CN101632741A - Quality control method for Jian'er Qingjie liquid - Google Patents
Quality control method for Jian'er Qingjie liquid Download PDFInfo
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Abstract
The invention discloses a quality control method for Jian'er Qingjie liquid. Through the thin-layer qualitative identification of hawthorn fruits and tangerine peel, the specificity of the quality control method is enhanced, and the method can accurately reflect the quality of medicaments so as to ensure the safety and effectiveness of medicaments, improve product quality and facilitate the standardized production of the medicaments.
Description
Technical field
The present invention relates to a kind of method of quality control of Jian ' er Qingjie liquid, belong to technical field of Chinese medicines.
Background technology
Jian ' er Qingjie liquid has heat-clearing and toxic substances removing, the effect of the stagnant stomach function regulating that disappears.Be used to the pharyngalgia of coughing, inappetence, distension and fullness in the abdomen is the clinical common drug of department of pediatrics.The 10th 148 pages of national standards " Chinese traditional patent formulation preparation ", standard No. is WS3-B-2015-95, has recorded prescription, method for making and the method for quality control of said preparation.
The prescription of said preparation:
Flos Lonicerae 110g Flos Chrysanthemi 100g Fructus Forsythiae 65g
Fructus Crataegi 50g Semen Armeniacae Amarum 50g Pericarpium Citri Reticulatae 2.5g
The preparation method of said preparation is: above Six-element, and Flos Lonicerae, Flos Chrysanthemi, Fructus Forsythiae, Semen Armeniacae Amarum be the distillation extraction Aromatic water respectively, and Fructus Crataegi is with 80% ethanol heating extraction secondary, each 2 hours, filter merging filtrate, filtrate recycling ethanol is condensed into extractum, adds an amount of water dissolution; Pericarpium Citri Reticulatae carries out percolation with 60% ethanol as solvent according to the percolation (appendix IO of Chinese Pharmacopoeia version in 2005) under the fluid extract item, collects percolate, reclaims ethanol, and the water dilution with an amount of filters; Merge above-mentioned medicinal liquid and Aromatic water, adding citric acid 0.05g, simple syrup 300ml and benzoic acid are an amount of, add water and make into 1000ml, stir evenly, and filter, promptly.
The method of quality control of said preparation is:
(1) get this product 6ml, put in the test tube, hang a trinitrophenol reagent paper in the pipe, reuse cork jam-pack is put in 40～50 ℃ of water-baths, and reagent paper shows brick-red after 5 minutes.
(2) get the about 2ml of this product, put in the separatory funnel, add petroleum ether (60～90 ℃) 10ml, jolting 10 minutes is placed, and divides and gets petroleum ether layer, puts evaporate to dryness in the water-bath, and residue adds 2～3 of 5% vanillin sulfuric acid solutions, and displaing amaranth is placed color burn.
This method of quality control has only carried out chemical discriminating to the composition of said preparation, the method specificity is not strong, be unfavorable in pharmaceutical production, product being carried out quality control, can not effectively supervise the quality of this product on the market, it is safe and effective to guarantee that clinical drug is used, the standardized production that is unfavorable for medicine does not meet the trend that modern Chinese medicine develops yet.
Summary of the invention
The purpose of this invention is to provide and a kind of described Jian ' er Qingjie liquid is carried out the method for quality control,, improve the quality of products, be convenient to standardization, the modern production of medicine to guarantee the safety and the effectiveness of medicine.
In order to achieve the above object, the invention provides a kind of method of quality control of Jian ' er Qingjie liquid, this method comprises a kind of in two kinds of detections of following a, b at least:
A. get Jian ' er Qingjie liquid, put in the separatory funnel, extract with the ether jolting, ether solution evaporate to dryness, residue add diethyl ether 2ml as need testing solution.Other gets the Fructus Crataegi control medicinal material, adds 80% ethanol supersound process, filters, and filtrate evaporate to dryness, residue add water makes dissolving, extracts with the ether jolting, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw above-mentioned two kinds of solution, put respectively on same polyamide film, with butanone-ethyl acetate-formic acid-water is developing solvent, launches, and takes out, dry, spray is with 2% aluminum chloride test solution, and 105 ℃ were heated 1 minute, and putting wavelength is to inspect under the 365nm ultra-violet lamp.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
B. get Jian ' er Qingjie liquid, put in the separatory funnel, extract with the ethyl acetate jolting, extracting solution low temperature evaporate to dryness, residue add methanol 2ml as need testing solution, and other gets the Pericarpium Citri Reticulatae control medicinal material, adds the methanol supersound process, gets supernatant medical material solution in contrast.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw need testing solution, control medicinal material solution, putting respectively on same silica gel g thin-layer plate, is developing solvent with butyl acetate-methanol-formic acid, launches, take out, dry, spray is with vanillin sulphuric acid test solution, and 105 ℃ to be heated to speckle colour developing clear.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Preferably, this method of quality control comprises a kind of in two kinds of detections of following a, b at least:
A. get Jian ' er Qingjie liquid 30ml, put in the separatory funnel, extract 2 times with the ether jolting, each 30ml merges ether solution, and ether solution evaporate to dryness, residue add diethyl ether 2ml as need testing solution.Other gets Fructus Crataegi control medicinal material 2g, adds 80% ethanol 20ml supersound process 20 minutes, filters, and filtrate evaporate to dryness, residue add water 20ml makes dissolving, extracts 2 times with the ether jolting, and each 30ml shines medical material solution in pairs with legal system.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, (4: 4: 2: 1) be developing solvent, expansion was taken out with butanone-ethyl acetate-formic acid-water, dry, spray is with 2% aluminum chloride test solution, and 105 ℃ were heated 1 minute, and 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 same color;
B. get Jian ' er Qingjie liquid 10ml, put in the separatory funnel, extract twice with the ethyl acetate jolting, each 15 milliliters, combined ethyl acetate liquid, extracting solution low temperature evaporate to dryness, residue adds methanol 2ml as need testing solution, other gets Pericarpium Citri Reticulatae control medicinal material 0.5g, adds methanol 10ml supersound process 10 minutes, gets supernatant medical material solution in contrast.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw need testing solution 5 μ l, control medicinal material solution 3 μ l, putting respectively on same silica gel g thin-layer plate, is developing solvent with butyl acetate-methanol-formic acid (6: 4: 0.5), launches, take out, dry, spray is with vanillin sulphuric acid test solution, and 105 ℃ to be heated to speckle colour developing clear.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Preferably, this method of quality control can also comprise a kind of in two kinds of detections of following c, d:
C. get Jian ' er Qingjie liquid 6ml, put in the test tube, hang a trinitrophenol reagent paper in the pipe, reuse cork jam-pack is put in 40～50 ℃ of water-baths, and reagent paper shows brick-red after 5 minutes.
D. get Jian ' er Qingjie liquid 2ml, put in the separatory funnel, add petroleum ether (60～90 ℃) 10ml, jolting 10 minutes is placed, and divides and gets petroleum ether layer, puts evaporate to dryness in the water-bath, and residue adds 2～3 of 5% vanillin sulfuric acid solutions, and displaing amaranth is placed color burn.
This detection method adopts thin layer chromatography that Jian ' er Qingjie liquid is carried out quality control, and specificity is strong, can effectively control this drug quality, guarantees the safety and the effectiveness of this medicine.
The specific embodiment
Following experimental example and embodiment further specify but are not limited to the present invention.
The qualitative detection of experimental example 1 Pericarpium Citri Reticulatae
1. the investigation of control medicinal material processing method:
Method a. gets Pericarpium Citri Reticulatae control medicinal material 0.5g, adds methanol 5ml, and supersound process 15 minutes filters, and filtrate is medical material solution in contrast.
Method b. gets Pericarpium Citri Reticulatae control medicinal material 0.5g, adds ethyl acetate 20ml, and reflux 1 hour filters, and filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, in contrast medical material solution.
Method c. gets Pericarpium Citri Reticulatae control medicinal material 0.5g, adds methanol 20ml, and reflux 1 hour filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.
Method d. gets Pericarpium Citri Reticulatae control medicinal material 0.5g, adds methanol 10ml supersound process 10 minutes, gets supernatant medical material solution in contrast.
Other gets the Hesperidin reference substance, adds methanol and makes the solution that every 1ml contains 0.2mg, in contrast product solution.Draw each 3 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (60～90 ℃)-acetone (9: 4) is developing solvent, launches, and takes out, dry, spray is with vanillin sulphuric acid test solution, and 105 ℃ of heating are in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, colour developing the results are shown in following table.
| Method | Method a | Method b | Method c | Method d |
| The result | Control medicinal material chromatograph speckle is less, and reference substance chromatograph speckle is very shallow | Control medicinal material chromatograph speckle is less, and reference substance chromatograph speckle is more shallow | The control medicinal material chromatograph shows the fluorescence speckle of same color in reference substance chromatograph relevant position, but speckle is very shallow | Speckle separates better, and it is clear to develop the color, and the control medicinal material chromatograph shows the fluorescence speckle of same color in reference substance chromatograph relevant position. |
By above experiment, discover method d is as the processing method of control medicinal material in this detection method, and sensitivity is higher, is easy to detected composition is extracted.
2. the investigation of pharmaceutical composition sample treatment of the present invention:
Method a. gets this product 10ml, extracts 2 times with the ethyl acetate jolting, each 15ml, and combined ethyl acetate liquid, evaporate to dryness, residue add ethyl acetate 2ml makes dissolving, as need testing solution.
Method b. gets this product 10ml, extracts 2 times with the ether jolting, and each 15ml merges ether, and evaporate to dryness, the residue 2ml that adds diethyl ether makes dissolving, as need testing solution.
Method c. gets this product 10ml, extracts 2 times with the n-butyl alcohol jolting, and each 15ml merges n-butyl alcohol liquid, and evaporate to dryness, residue add n-butyl alcohol 2ml makes dissolving, as need testing solution.
Get Pericarpium Citri Reticulatae control medicinal material 0.5g, add methanol 10ml supersound process 10 minutes, get supernatant medical material solution in contrast.Draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (60～90 ℃)-acetone (9: 4) is developing solvent, launches, and takes out, dry, spray is with vanillin sulphuric acid test solution, and 105 ℃ of heating are in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, colour developing the results are shown in following table.
| Method | Method a | Method b | Method c |
| The result | Speckle separates better, and it is clear develop the color, sample chromatogram with the fluorescence speckle of the apparent same color in control medicinal material chromatograph relevant position. | Sample chromatogram shows the fluorescence speckle of same color in control medicinal material chromatograph relevant position, but speckle is very shallow | Sample chromatogram speckle number is less than the control medicinal material spot and counts |
By above experiment, discover method a is as the processing method of sample in this detection method, and sensitivity is higher, is easy to detected composition is all extracted.
3. developing solvent consumption proportion preferred in this detection method:
Get each 2 μ l of above-mentioned need testing solution a, control medicinal material solution d, put respectively on same silica gel g thin-layer plate, launch with the developing solvent of following ratio respectively: (20: 10: 1: upper strata 1) was molten, butyl acetate-methanol-formic acid (6: 4: 0.5), chloroform-acetone-methanol (5: 1: 1), normal hexane-ethyl acetate (2: 3), petroleum ether (60～90 ℃)-acetone (9: 4) launch for toluene-ethyl acetate-formic acid-water, take out, dry, spray is with vanillin sulphuric acid test solution, 105 ℃ of heating.The results are shown in Table 2
Table 2 developing solvent optimization experiment result
| The developing solvent proportioning | Toluene-ethyl acetate-formic acid-water (20: 10: 1: upper strata 1) is molten, | Chloroform-acetone-methanol (5: 1: 1) | Normal hexane-ethyl acetate (2: 3) | Butyl acetate-methanol-formic acid (6: 4: 0.5) | Petroleum ether (60～90 ℃)-acetone (9: 4) |
| Launch effect | Separate badly, holder tail phenomenon is arranged | Separate badly, holder tail phenomenon is arranged | Principal spot separates bad | Clear spot separates better | Speckle is visible to be separated better |
When developing solvent was butyl acetate-methanol-formic acid (6: 4: 0.5) as can be seen from Table 2, it is best that need testing solution launches effect, and appearance hangover, principal spot separate phenomenons such as bad.
4. sample solution point sample amount preferred in this detection method:
Getting need testing solution each 0.5 μ l, 1.0 μ l, 3.0 μ l, 5.0 μ l, 7.0 μ l respectively, put on same silica gel g thin-layer plate, is developing solvent with butyl acetate-methanol-formic acid (6: 4: 0.5), launch, take out, dry, spray is with vanillin sulphuric acid test solution, 105 ℃ of heating.With the corresponding position of control medicinal material chromatograph on, speckle colour developing situation sees Table 3:
Table 3 sample solution point sample amount optimization experiment result
| The point sample amount | ??0.5μl | ??1.0μl | ??3.0μl | ??5.0μl | ??7.0μl |
| Effect | Test sample is at corresponding reference substance position immaculate | Test sample is very shallow in the colour developing of corresponding reference substance position speckle | Test sample is more shallow in the colour developing of corresponding reference substance position speckle | Test sample is clear in the colour developing of corresponding reference substance position speckle | Test sample separates bad at corresponding reference substance position speckle |
Test sample point sample amount is when 5.0 μ l as can be seen from Table 3, and color developing effect is better on lamellae, is fit to test requirements document.
In sum, the qualitative checking method of Pericarpium Citri Reticulatae is in the preparation of the present invention: get oral liquid 10ml of the present invention, put in the separatory funnel, extract twice with the ethyl acetate jolting, each 15 milliliters, combined ethyl acetate liquid, extracting solution low temperature evaporate to dryness, residue add methanol 2ml as need testing solution, and other gets Pericarpium Citri Reticulatae control medicinal material 0.5g, add methanol 10ml supersound process 10 minutes, get supernatant medical material solution in contrast.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw need testing solution 5 μ l, control medicinal material solution 3 μ l, putting respectively on same silica gel g thin-layer plate, is developing solvent with butyl acetate-methanol-formic acid (6: 4: 0.5), launches, take out, dry, spray is with vanillin sulphuric acid test solution, and 105 ℃ to be heated to speckle colour developing clear.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
The qualitative detection of experimental example 2 Fructus Crataegis
1. the investigation of control medicinal material processing method:
Method a. gets Fructus Crataegi control medicinal material 2g, the 30ml that adds diethyl ether, and supersound process 15 minutes filters, and filtrate volatilizes, and residue adds dehydrated alcohol 1ml makes dissolving, in contrast medical material solution.
Method b. gets Fructus Crataegi control medicinal material 2g, adds water 100ml, decocts 1 hour, filters, filtrate is concentrated into 20ml, regulates pH value to 1 ~ 2 with dilute hydrochloric acid, extracts 2 times with the ethyl acetate jolting, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.
Method c. gets Fructus Crataegi control medicinal material 2g, the 40ml that adds diethyl ether, and heating and refluxing extraction 2 hours, extracting solution low temperature volatilizes, and residue adds dehydrated alcohol 1ml makes dissolving, in contrast medical material solution.
Method d. gets Fructus Crataegi control medicinal material 2g, adds 80% ethanol 20ml supersound process 20 minutes, filters the filtrate evaporate to dryness, residue adds water 20ml makes dissolving, extracts 2 times with the ether jolting, each 30ml, merge ether solution, ether solution evaporate to dryness, the residue 2ml medical material solution in contrast that adds diethyl ether.
Other gets the ursolic acid reference substance, adds dehydrated alcohol and makes the solution that every 1ml contains 0.5mg, in contrast product solution.Draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, with butanone-ethyl acetate-formic acid-water (4: 4: 2: 1) be developing solvent, launch, take out, dry, spray is with 2% aluminum chloride test solution, and 105 ℃ were heated 1 minute, and put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, colour developing the results are shown in following table.
| Method | Method a | Method b | Method c | Method d |
| The result | Reference substance chromatograph speckle is very shallow | Reference substance chromatograph speckle is more shallow | The control medicinal material chromatograph does not show the fluorescence speckle of same color in reference substance chromatograph relevant position | The control medicinal material chromatograph shows the fluorescence speckle of same color, clear spot in reference substance chromatograph relevant position |
By above experiment, discover method d is as the processing method of control medicinal material in this detection method, and sensitivity is higher, is easy to detected composition is extracted.
2. the investigation of pharmaceutical composition sample treatment of the present invention:
Method a. gets this product 30ml, puts in the separatory funnel, extracts 2 times with the ethyl acetate jolting, each 30ml, and combined ethyl acetate liquid, acetic acid ethyl fluid evaporate to dryness, residue add ethyl acetate 2ml as need testing solution.
Method b. gets this product 30ml, puts in the separatory funnel, extracts 2 times with the ether jolting, and each 30ml merges ether solution, and ether solution evaporate to dryness, residue add diethyl ether 2ml as need testing solution.
Method c. gets this product 30ml, puts in the separatory funnel, extracts 2 times with the n-butyl alcohol jolting, and each 30ml merges n-butyl alcohol liquid, and n-butyl alcohol liquid evaporate to dryness, residue add n-butyl alcohol 2ml as need testing solution.
Get Fructus Crataegi control medicinal material 2g, add 80% ethanol 20ml supersound process 20 minutes, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, extracts 2 times with the ether jolting, and each 30ml merges ether solution, ether solution evaporate to dryness, the residue 2ml medical material solution in contrast that adds diethyl ether.
Draw above-mentioned need testing solution, each 5 μ l of control medicinal material solution, put respectively on same polyamide film, with butanone-ethyl acetate-formic acid-water (4: 4: 2: 1) be developing solvent, launch, take out, dry, spray is with 2% aluminum chloride test solution, 105 ℃ were heated 1 minute, and put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, colour developing the results are shown in following table.
| Method | Method a | Method b | Method c |
| The result | Sample chromatogram shows the fluorescence speckle of same color in control medicinal material chromatograph relevant position, but speckle is unintelligible | Speckle separates better, and it is clear to develop the color, and sample chromatogram is showing the glimmering of same color with control medicinal material chromatograph relevant position | Sample chromatogram speckle number is less than the control medicinal material spot counts, and very slight color |
| The hot spot point. |
By above experiment, discover method b is as the processing method of sample in this detection method, and sensitivity is higher, is easy to detected composition is all extracted.
3. developing solvent consumption proportion preferred in this detection method:
Get each 5 μ l of above-mentioned need testing solution b, control medicinal material solution d, put respectively on same polyamide film, 1), toluene-ethyl acetate-formic acid (20: 4: 0.5), chloroform-acetone (9: 1), cyclohexane extraction-chloroform-ethyl acetate (20: 5: 8), cyclohexane extraction-ethyl acetate-formic acid (20: 20: 1) launch launches with the developing solvent of following ratio respectively: butanone-ethyl acetate-formic acid-water (4: 4: 2:, take out, dry, spray is with 2% aluminum chloride test solution, 105 ℃ were heated 1 minute, and put under the ultra-violet lamp (365nm) and inspect.The results are shown in Table 2
Table 2 developing solvent optimization experiment result
| The developing solvent proportioning | Butanone-ethyl acetate-formic acid-water (4: 4: 2: 1) | Toluene-ethyl acetate-formic acid (20: 4: 0.5) | Chloroform-acetone (9: 1) | Cyclohexane extraction-chloroform-ethyl acetate (20: 5: 8) | Cyclohexane extraction-ethyl acetate-formic acid (20: 20: 1) |
| Launch effect | Clear spot, separator well | Separate badly, holder tail phenomenon is arranged | Principal spot separates bad | Speckle separates bad | Speckle is rectified shallow, separates better |
Developing solvent is that (4: 4: 2: in the time of 1), it is best that need testing solution launches effect, and appearance hangover, principal spot separate phenomenons such as bad for butanone-ethyl acetate-formic acid-water as can be seen from Table 2.
4. sample solution point sample amount preferred in this detection method:
Get need testing solution each 4.0 μ l, 6.0 μ l, 8.0 μ l, 10.0 μ l, 12.0 μ l respectively, put respectively on same polyamide film, with butanone-ethyl acetate-formic acid-water (4: 4: 2: 1) be developing solvent, launch, take out, dry, spray is with 2% aluminum chloride test solution, 105 ℃ were heated 1 minute, and put under the ultra-violet lamp (365nm) and inspect.With the corresponding position of control medicinal material chromatograph on, speckle colour developing situation sees Table 3:
Table 3 sample solution point sample amount optimization experiment result
| The point sample amount | ??4.0μl | ??6.0μl | ??8.0μl | ??10.0μl | ??12.0μl |
| Effect | Test sample is very shallow in the colour developing of corresponding reference substance position speckle | Test sample is more shallow in the colour developing of corresponding reference substance position speckle | Test sample is more shallow in the colour developing of corresponding reference substance position speckle | Test sample is clear in the colour developing of corresponding reference substance position speckle | Test sample separates bad at corresponding reference substance position speckle, holder tail phenomenon is arranged |
Test sample point sample amount is when 10.0 μ l as can be seen from Table 3, and color developing effect is better on lamellae, is fit to test requirements document.In sum, the qualitative checking method of Fructus Crataegi is in this preparation: get this product 30ml, put in the separatory funnel, extract 2 times with the ether jolting, each 30ml merges ether solution, and ether solution evaporate to dryness, residue add diethyl ether 2ml as need testing solution.Other gets Fructus Crataegi control medicinal material 2g, adds the ultrasonic place of 80% ethanol 20ml 20 minutes, filters, and filtrate evaporate to dryness, residue add water 20ml makes dissolving, extracts 2 times with the ether jolting, and each 30ml shines medical material solution in pairs with legal system.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, (4: 4: 2: 1) be developing solvent, expansion was taken out with butanone-ethyl acetate-formic acid-water, dry, spray is with 2% aluminum chloride test solution, and 105 ℃ were heated 1 minute, and 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 same color.
Following embodiment all can realize the described effect of above-mentioned experimental example
Embodiment 1
Take by weighing the crude drug of following weight portion (kg):
Flos Lonicerae 11 Flos Chrysanthemis 10 Fructus Forsythiaes 6.5
Fructus Crataegi 5 Semen Armeniacae Amarums 5 Pericarpium Citri Reticulataes 0.25
The preparation method of said preparation is: above Six-element, and Flos Lonicerae, Flos Chrysanthemi, Fructus Forsythiae, Semen Armeniacae Amarum be the distillation extraction Aromatic water respectively, and Fructus Crataegi is with 80% ethanol heating extraction secondary, each 2 hours, filter merging filtrate, filtrate recycling ethanol is condensed into extractum, adds an amount of water dissolution; Pericarpium Citri Reticulatae carries out percolation with 60% ethanol as solvent according to the percolation (appendix IO of Chinese Pharmacopoeia version in 2005) under the fluid extract item, collects percolate, reclaims ethanol, and the water dilution with an amount of filters; Merge above-mentioned medicinal liquid and Aromatic water, adding citric acid 0.05g, simple syrup 300ml and benzoic acid are an amount of, add water and make into 1000ml, stir evenly, and filter, promptly.
Embodiment 2-3
According to test agent in 2 batches of the identical recipe quantity of embodiment 1 and the method for making preparations.
Embodiment 4. method of quality control:
A. get embodiment 1-3 gained Jian ' er Qingjie liquid 30ml, put in the separatory funnel, extract 2 times with the ether jolting, each 30ml merges ether solution, and ether solution evaporate to dryness, residue add diethyl ether 2ml as need testing solution.Other gets Fructus Crataegi control medicinal material 2g, adds the ultrasonic place of 80% ethanol 20ml 20 minutes, filters, and filtrate evaporate to dryness, residue add water 20ml makes dissolving, extracts 2 times with the ether jolting, and each 30ml shines medical material solution in pairs with legal system.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, (4: 4: 2: 1) be developing solvent, expansion was taken out with butanone-ethyl acetate-formic acid-water, dry, spray is with 2% aluminum chloride test solution, and 105 ℃ were heated 1 minute, and put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, all show the fluorescence speckle of same color;
B. get embodiment 1-3 gained Jian ' er Qingjie liquid 10ml, put in the separatory funnel, extract twice with the ethyl acetate jolting, each 15 milliliters, combined ethyl acetate liquid, extracting solution low temperature evaporate to dryness, residue adds methanol 2ml as need testing solution, other gets Pericarpium Citri Reticulatae control medicinal material 0.5g, adds methanol 10ml supersound process 10 minutes, gets supernatant medical material solution in contrast.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw need testing solution 5 μ l, control medicinal material solution 3 μ l, putting respectively on same silica gel g thin-layer plate, is developing solvent with butyl acetate-methanol-formic acid (6: 4: 0.5), launches, take out, dry, spray is with vanillin sulphuric acid test solution, and 105 ℃ to be heated to speckle colour developing clear.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, all show the speckle of same color.
C. get Jian ' er Qingjie liquid 6ml, put in the test tube, hang a trinitrophenol reagent paper in the pipe, reuse cork jam-pack is put in 40～50 ℃ of water-baths, and reagent paper shows brick-red after 5 minutes.
Embodiment 5. method of quality control:
A. get embodiment 1-3 gained Jian ' er Qingjie liquid 30ml, put in the separatory funnel, extract 2 times with the ether jolting, each 30ml merges ether solution, and ether solution evaporate to dryness, residue add diethyl ether 2ml as need testing solution.Other gets Fructus Crataegi control medicinal material 2g, adds 80% ethanol 20ml supersound process 20 minutes, filters, and filtrate evaporate to dryness, residue add water 20ml makes dissolving, extracts 2 times with the ether jolting, and each 30ml shines medical material solution in pairs with legal system.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, (4: 4: 2: 1) be developing solvent, expansion was taken out with butanone-ethyl acetate-formic acid-water, dry, spray is with 2% aluminum chloride test solution, and 105 ℃ were heated 1 minute, and put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, all show the fluorescence speckle of same color;
B. get embodiment 1-3 gained Jian ' er Qingjie liquid 10ml, put in the separatory funnel, extract twice with the ethyl acetate jolting, each 15 milliliters, combined ethyl acetate liquid, extracting solution low temperature evaporate to dryness, residue adds methanol 2ml as need testing solution, other gets Pericarpium Citri Reticulatae control medicinal material 0.5g, adds methanol 10ml supersound process 10 minutes, gets supernatant medical material solution in contrast.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw need testing solution 5 μ l, control medicinal material solution 3 μ l, putting respectively on same silica gel g thin-layer plate, is developing solvent with butyl acetate-methanol-formic acid (6: 4: 0.5), launches, take out, dry, spray is with vanillin sulphuric acid test solution, and 105 ℃ to be heated to speckle colour developing clear.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, all show the speckle of same color.
C. get Jian ' er Qingjie liquid 2ml, put in the separatory funnel, add petroleum ether (60～90 ℃) 10ml, jolting 10 minutes is placed, and divides and gets petroleum ether layer, puts evaporate to dryness in the water-bath, and residue adds 2～3 of 5% vanillin sulfuric acid solutions, and displaing amaranth is placed color burn.
In addition, also ratio and the preparation technology with the prescription crude drug made the negative sample that does not contain Fructus Crataegi, Pericarpium Citri Reticulatae, prepared negative control solution according to the preparation method for test agent in the method for quality control, on silica gel g thin-layer plate, speckle does not appear in described 2 kinds of negative samples on the relevant position.
Through repetition test, therefore this method of quality control specificity, good reproducibility as the method for quality control of Jian ' er Qingjie liquid, carry out quality control to Jian ' er Qingjie liquid.
Claims (3)
1. the method for quality control of a Jian ' er Qingjie liquid is characterized in that this method comprises a kind of in two kinds of detections of following a, b at least:
A. get Jian ' er Qingjie liquid, put in the separatory funnel, extract with the ether jolting, ether solution evaporate to dryness, residue add diethyl ether 2ml as need testing solution; Other gets the Fructus Crataegi control medicinal material, adds 80% ethanol supersound process, filters, and filtrate evaporate to dryness, residue add water makes dissolving, extracts with the ether jolting, shines medical material solution in pairs with legal system; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw above-mentioned two kinds of solution, put respectively on same polyamide film, with butanone-ethyl acetate-formic acid-water is developing solvent, launches, and takes out, dry, spray is with 2% aluminum chloride test solution, and 105 ℃ were heated 1 minute, and putting wavelength is to inspect under the 365nm ultra-violet lamp; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
B. get Jian ' er Qingjie liquid, put in the separatory funnel, extract with the ethyl acetate jolting, extracting solution low temperature evaporate to dryness, residue add methanol 2ml as need testing solution, and other gets the Pericarpium Citri Reticulatae control medicinal material, adds the methanol supersound process, gets supernatant medical material solution in contrast; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw need testing solution, control medicinal material solution, putting respectively on same silica gel g thin-layer plate, is developing solvent with butyl acetate-methanol-formic acid, launches, take out, dry, spray is with vanillin sulphuric acid test solution, and 105 ℃ to be heated to speckle colour developing clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
2. method of quality control as claimed in claim 1 is characterized in that this method of quality control comprises a kind of in two kinds of detections of following a, b at least:
A. get Jian ' er Qingjie liquid 30ml, put in the separatory funnel, extract 2 times with the ether jolting, each 30ml merges ether solution, and ether solution evaporate to dryness, residue add diethyl ether 2ml as need testing solution; Other gets Fructus Crataegi control medicinal material 2g, adds 80% ethanol 20ml supersound process 20 minutes, filters, and filtrate evaporate to dryness, residue add water 20ml makes dissolving, extracts 2 times with the ether jolting, and each 30ml shines medical material solution in pairs with legal system; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, (4: 4: 2: 1) be developing solvent, expansion was taken out with butanone-ethyl acetate-formic acid-water, dry, spray is with 2% aluminum chloride test solution, and 105 ℃ were heated 1 minute, and 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 same color;
B. get Jian ' er Qingjie liquid 10ml, put in the separatory funnel, extract twice with the ethyl acetate jolting, each 15 milliliters, combined ethyl acetate liquid, extracting solution low temperature evaporate to dryness, residue adds methanol 2ml as need testing solution, other gets Pericarpium Citri Reticulatae control medicinal material 0.5g, adds methanol 10ml supersound process 10 minutes, gets supernatant medical material solution in contrast; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw need testing solution 5 μ l, control medicinal material solution 3 μ l, putting respectively on same silica gel g thin-layer plate, is developing solvent with butyl acetate-methanol-formic acid (6: 4: 0.5), launches, take out, dry, spray is with vanillin sulphuric acid test solution, and 105 ℃ to be heated to speckle colour developing clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
3. method of quality control as claimed in claim 2 is characterized in that this method of quality control can also comprise a kind of in two kinds of detections of following c, d:
C. get Jian ' er Qingjie liquid 6ml, put in the test tube, hang a trinitrophenol reagent paper in the pipe, reuse cork jam-pack is put in 40～50 ℃ of water-baths, and reagent paper shows brick-red after 5 minutes;
D. get Jian ' er Qingjie liquid 2ml, put in the separatory funnel, add petroleum ether (60～90 ℃) 10ml, jolting 10 minutes is placed, and divides and gets petroleum ether layer, puts evaporate to dryness in the water-bath, and residue adds 2～3 of 5% vanillin sulfuric acid solutions, and displaing amaranth is placed color burn.
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