CN102507839A - Method for controlling quality of Su Geng capsules - Google Patents
Method for controlling quality of Su Geng capsules Download PDFInfo
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Abstract
The invention discloses a method for controlling quality of Su Geng capsules and a Su Geng preparation, and belongs to the technical field of medicines. According to the method, the current quality standard of the Su Geng capsules is improved correspondingly, and the identification of cardamun and agilawood, and the cardamun determination are adopted on the basis of the original standard; and the method is wide in controlling rang, and high in specificity, improves the quality standard of a product further, and guarantees the effectiveness, quality controllability and stability of a medicine.
Description
Technical field
The present invention relates to a kind of method of quality control of compound Chinese medicinal preparation, the method for quality control of particularly a kind of easypro more capsule and preparation thereof belongs to medical technical field.
Background technology
Easypro more capsule records in the national drug standards, and the standard numbering: WS-11010 (ZD-1010)-2002 is the representative medicines that are used for climacteric metancholia of women in the Tibetan medicine, has the regulation of qi and blood, the effect of calming the nerves.Be used for the emotional lability that climacteric metancholia of women causes, stress is had the fidgets, and is dizzy weak, insomnia.To irregular menstruation, gynecological disease effects such as leucorrhea increasing are good.Owing to obvious toxic-side effects evident in efficacy, no is selected in the OTC kind.
Yet; The existing easypro more quality inspection standard of capsule only comprises the discriminating of microscopical identification, eugenol; These two parts of the assay of cloves; The product quality and the curative effect of capsule seem backward and thin unable to above-mentioned control method for guaranteeing to relax more, can not effectively control the quality of other principal ingredients.Therefore, cause and relax that more the capsule product quality control is not accurate, quality standard has much room for improvement, need badly a cover more accurately, more comprehensive method of quality control.
Summary of the invention
To the deficiency of prior art, the purpose of this invention is to provide the method for quality control of a kind of easypro more capsule and preparation thereof.
Summary of the invention
The present invention has carried out corresponding raising to existing easypro more capsule quality standard; On the basis of primary standard, increased the discriminating of cardamom, agalloch eaglewood; Increased myristic assay; Chain of command is wider, specificity is stronger, has further promoted the quality standard of product, guarantees validity, quality controllability and the stability of this medicine.
The term explanation:
Relaxing more, capsule is the nomenclature of drug of national standard for traditional Chinese medicines compilation (Chinese patent drug provincial standard rising national standard part) record.
The capsule preparations that relaxes more comprises the capsule and with easypro more other preparations of capsule 's content formulation of relaxing more.
Technical scheme of the present invention is following:
A kind of bulk drug consists of the method for quality control that cardamom 188 weight portions, sealwort 32 weight portions, asparagus fern 32 weight portions, nutmeg 32 weight portions, agalloch eaglewood 32 weight portions, cloves 32 weight portions, hand are joined the relax capsule more and the preparation thereof of 32 weight portions, and this method comprises one or more in following discriminating and/or the content assaying method:
Differentiate:
A. the discriminating of cardamom
Get relax more capsule or its preparation content 2～6g, the 20-45mL that adds methylene chloride, sonicated 20-45min filters, and filtrates 30 ℃-60 ℃ and is concentrated into 3-8mL, as need testing solution; Other gets cardamom control medicinal material 2～6g, the 20-45mL that adds methylene chloride, and sonicated 20-45min filters, and filtrates 30 ℃-60 ℃ and is concentrated into 3-8mL, as control medicinal material solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5～15 μ L of above-mentioned 2 kinds of solution, put respectively on same silica gel g thin-layer plate; With the volume parts ratio is 5～10: 1.5～2.5: 0.5～1.5 xylene-ethyl acetate-methylene chloride is a developping agent; Launch, take out, dry; Spray is with bulking value portion rate 1-3% vanillic aldehyde ethanol solution of sulfuric acid, and 100 ℃-115 ℃ to be heated to the spot colour developing clear; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on show the spot of same color.
B. the discriminating of agalloch eaglewood
Get relax more capsule or its preparation content 1～5g, adding boiling range is 30～60 ℃ of sherwood oil 10ml, and sonicated 20-45min filters, and filtrating is concentrated into 2ml as need testing solution; Other gets agalloch eaglewood control medicinal material 1～5g, and adding boiling range is 60～90 ℃ of sherwood oil 10ml, and sonicated 20-45min filters, and filtrating is as control medicinal material solution; Test according to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B); Draw each 5-15 μ L of above-mentioned 2 kinds of solution; Putting respectively on same silica gel g thin-layer plate, is 5～10: 1.5～2.5 with the volume parts ratio: 0.5～1.5 xylene-ethyl formate-methenyl choloride is a developping agent, launches; Take out, dry; Spray is with bulking value portion rate 1-3% vanillic aldehyde ethanol solution of sulfuric acid, and 100 ℃-115 ℃ to be heated to the spot colour developing clear; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
Assay:
Measure according to high-efficient liquid phase technique (an appendix VI of Chinese Pharmacopoeia version in 2010 D);
Myristic assay
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; With volume parts than 60-80: 40-20 methyl alcohol-volume parts is a moving phase than 0.1% phosphate aqueous solution; The detection wavelength is 274nm; Number of theoretical plate calculates by dehydrogenation two isoeugenol peaks should be not less than 3000;
The preparation of reference substance solution: it is an amount of that precision takes by weighing dehydrogenation two isoeugenol reference substances, adds methyl alcohol and process the solution that every 1ml contains dehydrogenation two isoeugenol reference substance 20-50ug, promptly gets;
The preparation of need testing solution: behind easypro more capsule or its preparation porphyrize, get powder 6g, put in the conical flask of tool plug, add methyl alcohol 40-60ml, close plug; Claim decide weight, ultrasonic 20-50min is put coldly, and weight decided in title again, supplies the weight that subtracts mistake with methyl alcohol; Shake up, filter, get subsequent filtrate, promptly get;
Determination method: accurate respectively reference substance solution and each 10-15 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get.
Above-mentioned easypro more capsule and preparation thereof are made up of following bulk drugs:
Cardamom 188 weight portions, sealwort 32 weight portions, asparagus fern 32 weight portions, nutmeg 32 weight portions, agalloch eaglewood 32 weight portions, cloves 32 weight portions, hand are joined 32 weight portions.
Described preparation is meant gets the above-mentioned raw materials medicine, presses common process, adds conventional auxiliary material and is prepared into clinical acceptable any formulation.
Preferably, a kind of more method of quality control of capsule that relaxes, this method comprises one or more in following discriminating and/or the content assaying method:
Differentiate:
A. the discriminating of cardamom
Get the more capsule 's content 4g that relaxes, the 30mL that adds methylene chloride, sonicated 30min filters, and filtrates 50 ℃ and is concentrated into 5mL, as need testing solution; Other gets cardamom control medicinal material 2g, the 30mL that adds methylene chloride, and sonicated 30min filters, and filtrates 50 ℃ and is concentrated into 5mL, as control medicinal material solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5 μ L of above-mentioned 2 kinds of solution, put respectively on same silica gel g thin-layer plate; With the volume parts ratio is that 7: 2: 1 xylene-ethyl acetate-methylene chloride are developping agent; Launch, take out, dry; Spray is with bulking value portion rate 2% vanillic aldehyde ethanol solution of sulfuric acid, and 105 ℃ to be heated to the spot colour developing clear; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on show the spot of same color.
B. the discriminating of agalloch eaglewood
Get the more capsule 's content 3g that relaxes, add 30～60 ℃ of sherwood oil 10ml of boiling range, sonicated 30min filters, and filtrating is concentrated into 2ml as need testing solution; Other gets agalloch eaglewood control medicinal material 1g, adds 60～90 ℃ of sherwood oil 10ml of boiling range, and sonicated 30min filters, and filtrating is as control medicinal material solution; Test according to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B); Draw each 15 μ L of above-mentioned 2 kinds of solution; Putting respectively on same silica gel g thin-layer plate, is that 7: 2: 1 xylene-ethyl formate-methenyl cholorides are developping agent with the volume parts ratio, launches; Take out, dry; Spray is with bulking value portion rate 2% vanillic aldehyde ethanol solution of sulfuric acid, and 105 ℃ to be heated to the spot colour developing clear; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
Assay:
Measure according to high-efficient liquid phase technique (an appendix VI of Chinese Pharmacopoeia version in 2010 D);
Myristic assay
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; Is moving phase than 70: 30 methyl alcohol-volume parts than 0.1% phosphate aqueous solution with volume parts; The detection wavelength is 274nm; Number of theoretical plate calculates by dehydrogenation two isoeugenol peaks should be not less than 3000;
The preparation of reference substance solution: it is an amount of to take by weighing dehydrogenation two isoeugenol reference substances, adds methyl alcohol and processes the solution that every 1ml contains dehydrogenation two isoeugenol reference substance 30ug, promptly gets;
The preparation of need testing solution: behind the easypro more capsule 's content porphyrize, get powder 6g, put in the conical flask of tool plug, add methyl alcohol 50ml, close plug; Claim decide weight, ultrasonic 30min is put coldly, and weight decided in title again, supplies the weight that subtracts mistake with methyl alcohol; Shake up, filter, get subsequent filtrate, promptly get;
Determination method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get.
Wherein, the above-mentioned easypro more bulk drug of capsule consists of:
Cardamom 188 weight portions, sealwort 32 weight portions, asparagus fern 32 weight portions, nutmeg 32 weight portions, agalloch eaglewood 32 weight portions, cloves 32 weight portions, hand are joined 32 weight portions.
Above-mentioned easypro more capsule is prepared from following method:
More than seven the flavor, be ground into fine powder, mixing incapsulates, and promptly gets.
The relation of weight portion according to the invention and parts by volume is the relation of g/ml.
Relaxing only comprises the discriminating of microscopical identification, eugenol under the capsule proper mass normal term more, and these two parts of the assay of cloves can not effectively be controlled the quality of other principal ingredients.The present invention has increased the discriminating of cardamom, agalloch eaglewood on the basis of primary standard, increased myristic assay, and chain of command is wider, specificity is stronger, has further promoted the quality standard of product, guarantees validity, quality controllability and the stability of this medicine.
Following experimental example and embodiment are used to further specify but are not limited to the present invention.
Experimental example 1 identification experiment
1, the discriminating of cardamom
Get the more capsule 's content 2～6g that relaxes, the 30mL that adds methylene chloride, sonicated 30min filters, and filtrates 50 ℃ and is concentrated into 5mL, as need testing solution.Other gets cardamom control medicinal material 2g, the 30mL that adds methylene chloride, and sonicated 30min filters, and filtrates 50 ℃ and is concentrated into 5mL, as control medicinal material solution.Other gets the negative control medicinal material 4g in the scarce cardamom of prescription ratio preparation, and the preparation method processes negative control solution with need testing solution.According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5～15 μ L of above-mentioned 3 kinds of solution, put respectively on same silica gel g thin-layer plate; With the volume parts ratio is 5～10: 1.5～2.5: 0.5～1.5 xylene-ethyl acetate-methylene chloride is a developping agent; Launch, take out, dry; Spray is with bulking value portion rate 2% vanillic aldehyde ethanol solution of sulfuric acid, and 105 ℃ to be heated to the spot colour developing clear.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on show the spot of same color, negative noiseless.
Interpretation of result: cardamom TLC result shows, in volume ratio 5～10: have under xylene-ethyl acetate of 1.5～2.5: 0.5～1.5-methylene chloride condition and launch effect preferably.It is best under xylene-ethyl acetate of 7: 2: 1 of volume ratio-methylene chloride condition, to launch effect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color, negative noiseless.The method can be used as the discrimination method of cardamom in the easypro more capsule.
2, the discriminating of agalloch eaglewood
Get the more capsule 's content 1～5g that relaxes, add 30～60 ℃ of sherwood oil 10ml of boiling range, sonicated 30min filters, and filtrating is concentrated into 2ml, as need testing solution.Other gets agalloch eaglewood control medicinal material 1g, adds 60～90 ℃ of sherwood oil 10ml of boiling range, and sonicated 30min filters, and filtrating is as control medicinal material solution.Other gets the negative control medicinal material 2.5g in the scarce agalloch eaglewood of prescription ratio preparation, processes negative control solution with method.Test according to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B); Draw each 5～15 μ L of above-mentioned 3 kinds of solution; Putting respectively on same silica gel g thin-layer plate, is 5～10: 1.5～2.5 with the volume parts ratio: 0.5～1.5 xylene-ethyl formate-methenyl choloride is a developping agent, launches; Take out, dry.Spray is with bulking value portion rate 2% vanillic aldehyde ethanol solution of sulfuric acid, and 105 ℃ to be heated to the spot colour developing clear.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color, negative noiseless.
Interpretation of result: agalloch eaglewood TLC result shows, in volume ratio 5～10: have under xylene-ethyl formate of 1.5～2.5: 0.5～1.5-methenyl choloride condition and launch effect preferably.Expansion effect under xylene-ethyl formate of 7: 2: 1 of volume ratio-methenyl choloride condition is best.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color, negative noiseless.The method can be used as the discrimination method of agalloch eaglewood in the easypro more capsule.
Experimental example 2: assay experiment
1. instrument, reagent and confession test agent
Instrument: high performance liquid chromatograph: the L-2100 of Hitachi pump, the L-2400 of Hitachi detecting device; Tianjin, island AUW220D electronic balance
Reference substance: dehydrogenation two isoeugenol reference substances, lot number: 12045-20110641.
Sample: the more capsule (the Qinghai gold is scolded Tibetan medicine medicine company incorporated company) that relaxes, lot number: 090501,090502,090503
2. moving phase is selected
This law adopts toxicity less; And easy methyl alcohol is mobile with volume fraction than 0.1% phosphate aqueous solution mixed liquor; Control myristic content in its easypro more capsule; Through discovering that mobile methyl alcohol-0.1% phosphate aqueous solution is excellent with volume fraction than 60-80: 40-20, be optimum than 70: 30 wherein with volume parts.
3. reference substance preparation
It is an amount of to remove hydrogen two isoeugenol reference substances, and accurate the title decides, and adds methyl alcohol and processes the solution that every 1ml contains 30ug, promptly gets.
4. test sample preparation
Relax more behind the capsule 's content porphyrize, get powder 6g, accurately claim surely, put in the conical flask of tool plug, the accurate methyl alcohol 50ml that adds, close plug is claimed decide weight, and ultrasonic 30min is put coldly, supplies the weight that subtracts mistake with methyl alcohol, shakes up, and subsequent filtrate is got in filtration, promptly gets.
5. system suitability test and the negative investigation of disturbing
Under above-mentioned chromatographic condition, accurate respectively each the 10 μ l of reference substance solution, need testing solution and negative control solution that draw inject liquid chromatograph, the record chromatogram.The result shows that the degree of separation that dehydrogenation two isoeugenols are adjacent chromatographic peak in the test sample chromatogram is greater than 1.5, and negative control is noiseless.See Fig. 1, Fig. 2, Fig. 3.
6. linear test
Precision is measured dehydrogenation two isoeugenol reference substance stock solution solution (58.0ug/ml) 1ml, 3ml, 5ml, 8ml, 10ml; Put respectively in the 10ml volumetric flask, methyl alcohol is diluted to scale, shakes up; Each accurate sample introduction 10 μ l carries out linear regression with peak area (A) to reference substance concentration (C).The result shows: in 5.8ug/ml～58.0ug/ml scope, the peak area (A) of dehydrogenation two isoeugenols is good with concentration (C) linear relationship.See table 1, Fig. 4.
Table 1 dehydrogenation two isoeugenol linear test results
| Sequence number | Concentration (ug/ml) | Peak area (A) |
| 1 | 5.8 | 114422 |
| 2 | 17.4 | 349253 |
| 3 | 29.0 | 579728 |
| 4 | 40.6 | 800954 |
| 5 | 58.0 | 1004241 |
Linear equation: A=19236C+11885, related coefficient: R=0.9996.
7. precision test
The accurate respectively dehydrogenation two isoeugenol reference substance solution 10 μ l that draw inject liquid chromatograph, each METHOD FOR CONTINUOUS DETERMINATION 6 times, and the record peak area also calculates relative standard deviation, RSD=0.690%.The result shows that instrument precision is good.See table 2.
Table 2 dehydrogenation two isoeugenol Precision test result
8. stability test
After the need testing solution preparation was accomplished, the accurate 10 μ l that draw injected liquid chromatograph, and the record peak area was whenever measured once at a distance from 2 hours later on, investigated 8 hours, calculated the relative standard deviation of peak area, RSD=0.440%.The result shows: in 8 hours, to measure the result stable for dehydrogenation two isoeugenols in the test sample.
The stability test result of table 3 dehydrogenation two isoeugenols
9. replica test
These article of getting, replication 6 times, the content of dehydrogenation two isoeugenols in the calculation sample, RSD=0.424%.Show that analytical approach repeatability is good.
Table 4 dehydrogenation two isoeugenol replica test results
10. recovery test
Precision takes by weighing 6 parts of same lot sample article, and the accurate dehydrogenation two isoeugenol reference substances that add are measured its content, calculate recovery rate, and the result is following.Dehydrogenation two isoeugenol average recovery rates are 99.26%, RSD=1.15%.It is accurate to show that this assay method is measured the result.
Table 5 dehydrogenation two isoeugenol recovery test results
11. sample determination
Measure the content of dehydrogenation two isoeugenols in three batches of easypro more capsules, the result is following:
Table 6 sample size is measured the result
| Lot number | Content (mg/ grain) |
| 090501 | 0.518 |
| 090502 | 0.503 |
| 090503 | 0.487 |
Following embodiment all can realize the described effect of above-mentioned experimental example.
Description of drawings:
Fig. 1 is dehydrogenation two an isoeugenols contrast liquid phase collection of illustrative plates; Fig. 2 is the more capsule sample liquid phase collection of illustrative plates that relaxes; Fig. 3 is the more capsule negative controls phase collection of illustrative plates that relaxes; Wherein, the horizontal ordinate of Fig. 1-3 is the time, unit: minute (Minutes); Ordinate is a voltage, unit: volt (Volts);
Fig. 4 is dehydrogenation two isoeugenol canonical plottings.
Embodiment
Below in conjunction with embodiment the present invention is done detailed elaboration, but be not limited to the embodiment of these concrete records.The easypro more capsule that is detected is scolded Tibetan medicine medicine company incorporated company for the Qinghai gold and is produced.
Embodiment 1: the more method of quality control of capsule relaxes
A. the discriminating of cardamom
Get the more capsule 's content 4g that relaxes, the 30mL that adds methylene chloride, sonicated 30min filters, and filtrates 50 ℃ and is concentrated into 5mL, as need testing solution; Other gets cardamom control medicinal material 2g, the 30mL that adds methylene chloride, and sonicated 30min filters, and filtrates 50 ℃ and is concentrated into 5mL, as control medicinal material solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5 μ L of above-mentioned 2 kinds of solution, put respectively on same silica gel g thin-layer plate; With the volume parts ratio is that 7: 2: 1 xylene-ethyl acetate-methylene chloride are developping agent; Launch, take out, dry; Spray is with bulking value portion rate 2% vanillic aldehyde ethanol solution of sulfuric acid, and 105 ℃ to be heated to the spot colour developing clear; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on show the spot of same color.
B. the discriminating of agalloch eaglewood
Get the more capsule 's content 3g that relaxes, add 30～60 ℃ of sherwood oil 10ml of boiling range, sonicated 30min filters, and filtrating is concentrated into 2ml as need testing solution; Other gets agalloch eaglewood control medicinal material 1g, adds 60～90 ℃ of sherwood oil 10ml of boiling range, and sonicated 30min filters, and filtrating is as control medicinal material solution; Test according to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B); Draw each 15 μ L of above-mentioned 2 kinds of solution; Putting respectively on same silica gel g thin-layer plate, is that 7: 2: 1 xylene-ethyl formate-methenyl cholorides are developping agent with the volume parts ratio, launches; Take out, dry; Spray is with bulking value portion rate 2% vanillic aldehyde ethanol solution of sulfuric acid, and 105 ℃ to be heated to the spot colour developing clear; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
Assay:
Measure according to high-efficient liquid phase technique (an appendix VI of Chinese Pharmacopoeia version in 2010 D);
Myristic assay
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; Is moving phase than 70: 30 methyl alcohol-volume parts than 0.1% phosphate aqueous solution with volume parts; The detection wavelength is 274nm; Number of theoretical plate calculates by dehydrogenation two isoeugenol peaks should be not less than 3000;
The preparation of reference substance solution: it is an amount of to take by weighing dehydrogenation two isoeugenol reference substances, adds methyl alcohol and processes the solution that every 1ml contains dehydrogenation two isoeugenol reference substance 30ug, promptly gets;
The preparation of need testing solution: behind the capsule porphyrize that relaxes more, get powder 6g, put in the conical flask of tool plug, add methyl alcohol 50ml, close plug is claimed decide weight, and ultrasonic 30min is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with methyl alcohol, shakes up, and subsequent filtrate is got in filtration, promptly gets;
Determination method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get.
Embodiment 2: the method for quality control of capsule for treating climacteric syndrome agent
Differentiate:
A. the discriminating of cardamom
Get capsule for treating climacteric syndrome agent content 6g, the 45mL that adds methylene chloride, sonicated 45min filters, and filtrates 60 ℃ and is concentrated into 8mL, as need testing solution; Other gets cardamom control medicinal material 2g, the 45mL that adds methylene chloride, and sonicated 45min filters, and filtrates 60 ℃ and is concentrated into 8mL, as control medicinal material solution; According to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B) test, draw each 5 μ L of above-mentioned 2 kinds of solution, put respectively on same silica gel g thin-layer plate; With the volume parts ratio is that 10: 2.5: 0.5 xylene-ethyl acetate-methylene chloride are developping agent; Launch, take out, dry; Spray is with bulking value portion rate 1% vanillic aldehyde ethanol solution of sulfuric acid, and 105 ℃ to be heated to the spot colour developing clear; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on show the spot of same color.
B. the discriminating of agalloch eaglewood
Get capsule for treating climacteric syndrome agent content 5g, add 30～60 ℃ of sherwood oil 10ml of boiling range, sonicated 20min filters, and filtrating is concentrated into 2ml as need testing solution; Other gets agalloch eaglewood control medicinal material 5g, adds 60～90 ℃ of sherwood oil 10ml of boiling range, and sonicated 20min filters, and filtrating is as control medicinal material solution; Test according to thin-layered chromatography (an appendix VI of Pharmacopoeia of the People's Republic of China version in 2010 B); Draw each 10 μ L of above-mentioned 2 kinds of solution; Putting respectively on same silica gel g thin-layer plate, is that 8: 2.5: 0.5 xylene-ethyl formate-methenyl cholorides are developping agent with the volume parts ratio, launches; Take out, dry; Spray is with bulking value portion rate 2% vanillic aldehyde ethanol solution of sulfuric acid, and 100 ℃ to be heated to the spot colour developing clear; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
Assay:
Measure according to high-efficient liquid phase technique (an appendix VI of Chinese Pharmacopoeia version in 2010 D);
Myristic assay
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; Is moving phase than 75: 25 methyl alcohol-volume parts than 0.1% phosphate aqueous solution with volume parts; The detection wavelength is 274nm; Number of theoretical plate calculates by dehydrogenation two isoeugenol peaks should be not less than 3000;
The preparation of reference substance solution: it is an amount of that precision takes by weighing dehydrogenation two isoeugenol reference substances, adds methyl alcohol and process the solution that every 1ml contains dehydrogenation two isoeugenol reference substance 45ug, promptly gets;
The preparation of need testing solution: behind the capsule for treating climacteric syndrome agent porphyrize, get powder 6g, put in the conical flask of tool plug, add methyl alcohol 60ml, close plug; Claim decide weight, ultrasonic 50min is put coldly, and weight decided in title again, supplies the weight that subtracts mistake with methyl alcohol; Shake up, filter, get subsequent filtrate, promptly get;
Determination method: accurate respectively reference substance solution and each 15 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get.
Described capsule for treating climacteric syndrome agent is joined 32 weight portions by cardamom 188 weight portions, sealwort 32 weight portions, asparagus fern 32 weight portions, nutmeg 32 weight portions, agalloch eaglewood 32 weight portions, cloves 32 weight portions, hand, adds conventional auxiliary material, is prepared into granule according to conventional method.
Claims (3)
1. a bulk drug consists of the method for quality control that cardamom 188 weight portions, sealwort 32 weight portions, asparagus fern 32 weight portions, nutmeg 32 weight portions, agalloch eaglewood 32 weight portions, cloves 32 weight portions, hand are joined the relax capsule more and the preparation thereof of 32 weight portions; It is characterized in that this method comprises one or more in following discriminating and/or the content assaying method:
Differentiate:
A. the discriminating of cardamom
Get relax more capsule or its preparation content 2～6g, the 20-45mL that adds methylene chloride, sonicated 20-45min filters, and filtrates 30 ℃-60 ℃ and is concentrated into 3-8mL, as need testing solution; Other gets cardamom control medicinal material 2～6g, the 20-45mL that adds methylene chloride, and sonicated 20-45min filters, and filtrates 30 ℃-60 ℃ and is concentrated into 3-8mL, as control medicinal material solution; According to an appendix VI of thin-layered chromatography Pharmacopoeia of the People's Republic of China version in 2010 B test, draw each 5～15 μ L of above-mentioned 2 kinds of solution, put respectively on same silica gel g thin-layer plate; With the volume parts ratio is 5～10: 1.5～2.5: 0.5～1.5 xylene-ethyl acetate-methylene chloride is a developping agent; Launch, take out, dry; Spray is with bulking value portion rate 1-3% vanillic aldehyde ethanol solution of sulfuric acid, and 100 ℃-115 ℃ to be heated to the spot colour developing clear; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on show the spot of same color;
B. the discriminating of agalloch eaglewood
Get relax more capsule or its preparation content 1～5g, adding boiling range is 30～60 ℃ of sherwood oil 10ml, and sonicated 20-45min filters, and filtrating is concentrated into 2ml as need testing solution; Other gets agalloch eaglewood control medicinal material 1～5g, and adding boiling range is 60～90 ℃ of sherwood oil 10ml, and sonicated 20-45min filters, and filtrating is as control medicinal material solution; Test according to an appendix VI of thin-layered chromatography Pharmacopoeia of the People's Republic of China version in 2010 B; Draw each 5-15 μ L of above-mentioned 2 kinds of solution; Putting respectively on same silica gel g thin-layer plate, is 5～10: 1.5～2.5 with the volume parts ratio: 0.5～1.5 xylene-ethyl formate-methenyl choloride is a developping agent, launches; Take out, dry; Spray is with bulking value portion rate 1-3% vanillic aldehyde ethanol solution of sulfuric acid, and 100 ℃-115 ℃ to be heated to the spot colour developing clear; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
Assay:
Measure according to high-efficient liquid phase technique (an appendix VI of Chinese Pharmacopoeia version in 2010 D);
Myristic assay
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; With volume parts than 60-80: 40-20 methyl alcohol-volume parts is a moving phase than 0.1% phosphate aqueous solution; The detection wavelength is 274nm; Number of theoretical plate calculates by dehydrogenation two isoeugenol peaks should be not less than 3000;
The preparation of reference substance solution: it is an amount of that precision takes by weighing dehydrogenation two isoeugenol reference substances, adds methyl alcohol and process the solution that every 1ml contains dehydrogenation two isoeugenol reference substance 20-50ug, promptly gets;
The preparation of need testing solution: behind easypro more capsule or its preparation porphyrize, get powder 6g, put in the conical flask of tool plug, add methyl alcohol 40-60ml, close plug; Claim decide weight, ultrasonic 20-50min is put coldly, and weight decided in title again, supplies the weight that subtracts mistake with methyl alcohol; Shake up, filter, get subsequent filtrate, promptly get;
Determination method: accurate respectively reference substance solution and each 10-15 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get.
2. the method for quality control of relax capsule more and preparation thereof as claimed in claim 1, the wherein said preparation that relaxes more are meant bulk drug and add conventional auxiliary material and to be prepared into clinical acceptable any formulation by common process.
3. according to claim 1 or claim 2 the method for quality control of relax capsule more and preparation thereof is characterized in that this method comprises one or more in following discriminating and/or the content assaying method:
Differentiate:
A. the discriminating of cardamom
Get the more capsule 's content 4g that relaxes, the 30mL that adds methylene chloride, sonicated 30min filters, and filtrates 50 ℃ and is concentrated into 5mL, as need testing solution; Other gets cardamom control medicinal material 2g, the 30mL that adds methylene chloride, and sonicated 30min filters, and filtrates 50 ℃ and is concentrated into 5mL, as control medicinal material solution; According to an appendix VI of thin-layered chromatography Pharmacopoeia of the People's Republic of China version in 2010 B test, draw each 5 μ L of above-mentioned 2 kinds of solution, put respectively on same silica gel g thin-layer plate; With the volume parts ratio is that 7: 2: 1 xylene-ethyl acetate-methylene chloride are developping agent; Launch, take out, dry; Spray is with bulking value portion rate 2% vanillic aldehyde ethanol solution of sulfuric acid, and 105 ℃ to be heated to the spot colour developing clear; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on show the spot of same color;
B. the discriminating of agalloch eaglewood
Get the more capsule 's content 3g that relaxes, add 30～60 ℃ of sherwood oil 10ml of boiling range, sonicated 30min filters, and filtrating is concentrated into 2ml as need testing solution; Other gets agalloch eaglewood control medicinal material 1g, adds 60～90 ℃ of sherwood oil 10ml of boiling range, and sonicated 30min filters, and filtrating is as control medicinal material solution; According to an appendix VI of thin-layered chromatography Pharmacopoeia of the People's Republic of China version in 2010 B test, draw each 15 μ L of above-mentioned 2 kinds of solution, put respectively on same silica gel g thin-layer plate; With the volume parts ratio is that 7: 2: 1 xylene-ethyl formate-methenyl cholorides are developping agent; Launch, take out, dry; Spray is with bulking value portion rate 2% vanillic aldehyde ethanol solution of sulfuric acid, and 105 ℃ to be heated to the spot colour developing clear; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
Assay:
Measure according to high-efficient liquid phase technique (an appendix VI of Chinese Pharmacopoeia version in 2010 D);
Myristic assay
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; Is moving phase than 70: 30 methyl alcohol-volume parts than 0.1% phosphate aqueous solution with volume parts; The detection wavelength is 274nm; Number of theoretical plate calculates by dehydrogenation two isoeugenol peaks should be not less than 3000;
The preparation of reference substance solution: it is an amount of to take by weighing dehydrogenation two isoeugenol reference substances, adds methyl alcohol and processes the solution that every 1ml contains dehydrogenation two isoeugenol reference substance 30ug, promptly gets;
The preparation of need testing solution: behind the easypro more capsule 's content porphyrize, get powder 6g, put in the conical flask of tool plug, add methyl alcohol 50ml, close plug; Claim decide weight, ultrasonic 30min is put coldly, and weight decided in title again, supplies the weight that subtracts mistake with methyl alcohol; Shake up, filter, get subsequent filtrate, promptly get;
Determination method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get.
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| CN109541116A (en) * | 2018-11-23 | 2019-03-29 | 北京三和药业有限公司 | A kind of discrimination method of agalloch eaglewood |
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