physochlainae paste and substrate (Polyethylene Glycol) are made in right amount; The method for making of Radix Physochlainae paste: get the Radix Physochlainae piece,, add 1-10 and doubly measured backflow 1-3 hour for the 1st time with alcohol heating reflux 2 times, add 1-10 for the 2nd time and doubly measured backflow 1-3 hour, merge extractive liquid, filters, reclaim ethanol, leave standstill, get supernatant and be recycled to the thick paste shape, add the dilution of 1-10 times of water, after regulating PH and being 9-10, with 1/2 times of chloroform extraction 1-10 time, merge extractive liquid, filters, and water-bath concentrates, that is, it is characterized in that every ball contains Anisodamine and atropine content total should be 150.00 μ g ± 20%.
The quality standard of described Radix Physochlainae drop pill, it is characterized in that increase the thin layer diagnostic test project that is provided with scopoletin in the quality standard, the thin layer identification of test method of wherein set scopoletin is: get this product 0.5g, grind, add dehydrated alcohol 20ml, extract, put into refrigerator cold-storage after the dissolving with ultrasonic or hot reflux or merceration processing, filter, the filtrate evaporate to dryness adds methanol or ethanol or n-butyl alcohol or chloroform 1ml dissolving, as need testing solution; Other gets the scopoletin reference substance, adds methanol or ethanol or n-butyl alcohol or chloroform and makes the solution that every ml contains 1mg, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-methanol-liquor ammoniae fortis (1～20): (0.1～5): (0.5～3) is 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.
The quality standard of described Radix Physochlainae drop pill is characterized in that, is provided with the diagnostic test project of the assay of Anisodamine and atropine content in the quality standard, and wherein set atropine, the identification of test method of Anisodamine are:
Chromatographic condition and system suitability test: with eight alkyl silane bonded silica gels is filler, with acetonitrile-(5～12) mmol/L sodium lauryl sulphate (30～60): (40～70) are as mobile phase, detecting wavelength is (205～260) nm, flow velocity 0.5-1.5ml/min, 20～50 ℃ of column temperatures, theoretical cam curve is for being not less than 2000.
The preparation of reference substance solution: it is an amount of to get the anisodamine hydrobromide reference substance, and accurate the title decides, and adds sulphuric acid or hydrochloric acid and makes the solution that every 1ml contains 700 μ g, in contrast the product solution I; It is an amount of that other gets the atropine sulfate reference substance, and accurate the title decides, and adds sulphuric acid or hydrochloric acid and makes the solution that every 1ml contains 750 μ g, in contrast the product solution II; Precision is measured in reference substance solution I and each 1ml to 10ml volumetric flask of reference substance solution II, with sulphuric acid or hydrochloric acid standardize solution, makes every 1ml and contains Anisodamine 70 μ g, and the solution of atropine 75 μ g promptly;
The preparation of need testing solution: precision takes by weighing profit and requires 1 described Radix Physochlainae drop pill test sample sample to get 20 of this product, porphyrize, and precision takes by weighing 300mg, put in the 10ml volumetric flask, with sulphuric acid or hydrochloric acid standardize solution, extracted supersound process or hot reflux or merceration 20 minutes, shake up;
Algoscopy: accurate reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
The quality standard of described Radix Physochlainae drop pill is characterized in that, is provided with the diagnostic test project of the assay of Anisodamine and atropine content in the quality standard, and wherein set atropine, the identification of test method of Anisodamine are:
Chromatographic condition and system suitability test: with eight alkyl silane bonded silica gels is filler; Acetonitrile-0.01mol/L sodium lauryl sulphate 33: 67; Detect wavelength: 210nm, flow velocity: 1ml/min column temperature: 40 ℃; Number of theoretical plate is 2500, and the separating degree of adjacent chromatographic peak is greater than 1.5;
The preparation of reference substance solution: it is an amount of to get the anisodamine hydrobromide reference substance, and accurate the title decides, and adds sulphuric acid and makes the solution that every 1ml contains 700 μ g, in contrast the product solution I; Other is taken at 120 ℃, and 1 hour atropine sulfate reference substance of drying is an amount of down, and accurate the title decides, and adds sulphuric acid to make the solution that every 1ml contains 750 μ g, in contrast the product solution II; Precision is measured in reference substance solution I and each 1ml to 10ml volumetric flask of reference substance solution II, uses the sulphuric acid standardize solution, makes every 1ml and contains Anisodamine 70 μ g, and the solution of atropine 75 μ g promptly;
The preparation of need testing solution: precision takes by weighing profit and requires 1 described Radix Physochlainae drop pill test sample sample to get 20 of this product, porphyrize, and precision takes by weighing 300mg, puts in the 10ml volumetric flask, uses the sulphuric acid standardize solution, extracts supersound process or hot reflux or merceration 20 minutes, shakes up;
Algoscopy: accurate reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
The invention effect: the present invention deletes one of the physicochemical identification of primary standard special secondary school attribute difference, the thin layer that has increased scopoletin is differentiated, cancelled the method for acid-dye colorimetry mensuration alkaloid in the primary standard, adopt liquid chromatography for measuring Anisodamine and atropinic content, the content detecting method of atropine, Anisodamine has following superiority:
1, operating procedure is simple;
2, the operating time shortens than prior art, and the detection time of common a collection of product is about 2 hours;
3, in the whole operation process, manual operation is few, the error that individual variation causes drops to minimum, computer software are all adopted in the observation of data and processing, and this method is accurate, reliable, easy operating, favorable reproducibility, can be used for the daily quality control of Radix Physochlainae drop pill, further guarantee the product inherent quality, for guaranteeing that the patient safety medication is significant.
The specific embodiment
Embodiment 1: definite target component that can be detected
Several composition mother nucleus structure unanimities of hyoscyami alkanes, the difference part only is the difference of substituted radical, its chemical property is quite similar, still selected liquid chromatography as experimental program, our experiment two subject matters that will solve are to determine that the target component that can be detected and the screening of experiment condition determine.
Come alternative or combination by investigating separating degree and contents level, preliminary experiment, we find mainly to contain atropine, scopolamine and Anisodamine in the total alkaloids of Radix Physochlainae drop pill, therefore, as investigating object, see Table 1 with these three kinds of compositions
Table 1 separating degree is investigated the result
| Separating degree (r) | Contents level | |
| Atropine | ＞1.5 | Can be detected |
| Scopolamine | ＜1.5 | Can be detected |
| Anisodamine | ＞1.5 | Can be detected |
We find in the total alkaloids of Radix Physochlainae drop pill with atropinic content maximum, and separating degree is better, and its contents level in alkaloid is also comparatively stable; Though scopolamine detects, separating degree does not meet the methodology requirement.Simultaneously, we consider that again only to measure atropine more single for control of product quality, so increased Anisodamine again, such two kinds of materials are investigated simultaneously and had more representativeness, and can accurately measure, and can obtain good effect.So, determine that the target component that can be detected is: atropine, Anisodamine.Therefore our decision is that the index thing detects with reflection total alkaloids level with Anisodamine and atropine.
Differentiate:
1, one of physicochemical identification in the primary standard is deleted.Reason is that the specificity of precipitation is poor in the compound preparation, can not say something.
2, the thin layer that has increased scopoletin is differentiated: get this product 0.5g, grind, add dehydrated alcohol 20ml, supersound process was put into refrigerator cold-storage about 30 minutes after the dissolving, filtered, and the filtrate evaporate to dryness adds methanol 1ml dissolving, as need testing solution.Other gets the scopoletin reference substance, adds methanol and makes the solution that every ml contains 1mg, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-methanol-liquor ammoniae fortis (17: 2: 1) is 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.The thin layer collection of illustrative plates is seen the accompanying drawing 1 in the substantive examination reference material 1.
Assay: cancelled the method for acid-dye colorimetry mensuration alkaloid in the primary standard, adopted liquid chromatography for measuring Anisodamine and atropinic content.
Embodiment 2: determine optimum experimental condition
1. instrument and reagent
1. instrument
HP1100 type chromatograph of liquid, VWD ultraviolet-visible detector, HP Chemstation chem workstation, Sai Duolisi R200D type electronic analytical balance; KQ-400DB type numerical control supersonic washer
2. reagent: standard substance: anisodamine hydrobromide: available from Nat'l Pharmaceutical ﹠ Biological Products Control Institute, lot number: 0051-94097; Atropine sulfate: available from Nat'l Pharmaceutical ﹠ Biological Products Control Institute, lot number: 200510. reagent: acetonitrile is a chromatographically pure; Sodium lauryl sulphate is an analytical pure; Water is the secondary redistilled water; Sample: the Radix Physochlainae drop pill, provide by the our factory, lot number is: experiment 06001,07001,07002,07003,07004,07005.
2. method and result
Chromatographic condition and system suitability test: with eight alkyl silane bonded silica gels is filler, with acetonitrile-5～12mmol/L sodium lauryl sulphate 30～60: 40～70 as mobile phase, the detection wavelength is 205～260nm, flow velocity 0.5～1.5ml/min, 20～50 ℃ of column temperatures, theoretical cam curve is for being not less than 2000.
Optimum experimental condition:
1. chromatographic condition: ZORBAX XDB-C8 (5 μ m, the chromatographic column of 4.6mm * 150mm), acetonitrile-0.01mol/L sodium lauryl sulphate (33: 67)
Detect wavelength: 210nm, flow velocity: 1ml/min column temperature: 40 ℃; Number of theoretical plate is 2500, and the separating degree of adjacent chromatographic peak is greater than 1.5.
2. the preparation of reference substance solution: it is an amount of to get the anisodamine hydrobromide reference substance, and accurate the title decides, and adds 0.01mol/L sulphuric acid and makes the solution that every 1ml contains 700 μ g, in contrast the product solution I.Other is taken at 120 ℃, and 1 hour atropine sulfate reference substance of drying is an amount of down, and accurate the title decides, and adds 0.01mol/L sulphuric acid to make the solution that every 1ml contains 750 μ g, in contrast the product solution II.Precision is measured in reference substance solution I and each 1ml to 10ml volumetric flask of reference substance solution II, with 0.01mol/L sulphuric acid standardize solution, makes every 1ml and contains Anisodamine 70 μ g, and the solution of atropine 75 μ g promptly.
3. the preparation of need testing solution: get 20 of this product, porphyrize, precision takes by weighing in right amount (about 300mg), puts in the 10ml volumetric flask, and with 0.01mol/L sulphuric acid standardize solution, supersound process 20 minutes shakes up.
Algoscopy: accurate reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.Chromatogram is seen accompanying drawing 2.
3. linear relationship is investigated:
Precision measures that anisodamine hydrobromide and atropine sulfate mix contrast liquid 0.2,0.6,1.0,1.4,1.8,2.2mL puts in the 10mL volumetric flask respectively, with the 0.01mol/l Dilution of sulphuric acid to scale, shake up, measure by above-mentioned chromatographic condition, being vertical coordinate with each component peaks area integral value respectively, is abscissa drawing standard curve with standard substance concentration, calculates regression equation and correlation coefficient, the result shows that linear relationship is good, the results are shown in Table 2.
Table 2. linear relationship is investigated result of the test
| Regression equation | Correlation coefficient (r) | The range of linearity (μ g/ml) | |
| Anisodamine hydrobromide | ??Y＝0.55054x-0.28771 | ??0.9999 | ??14.08～154.88 |
| Atropine sulfate | ??Y＝0.600876x-9.8736 | ??0.9998 | ??14.96~164.56 |
4. precision test:
Get Radix Physochlainae drop pill (lot number is 06001) 300.4mg by above-mentioned need testing solution preparation method preparation, repeat sample introduction continuously 6 times by above-mentioned chromatographic condition, measure content, average ball calculates RSD heavily by 20mg, the results are shown in Table 3.
Table 3. Precision test result (n=6)
| ??1 | ??2 | ??3 | ??4 | ??5 | ??6 | ??RSD ??(％) | |
| Anisodamine (μ g/ ball) | ??36.74 | ??36.83 | ??37.67 | ??37.88 | ??36.78 | ??35.86 | ??1.97 |
| Atropine (μ g/ ball) | ??39.02 | ??36.70 | ??40.12 | ??38.34 | ??39.70 | ??37.48 | ??3.40 |
| Add up on (μ g/ ball) | ??75.76 | ??73.53 | ??77.79 | ??76.22 | ??76.48 | ??73.34 | ??2.32 |
5. replica test:
Get Radix Physochlainae drop pill (lot number is 06001), by the preparation method of above-mentioned need testing solution, 6 parts of need testing solutions of parallel preparation are measured content by above-mentioned chromatographic condition respectively, and average ball calculates RSD heavily by 20mg, the results are shown in Table 4.
Table 4. replica test result (n=6)
| ??1 | ??2 | ??3 | ??4 | ??5 | ??6 | ??RSD ??(％) | |
| Anisodamine (μ g/ ball) | ??34.63 | ??34.65 | ??33.52 | ??36.23 | ??34.39 | ??36.65 | ??3.39 |
| Atropine (μ g/ ball) | ??37.86 | ??37.04 | ??36.55 | ??37.66 | ??37.00 | ??37.13 | ??1.28 |
| Add up on (μ g/ ball) | ??72.49 | ??71.69 | ??70.07 | ??73.89 | ??71.39 | ??73.78 | ??2.04 |
6. recovery test
Get Radix Physochlainae drop pill (lot number is 06001), precision takes by weighing 2.0051g and puts in the 25ml volumetric flask, 0.01mol/l sulphuric acid standardize solution.Precision is measured in 2ml to the 10ml volumetric flask, adds a certain amount of Anisodamine, atropine mixing reference substance solution 0.5ml, with 0.01mol/l sulphuric acid standardize solution.Measure by above-mentioned chromatographic condition, calculate average recovery.The results are shown in Table 5.
Table 5. recovery test result (n=6)
Conclusion: average recovery rate should be in 95～105% scopes.
7. sample determination:
Get 5 batches of Radix Physochlainae drop pill test samples, by the preparation method of above-mentioned need testing solution, make need testing solution, and measure by above-mentioned chromatographic condition, every part of need testing solution sample introduction 2 times obtains Anisodamine and atropinic content in 5 batches of test samples, the results are shown in Table 6.
Table 6. sample determination result (n=5)
8. stability test:
Get 1 batch of Radix Physochlainae drop pill, lot number is 07001, and the preparation method by above-mentioned need testing solution makes need testing solution, and measures by above-mentioned chromatographic condition, and respectively at 1h, 2h, 3h, 4h, 5h, 7h sample introduction once calculate the RSD% value, the results are shown in Table 7.
Table 7. stability test result
The sample determination presentation of results: since the precision test, replica test, and used sample lot number is 06001 in the recovery test, belong to the experiment lot number, by the production technology system of dripping, output is little by laboratory, loss is bigger, and conversion ratio is lower, so the content that records is lower.The used sample of sample determination and stability test is all for by the product of workshop by the production technology system of dripping, and all samples content is all stable, qualified.
9. content limit is formulated: per 1 ball of this product contains Anisodamine and atropine content total should be 150.00 μ g ± 20%.
10. experimental summary:
1. through the detection of methodology investigation and 5 batches of Radix Physochlainae drop pill samples, adopt high performance liquid chromatography that Anisodamine in the Radix Physochlainae drop pill and atropine content are measured.The result shows this method easy operating, highly sensitive, favorable reproducibility, can be used for the daily quality control of Radix Physochlainae drop pill.
2. the quality standard of revising, improve product is the sign that enterprise constantly follows after progress, and also is to respond actively a kind of active measures and the technological reserve that country constantly promotes the pharmaceutical producing enterprise standard.Finishing of this experiment promoted the technology content of Radix Physochlainae drop pill target level of product quality greatly, further guarantees the product inherent quality, for guaranteeing that the patient safety medication is significant.
Claims (4)
1, a kind of quality standard of Radix Physochlainae drop pill, the drop pill that Radix Physochlainae paste and substrate Polyethylene Glycol are made in right amount; The method for making of Radix Physochlainae paste: get the Radix Physochlainae piece,, add 1-10 and doubly measured backflow 1-3 hour for the 1st time with alcohol heating reflux 2 times, add 1-10 for the 2nd time and doubly measured backflow 1-3 hour, merge extractive liquid, filters, reclaim ethanol, leave standstill, get supernatant and be recycled to the thick paste shape, add the dilution of 1-10 times of water, after regulating PH and being 9-10, with 1/2 times of chloroform extraction 1-10 time, merge extractive liquid, filters, and water-bath concentrates, that is, it is characterized in that every ball contains Anisodamine and atropine content total should be 150.00 μ g ± 20%.
2, the quality standard of Radix Physochlainae drop pill according to claim 1, it is characterized in that increasing in the quality standard thin layer diagnostic test project that is provided with scopoletin, the thin layer identification of test method of wherein set scopoletin is: the weighting profit requires 1 described Radix Physochlainae drop pill 0.5g, grind, add dehydrated alcohol 20ml, extract with ultrasonic or hot reflux or merceration processing, put into refrigerator cold-storage after the dissolving, filter, the filtrate evaporate to dryness, add methanol or ethanol or n-butyl alcohol or chloroform 1ml dissolving, as need testing solution; Other gets the scopoletin reference substance, adds methanol or ethanol or n-butyl alcohol or chloroform and makes the solution that every ml contains 1mg, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-methanol-liquor ammoniae fortis 1～20: 0.1～5: 0.5～3 is 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.
3, the quality standard of Radix Physochlainae drop pill according to claim 1, it is characterized in that being provided with in the quality standard diagnostic test project of the assay of Anisodamine and atropine content, wherein set atropine, the identification of test method of Anisodamine are:
Chromatographic condition and system suitability test: with eight alkyl silane bonded silica gels is filler, with acetonitrile-5～12mmol/L sodium lauryl sulphate 30～60: 40～70 as mobile phase, the detection wavelength is 205～260nm, flow velocity 0.5～1.5ml/min, 20～50 ℃ of column temperatures, theoretical cam curve is for being not less than 2000.
The preparation of reference substance solution: it is an amount of to get the anisodamine hydrobromide reference substance, and accurate the title decides, and adds sulphuric acid or hydrochloric acid and makes the solution that every 1ml contains 700 μ g, in contrast the product solution I; It is an amount of that other gets the atropine sulfate reference substance, and accurate the title decides, and adds sulphuric acid or hydrochloric acid and makes the solution that every 1ml contains 750 μ g, in contrast the product solution II; Precision is measured in reference substance solution I and each 1ml to 10ml volumetric flask of reference substance solution II, with sulphuric acid or hydrochloric acid standardize solution, makes every 1ml and contains Anisodamine 70 μ g, and the solution of atropine 75 μ g promptly;
The preparation of need testing solution: precision takes by weighing profit and requires 20 in 1 described Radix Physochlainae drop pill test sample sample, porphyrize, and precision takes by weighing 300mg, puts in the 10ml volumetric flask, with sulphuric acid or hydrochloric acid standardize solution, extracts supersound process or hot reflux or merceration 20 minutes, shakes up;
Algoscopy: accurate reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
4, the quality standard of Radix Physochlainae drop pill according to claim 1, it is characterized in that, be provided with the diagnostic test project of the assay of Anisodamine and atropine content in the quality standard, wherein set atropine, the identification of test method of Anisodamine are:
Chromatographic condition and system suitability test: with eight alkyl silane bonded silica gels is filler; Acetonitrile-0.01mol/L sodium lauryl sulphate 33: 67; Detect wavelength: 210nm, flow velocity: 1ml/min column temperature: 40 ℃; Number of theoretical plate is 2500, and the separating degree of adjacent chromatographic peak is greater than 1.5;
The preparation of reference substance solution: it is an amount of to get the anisodamine hydrobromide reference substance, and accurate the title decides, and adds sulphuric acid and makes the solution that every 1ml contains 700 μ g, in contrast the product solution I; Other is taken at 120 ℃, and 1 hour atropine sulfate reference substance of drying is an amount of down, and accurate the title decides, and adds sulphuric acid to make the solution that every 1ml contains 750 μ g, in contrast the product solution II; Precision is measured in reference substance solution I and each 1ml to 10ml volumetric flask of reference substance solution II, uses the sulphuric acid standardize solution, makes every 1ml and contains Anisodamine 70 μ g, and the solution of atropine 75 μ g promptly;
The preparation of need testing solution: precision takes by weighing profit and requires 20 in 1 described Radix Physochlainae drop pill test sample sample, porphyrize, and precision takes by weighing 300mg, puts in the 10ml volumetric flask, uses the sulphuric acid standardize solution, extracts supersound process or hot reflux or merceration 20 minutes, shakes up;
Algoscopy: accurate reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810053757A CN101618119A (en) | 2008-07-04 | 2008-07-04 | Quality standard of Sinopanax formosanus pills |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810053757A CN101618119A (en) | 2008-07-04 | 2008-07-04 | Quality standard of Sinopanax formosanus pills |
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| CN200810053757A Pending CN101618119A (en) | 2008-07-04 | 2008-07-04 | Quality standard of Sinopanax formosanus pills |
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| CN104237448A (en) * | 2014-10-09 | 2014-12-24 | 成都中医药大学 | Anisodamine root thin-layer detection method |
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| CN104237448A (en) * | 2014-10-09 | 2014-12-24 | 成都中医药大学 | Anisodamine root thin-layer detection method |
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| CN105628853A (en) * | 2015-12-22 | 2016-06-01 | 新疆奇康哈博维药股份有限公司 | Quality detection method for medicinal herb herba cymbopogonis |
| CN108918718A (en) * | 2018-07-26 | 2018-11-30 | 承德市食品药品检验检测中心 | A kind of detection method of hyoscyamine and hyoscine |
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| CN110018257A (en) * | 2019-04-25 | 2019-07-16 | 成都第一制药有限公司 | A kind of detection method of the Anisodine in relation to substance |
| CN110095536A (en) * | 2019-04-25 | 2019-08-06 | 成都第一制药有限公司 | A kind of Anisodine detection method of content |
| CN110095538A (en) * | 2019-04-25 | 2019-08-06 | 成都第一制药有限公司 | A kind of detection method of the Anisodamine in relation to substance |
| CN110095537A (en) * | 2019-04-25 | 2019-08-06 | 成都第一制药有限公司 | A kind of Anisodamine detection method of content |
| CN111358855A (en) * | 2020-03-31 | 2020-07-03 | 毕宏生 | Application of radix physochlainae extract in preparing medicine for preventing and treating myopia |
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