CN102759600A - Detection method of sufi cough syrup - Google Patents
Detection method of sufi cough syrup Download PDFInfo
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- CN102759600A CN102759600A CN2012102768079A CN201210276807A CN102759600A CN 102759600 A CN102759600 A CN 102759600A CN 2012102768079 A CN2012102768079 A CN 2012102768079A CN 201210276807 A CN201210276807 A CN 201210276807A CN 102759600 A CN102759600 A CN 102759600A
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Abstract
The invention provides a detection method of sufi cough syrup. The method comprises identification of ammonium chloride in the sufi cough syrup, identification of the root bark of white mulberry, identification of platycodon grandiflorum, identification of liquorice, and identification of menthol crystal and content determination of ammonium chloride in the sufi cough syrup. The detection method conducts effective quality control on main ingredients of the ammonium chloride, the root bark of white mulberry, the platycodon grandiflorum, the liquorice, and the menthol crystal, can better and comprehensively reflect quality of the sufi cough syrup, and can effectively prevent illegal manufacturers from producing fake sufi cough syrup so as to guarantee safety and efficiency of pharmacy of the masses.
Description
Technical field
The present invention relates to the detection method of effective constituent in a kind of Chinese traditional patent formulation preparation, particularly relate to the detection method that a kind of Sufi coughs effective constituent in the syrup.
Background technology
It is the 13 kind of recording of " the Sanitation Ministry medicine standard " Chinese traditional patent formulation preparation that the Sufi coughs syrup; Standard is numbered WS3-B-2521-97; Prescription is the agent of Chinese and Western medicine compound syrup for Radix Stemonae fluidextract, root bark of white mulberry liquid extract, Platycodon glaucus fluidextract, liquid extract of liquorice, ammonium chloride, ephedrine hydrochloride, menthol.It has the effect of eliminating phlegm and relieving cough, and clinical being used for coughs, asthma, and many phlegm, the treatment of breathing problems such as bronchitis is the common drug that is used to treat breathing problems such as acute and chronic bronchitis, cough, asthma, many phlegm in the market.But the method that effective constituent in the prescription is not detected in the primary standard had not both had quality index, did not have the discrimination method of these quality index yet.Illegal manufacturer not in strict accordance with the dosage batching of prescription, reduces the high raw material of price wantonly when producing medicine, cause the curative effect of medicine obviously to descend, and influences the safe and effective of medicine, the grievous injury patients'benefit.
Summary of the invention
The object of the invention provides the detection method that a kind of Sufi coughs syrup.Throw or do not throw corresponding raw material less in order to monitor illegal manufacturer, control the quality that the Sufi coughs syrup effectively, make this drug safety effective, thereby guaranteed the clinical efficacy of this syrup preparation, safeguarded patients'benefit.
The prescription that the Sufi coughs syrup is: Radix Stemonae fluidextract 10ml, root bark of white mulberry liquid extract 16ml, Platycodon glaucus fluidextract 30ml, liquid extract of liquorice 35ml, ammonium chloride 20g, ephedrine hydrochloride 0.5g, menthol 0.1g.
This Sufi coughs the detection method of syrup, comprises differentiating and the assay project that said discriminating comprises the discriminating of the Sufi being coughed ammonium chloride in the syrup, the discriminating of the root bark of white mulberry, the discriminating of balloonflower root, the discriminating of Radix Glycyrrhizae, the discriminating of menthol; Said assay comprises the assay of the Sufi being coughed ammonium chloride in the syrup; Said detection method comprises following:
(1) discriminating of ammonium chloride
These article of getting 1～3ml adds water 5～15ml, after adding nitric acid and making into acidity, adds silver nitrate test solution 1.5～2.5ml, promptly generates the curdy precipitate of white, adds ammonia solution again, and deposition i.e. dissolving; With
/Or
These article of getting 5～15ml, after hydro-oxidation sodium test solution makes alkalize, heating, it is smelly that ammonia promptly takes place, and can make moistening litmus red test paper become blue;
(2) discriminating of the root bark of white mulberry
These article of getting 20～40ml puts and is evaporated to nearly thick paste shape in the water-bath, adds ethanol 30～70ml, and sonicated 15～25 minutes is centrifugal; Get the supernatant evaporate to dryness, add saturated sodium carbonate solution 15～25ml, sonicated 20 minutes filters, and filtrating adds watery hydrochloric acid and regulates pH value to 1～2; Left standstill 20～40 minutes, and filtered, filtrating is extracted 2～3 times with the ethyl acetate jolting, each 5～15ml; Combined ethyl acetate liquid, evaporate to dryness, residue add methyl alcohol 1～2ml makes dissolving, as need testing solution; Other gets root bark of white mulberry control medicinal material 0.5～1.5g and is ground into meal, adds saturated sodium carbonate solution 15～25ml, shines medicinal material solution in pairs with legal system; Draw each 4～8 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with 30～60 ℃ of sherwood oils: ethyl acetate=10～14: 6～8 is developping agent; Launch, take out, dry; Put under the ultraviolet lamp that wavelength is 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
(3) discriminating of balloonflower root
These article of getting 30～50ml, thin up to 80～120ml, centrifugal, get supernatant, through D
101Macroporous adsorptive resins, it is colourless that water is eluted to eluent, discards water liquid, uses 70% ethanol, 80～120ml wash-out again; Collect eluent, evaporate to dryness adds 7% sulfuric acid ethanol: water=0.8～1.2:2.5～3.5 mixed liquors, 17～23ml, reflux 2～3 hours; Put coldly, extract 2～4 times with the methenyl choloride jolting, each 10～30ml merges methenyl choloride liquid; Add ammonia solution 20～50ml washing, discard washing lotion, methenyl choloride liquid filters with the filter paper that a small amount of anhydrous sodium sulfate is housed; The filtrating evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets balloonflower root control medicinal material 0.5～1.5g and is ground into meal, adds 7% sulfuric acid ethanol: water=0.8～1.2:2.5～3.5 mixed liquors, 17～23ml, shine medicinal material solution in pairs with legal system; Draw each 4～8 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with methenyl choloride: ether=4.5～5.5: 3.5～4.5 is developping agent; Launch, take out, dry; Put under the ultraviolet lamp that wavelength is 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
(4) discriminating of Radix Glycyrrhizae
These article of getting 8～12ml, thin up to 25～35ml, centrifugal, get supernatant, through D
101The type macroporous adsorptive resins, it is colourless that water is eluted to eluent, discards water liquid, uses 60% ethanol, 40～80ml wash-out again, collects eluent; Evaporate to dryness, residue add water 8～12ml makes dissolving, extracts 2～4 times each 10～30ml with water saturated normal butyl alcohol; Merge normal butyl alcohol liquid, with the saturated water washing of normal butyl alcohol 2～4 times, each 5～15ml discards water liquid; Obtain normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 0.5～1.5ml makes dissolving, gets supernatant as need testing solution; Extracting liquorice control medicinal material 0.8～1.2g adds ethanol 15～25ml in addition, and reflux 25～35 minutes filters, and gets filtrating; Evaporate to dryness, residue add water 7～13ml makes dissolving, extracts 2～4 times each 5～15ml with water saturated normal butyl alcohol; Merge butanol solution, with normal butyl alcohol saturation water washing 2～4 times, each 5～15ml discards water liquid; Obtain normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 0.5～1.5ml makes dissolving, gets supernatant as reference substance solution; Draw each 5～10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate with the preparation of 1% sodium hydroxide solution, with normal butyl alcohol: glacial acetic acid: water=8～10:1.7～2.3:10～12 upper strata liquid are developping agent; Launch, take out, dry; Spray is with 10% 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 principal spot of same color;
(5) discriminating of menthol
These article of getting 15～25ml adds 60～90 ℃ of sherwood oil 30～50ml joltings and extracts 1～2 time, gets extract, waves and is dissipated to 1～2ml, as need testing solution; Other gets the menthol reference substance, adds 60～90 ℃ of sherwood oils and processes the solution that every 1ml contains menthol 2mg, as reference substance solution; Draw each 5～8 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane: ethyl acetate=22～28:3.5～4.5 are developping agent; Launch, take out, dry; Spray is with 2% vanillic aldehyde sulfuric acid solution: ethanol=0.8～1.2: 3.5～4.5 mixed solution, 105 ℃ of bakings 5～10 minutes, in the test sample chromatogram; With the corresponding position of reference substance chromatogram on, show the spot of same color;
(6) assay of ammonium chloride
These article of getting 15～25ml puts in the 100ml measuring bottle, adds water 50～90ml and activated charcoal 1.5～2.5g, places 10～30 minutes; Jolting constantly adds water to scale, shakes up, and filters with dry filter paper; Discard filtrating just, precision is measured subsequent filtrate 25ml, adds potassium chromate indicator solution 0.5ml; With the titration of 0.1mol/L silver nitrate solution, with among the every 1ml of 0.1mol/L silver nitrate titration liquid with 3.545mg ammonium chloride be standard, can calculate the content of ammonium chloride in these article;
These article chloride calculates with total chlorine amount and should be 1.27～1.60% (g/ml).
The concrete detection method of the present invention is:
(1) discriminating of ammonium chloride
These article of getting 2ml adds water 10ml, after adding nitric acid and making into acidity, adds silver nitrate test solution 2ml, promptly generates the curdy precipitate of white, adds ammonia solution again, and deposition i.e. dissolving; With
/Or
These article of getting 10ml, after hydro-oxidation sodium test solution makes alkalize, heating, it is smelly that ammonia promptly takes place, and can make moistening litmus red test paper become blue;
(2) discriminating of the root bark of white mulberry
These article of getting 30ml puts and is evaporated to nearly thick paste shape in the water-bath, adds ethanol 50ml, and sonicated 20 minutes is centrifugal; Get the supernatant evaporate to dryness, add saturated sodium carbonate solution 20ml, sonicated 20 minutes filters, and filtrating adds watery hydrochloric acid and regulates pH value to 1～2; Left standstill 30 minutes, and filtered, filtrating is extracted 2 times with the ethyl acetate jolting, each 10ml; Combined ethyl acetate liquid, evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution; Other gets root bark of white mulberry control medicinal material 1g and is ground into meal, adds saturated sodium carbonate solution 20ml, shines medicinal material solution in pairs with legal system; Draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with 30～60 ℃ of sherwood oils: ethyl acetate=12: 7 is a developping agent; Launch, take out, dry; Put under the ultraviolet lamp that wavelength is 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
(3) discriminating of balloonflower root
These article of getting 40ml, thin up are to 100ml, and be centrifugal, gets supernatant, through D
101Macroporous adsorptive resins, it is colourless that water is eluted to eluent, discards water liquid, uses 70% ethanol 100ml wash-out again, collects eluent; Evaporate to dryness adds 7% sulfuric acid ethanol: water=1:3 mixed liquor 20ml, and reflux 3 hours is put coldly, extracts 2 times with the methenyl choloride jolting; Each 20ml merges methenyl choloride liquid, adds ammonia solution 30ml washing, discards washing lotion; Methenyl choloride liquid filters with the filter paper that a small amount of anhydrous sodium sulfate is housed, the filtrating evaporate to dryness, and residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets balloonflower root control medicinal material 1g and is ground into meal, adds 7% sulfuric acid ethanol: water=1:3 mixed liquor 20ml, shine medicinal material solution in pairs with legal system; Draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with methenyl choloride: ether=5: 4 is a developping agent; Launch, take out, dry; Put under the ultraviolet lamp that wavelength is 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
(4) discriminating of Radix Glycyrrhizae
These article of getting 10ml, thin up are to 30ml, and be centrifugal, gets supernatant, through D
101The type macroporous adsorptive resins, it is colourless that water is eluted to eluent, discards water liquid, uses 60% ethanol 60ml wash-out again, collects eluent; Evaporate to dryness, residue add water 10ml makes dissolving, extracts 2 times with water saturated normal butyl alcohol, each 10ml; Merge normal butyl alcohol liquid, with the saturated water washing of normal butyl alcohol 2 times, 10ml discards water liquid at every turn; Obtain normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, gets supernatant as need testing solution; Extracting liquorice control medicinal material 1g adds ethanol 20ml in addition, and reflux 30 minutes filters, and gets filtrating; Evaporate to dryness, residue add water 10ml makes dissolving, extracts 2 times with water saturated normal butyl alcohol, each 10ml; Merge butanol solution, with normal butyl alcohol saturation water washing 2 times, each 10ml discards water liquid; Obtain normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, gets supernatant as reference substance solution; Draw each 8 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate with the preparation of 1% sodium hydroxide solution, with normal butyl alcohol: glacial acetic acid: water=9:2:11 upper strata liquid is developping agent; Launch, take out, dry; Spray is with 10% 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 principal spot of same color;
(5) discriminating of menthol
These article of getting 20ml adds 60～90 ℃ of sherwood oil 40ml joltings and extracts 1 time, gets extract, waves and is dissipated to 1ml, as need testing solution; Other gets the menthol reference substance, adds 60～90 ℃ of sherwood oils and processes the solution that every 1ml contains menthol 2 ㎎, as reference substance solution; Drawing each 6 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developping agent with cyclohexane: ethyl acetate=25:4; Launch, take out, dry; Spray is with 2% vanillic aldehyde sulfuric acid solution: the mixed solution of ethanol=1: 4,105 ℃ of bakings 8 minutes, in the test sample chromatogram; With the corresponding position of reference substance chromatogram on, show the spot of same color;
(6) assay of ammonium chloride
These article of getting 20ml puts in the 100ml measuring bottle, adds water 70ml and activated charcoal 2g, places 15 minutes; Jolting constantly adds water to scale, shakes up, and filters with dry filter paper; Discard filtrating just, precision is measured subsequent filtrate 25ml, adds potassium chromate indicator solution 0.5ml; With the titration of 0.1mol/L silver nitrate solution, with among the every 1ml of 0.1mol/L silver nitrate titration liquid with 3.545mg ammonium chloride be standard, can calculate the content of ammonium chloride in these article.
These article chloride calculates with total chlorine amount and should be 1.27～1.60% (g/ml).
Wherein, the D described in step (3) and the step (4)
101Type macroporous adsorptive resins internal diameter is 15mm, and height is 12cm.
Technique effect of the present invention:
The Sufi coughs the discriminating of syrup through ammonium chloride among the present invention, the discriminating of the root bark of white mulberry, the discriminating of balloonflower root; The discriminating of Radix Glycyrrhizae, the discriminating of menthol, the assay of ammonium chloride; Clear and definite component content index has been arranged; This method is scientific and reasonable, practical, and Main Ingredients and Appearances such as the ammonium chloride in the prescription, the root bark of white mulberry, balloonflower root, Radix Glycyrrhizae, menthol have all obtained effective component monitoring, and this can not only reflect better and more comprehensively that the Sufi coughs the quality of syrup; And can control illegal manufacturers produce Sufi of poor quality effectively and cough syrup, thereby guarantee that the masses are safe and effective for medication.
Embodiment
Embodiment 1:
[
Prescription] Radix Stemonae fluidextract 10ml, root bark of white mulberry liquid extract 16ml, Platycodon glaucus fluidextract 30ml, liquid extract of liquorice 35ml, ammonium chloride 20g, ephedrine hydrochloride 0.5g, menthol 0.1g.
[
Method for making] get sucrose 400g, add water boil, filter, process simple syrup, put cold.Other gets ammonium chloride 20g, ephedrine hydrochloride 0.5g, Sodium Benzoate 4g, Stevioside 0.3g; After adding the suitable quantity of water dissolving, add in the above-mentioned syrup, mixing adds Radix Stemonae fluidextract 10ml again; Root bark of white mulberry liquid extract 16ml, Platycodon glaucus fluidextract 30ml, menthol 0.1g and the ethanolic solution that contains Sang Zi essence, mixing; Add water to 1000ml, stir, promptly get these article Sufi and cough syrup.
[
Proterties] these article be brown dense liquid this; Gas fragrance, it is sweet to distinguish the flavor of.
[
Differentiate] discriminating of (1) ammonium chloride
These article of getting 1ml adds water 5ml, after adding nitric acid and making into acidity, adds silver nitrate test solution 1.5ml, promptly generates the curdy precipitate of white, adds ammonia solution again, and deposition i.e. dissolving; With
/Or
These article of getting 5ml, after hydro-oxidation sodium test solution makes alkalize, heating, it is smelly that ammonia promptly takes place, and can make moistening litmus red test paper become blue.
(2) discriminating of the root bark of white mulberry
These article of getting 20ml puts and is evaporated to nearly thick paste shape in the water-bath, adds ethanol 30ml, and sonicated 15 minutes is centrifugal; Get the supernatant evaporate to dryness, add saturated sodium carbonate solution 15ml, sonicated 20 minutes filters, and filtrating adds watery hydrochloric acid and regulates pH value to 1～2; Left standstill 20 minutes, and filtered, filtrating is extracted 2 times with the ethyl acetate jolting, each 5ml; Combined ethyl acetate liquid, evaporate to dryness, residue add methyl alcohol 1.5ml makes dissolving, as need testing solution; Other gets root bark of white mulberry control medicinal material 0.5g and is ground into meal, adds saturated sodium carbonate solution 15ml, shines medicinal material solution in pairs with legal system; Draw each 4 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with 30～60 ℃ of sherwood oils: ethyl acetate=11: 6 is a developping agent; Launch, take out, dry; Put under the ultraviolet lamp that wavelength is 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
(3) discriminating of balloonflower root
These article of getting 30ml, thin up are to 80ml, and be centrifugal, gets supernatant, through D
101Macroporous adsorptive resins (internal diameter is 15mm, and height is 12cm), it is colourless that water is eluted to eluent, discards water liquid; Use 70% ethanol 80ml wash-out again, collect eluent, evaporate to dryness adds 7% sulfuric acid ethanol: water=0.8:2.5 mixed liquor 17ml; Reflux 2 hours is put coldly, extracts 3 times each 10ml with the methenyl choloride jolting; Merge methenyl choloride liquid, add ammonia solution 20ml washing, discard washing lotion, methenyl choloride liquid filters with the filter paper that a small amount of anhydrous sodium sulfate is housed; The filtrating evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets balloonflower root control medicinal material 0.5g and is ground into meal, adds 7% sulfuric acid ethanol: water=0.8:2.5 mixed liquor 17ml, shine medicinal material solution in pairs with legal system; Draw each 4 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with methenyl choloride: ether=4.5: 3.5 is a developping agent; Launch, take out, dry; Put under the ultraviolet lamp that wavelength is 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
(4) discriminating of Radix Glycyrrhizae
These article of getting 8ml, thin up are to 25ml, and be centrifugal, gets supernatant, through D
101Type macroporous adsorptive resins (internal diameter is 15mm, and height is 12cm), it is colourless that water is eluted to eluent, discards water liquid, uses 60% ethanol 40ml wash-out again; Collect eluent, evaporate to dryness, residue add water 8ml makes dissolving, extracts 3 times with water saturated normal butyl alcohol, each 20ml; Merge normal butyl alcohol liquid, with the saturated water washing of normal butyl alcohol 3 times, 5ml discards water liquid at every turn; Obtain normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 0.5ml makes dissolving, gets supernatant as need testing solution; Extracting liquorice control medicinal material 0.8g adds ethanol 15ml in addition, and reflux 25 minutes filters, and gets filtrating; Evaporate to dryness, residue add water 7ml makes dissolving, extracts 3 times with water saturated normal butyl alcohol, each 5ml; Merge butanol solution, with normal butyl alcohol saturation water washing 3 times, each 5ml discards water liquid; Obtain normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 0.5ml makes dissolving, gets supernatant as reference substance solution; Draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate with the preparation of 1% sodium hydroxide solution, with normal butyl alcohol: glacial acetic acid: water=8:1.7:10 upper strata liquid is developping agent; Launch, take out, dry; Spray is with 10% 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 principal spot of same color.
(5) discriminating of menthol
These article of getting 15ml adds 60～90 ℃ of sherwood oil 30ml joltings and extracts 1 time, gets extract, waves and is dissipated to 1ml, as need testing solution; Other gets the menthol reference substance, adds 60～90 ℃ of sherwood oils and processes the solution that every 1ml contains menthol 2mg, as reference substance solution; Draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane: ethyl acetate=22: 3.5 is developping agent; Launch, take out, dry; Spray is with 2% vanillic aldehyde sulfuric acid solution: the mixed solution of ethanol=0.8: 3.5,105 ℃ of bakings 5 minutes, in the test sample chromatogram; With the corresponding position of reference substance chromatogram on, show the spot of same color.
[
Inspection]
Relative densityShould be not less than 1.25 (an appendix VII of Chinese Pharmacopoeia version in 2010 A).
OtherShould meet each item regulation (an appendix I of Chinese Pharmacopoeia version in 2010 H) relevant under the syrup item.
[
Assay]
The assay of ammonium chloride
These article of getting 15ml puts in the 100ml measuring bottle, adds water 50ml and activated charcoal 1.5g, places 10 minutes; Jolting constantly adds water to scale, shakes up, and filters with dry filter paper; Discard filtrating just, precision is measured subsequent filtrate 25ml, adds potassium chromate indicator solution 0.5ml; With the titration of 0.1mol/L silver nitrate solution, with among the every 1ml of 0.1mol/L silver nitrate titration liquid with 3.545mg ammonium chloride be standard, can calculate the content of ammonium chloride in these article.
These article chloride calculates content greater than 1.27% (g/ml), less than 1.60% (g/ml), for qualified with total chlorine amount.
[
Function with cure mainly] eliminating phlegm and relieving cough.Be used for cough, asthma, many phlegm, bronchitis.
[
Usage and consumption] oral, a 10ml, 3 times on the one.
[
Storage] sealing, put shady and cool place.
Embodiment 2:
[
Prescription] Radix Stemonae fluidextract 10ml, root bark of white mulberry liquid extract 16ml, Platycodon glaucus fluidextract 30ml, liquid extract of liquorice 35ml, ammonium chloride 20g, ephedrine hydrochloride 0.5g, menthol 0.1g.
[
Method for making] get sucrose 400g, add water boil, filter, process simple syrup, put cold.Other gets ammonium chloride 20g, ephedrine hydrochloride 0.5g, Sodium Benzoate 4g, Stevioside 0.3g; After adding the suitable quantity of water dissolving, add in the above-mentioned syrup, mixing adds Radix Stemonae fluidextract 10ml again; Root bark of white mulberry liquid extract 16ml, Platycodon glaucus fluidextract 30ml, menthol 0.1g and the ethanolic solution that contains Sang Zi essence, mixing; Add water to 1000ml, stir, promptly get these article Sufi and cough syrup.
[
Differentiate] discriminating of (1) ammonium chloride
These article of getting 3ml adds water 15ml, after adding nitric acid and making into acidity, adds silver nitrate test solution 2.5ml, promptly generates the curdy precipitate of white, adds ammonia solution again, and deposition i.e. dissolving; With
/Or
These article of getting 15ml, after hydro-oxidation sodium test solution makes alkalize, heating, it is smelly that ammonia promptly takes place, and can make moistening litmus red test paper become blue.
(2) discriminating of the root bark of white mulberry
These article of getting 40ml puts and is evaporated to nearly thick paste shape in the water-bath, adds ethanol 70ml, and sonicated 25 minutes is centrifugal; Get the supernatant evaporate to dryness, add saturated sodium carbonate solution 25ml, sonicated 20 minutes filters, and filtrating adds watery hydrochloric acid and regulates pH value to 1～2; Left standstill 40 minutes, and filtered, filtrating is extracted 3 times with the ethyl acetate jolting, each 15ml; Combined ethyl acetate liquid, evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as need testing solution; Other gets root bark of white mulberry control medicinal material 1.5g and is ground into meal, adds saturated sodium carbonate solution 25ml, shines medicinal material solution in pairs with legal system; Draw each 8 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with 30～60 ℃ of sherwood oils: ethyl acetate=14: 8 is a developping agent; Launch, take out, dry; Put under the ultraviolet lamp that wavelength is 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
(3) discriminating of balloonflower root
These article of getting 50ml, thin up are to 120ml, and be centrifugal, gets supernatant, through D
101Macroporous adsorptive resins (internal diameter is 15mm, and height is 12cm), it is colourless that water is eluted to eluent, discards water liquid; Use 70% ethanol 120ml wash-out again, collect eluent, evaporate to dryness adds 7% sulfuric acid ethanol: water=1.2:3.5 mixed liquor 23ml; Reflux 3 hours is put coldly, extracts 4 times each 30ml with the methenyl choloride jolting; Merge methenyl choloride liquid, add ammonia solution 50ml washing, discard washing lotion, methenyl choloride liquid filters with the filter paper that a small amount of anhydrous sodium sulfate is housed; The filtrating evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets balloonflower root control medicinal material 1.5g and is ground into meal, adds 7% sulfuric acid ethanol: water=1.2:3.5 mixed liquor 23ml, shine medicinal material solution in pairs with legal system; Draw each 8 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with methenyl choloride: ether=5.5: 4.5 is a developping agent; Launch, take out, dry; Put under the ultraviolet lamp that wavelength is 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
(4) discriminating of Radix Glycyrrhizae
These article of getting 12ml, thin up are to 35ml, and be centrifugal, gets supernatant, through D
101Type macroporous adsorptive resins (internal diameter is 15mm, and height is 12cm), it is colourless that water is eluted to eluent, discards water liquid, uses 60% ethanol 80ml wash-out again; Collect eluent, evaporate to dryness, residue add water 12ml makes dissolving, extracts 4 times with water saturated normal butyl alcohol, each 30ml; Merge normal butyl alcohol liquid, with the saturated water washing of normal butyl alcohol 4 times, 15ml discards water liquid at every turn; Obtain normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 1.5ml makes dissolving, gets supernatant as need testing solution; Extracting liquorice control medicinal material 1.2g adds ethanol 25ml in addition, and reflux 35 minutes filters, and gets filtrating; Evaporate to dryness, residue add water 13ml makes dissolving, extracts 4 times with water saturated normal butyl alcohol, each 15ml; Merge butanol solution, with normal butyl alcohol saturation water washing 4 times, each 15ml discards water liquid; Obtain normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 1.5ml makes dissolving, gets supernatant as reference substance solution; Draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate with the preparation of 1% sodium hydroxide solution, with normal butyl alcohol: glacial acetic acid: water=10:2.3:12 upper strata liquid is developping agent; Launch, take out, dry; Spray is with 10% 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 principal spot of same color.
(5) discriminating of menthol
These article of getting 25ml adds 60～90 ℃ of sherwood oil 50ml joltings and extracts 2 times, gets extract, waves and is dissipated to 2ml, as need testing solution; Other gets the menthol reference substance, adds 60～90 ℃ of sherwood oils and processes the solution that every 1ml contains menthol 2mg, as reference substance solution; Drawing each 8 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developping agent with cyclohexane: ethyl acetate=28:4.5; Launch, take out, dry; Spray is with 2% vanillic aldehyde sulfuric acid solution: the mixed solution of ethanol=1.2: 4.5,105 ℃ of bakings 10 minutes, in the test sample chromatogram; With the corresponding position of reference substance chromatogram on, show the spot of same color.
[
Assay]
The assay of ammonium chloride
These article of getting 25ml puts in the 100ml measuring bottle, adds water 90ml and activated charcoal 2.5g, places 30 minutes; Jolting constantly adds water to scale, shakes up, and filters with dry filter paper; Discard filtrating just, precision is measured subsequent filtrate 25ml, adds potassium chromate indicator solution 0.5ml; With the titration of 0.1mol/L silver nitrate solution, with among the every 1ml of 0.1mol/L silver nitrate titration liquid with 3.545mg ammonium chloride be standard, can calculate the content of ammonium chloride in these article;
These article chloride calculates content greater than 1.27% (g/ml), less than 1.60% (g/ml), for qualified with total chlorine amount.
Other is with embodiment 1.
Embodiment 3:
[
Prescription] Radix Stemonae fluidextract 10ml, root bark of white mulberry liquid extract 16ml, Platycodon glaucus fluidextract 30ml, liquid extract of liquorice 35ml, ammonium chloride 20g, ephedrine hydrochloride 0.5g, menthol 0.1g.
[
Method for making] get sucrose 400g, add water boil, filter, process simple syrup, put cold.Other gets ammonium chloride 20g, ephedrine hydrochloride 0.5g, Sodium Benzoate 4g, Stevioside 0.3g; After adding the suitable quantity of water dissolving, add in the above-mentioned syrup, mixing adds Radix Stemonae fluidextract 10ml again; Root bark of white mulberry liquid extract 16ml, Platycodon glaucus fluidextract 30ml, menthol 0.1g and the ethanolic solution that contains Sang Zi essence, mixing; Add water to 1000ml, stir, promptly get these article Sufi and cough syrup.
[
Differentiate] discriminating of (1) ammonium chloride
These article of getting 2ml adds water 10ml, after adding nitric acid and making into acidity, adds silver nitrate test solution 2ml, promptly generates the curdy precipitate of white, adds ammonia solution again, and deposition i.e. dissolving; With
/Or
These article of getting 10ml, after hydro-oxidation sodium test solution makes alkalize, heating, it is smelly that ammonia promptly takes place, and can make moistening litmus red test paper become blue.
(2) discriminating of the root bark of white mulberry
These article of getting 30ml puts and is evaporated to nearly thick paste shape in the water-bath, adds ethanol 50ml, and sonicated 20 minutes is centrifugal; Get the supernatant evaporate to dryness, add saturated sodium carbonate solution 20ml, sonicated 20 minutes filters, and filtrating adds watery hydrochloric acid and regulates pH value to 1～2; Left standstill 30 minutes, and filtered, filtrating is extracted 2 times with the ethyl acetate jolting, each 10ml; Combined ethyl acetate liquid, evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution; Other gets root bark of white mulberry control medicinal material 1g and is ground into meal, adds saturated sodium carbonate solution 20ml, shines medicinal material solution in pairs with legal system; Draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with 30～60 ℃ of sherwood oils: ethyl acetate=12: 7 is a developping agent; Launch, take out, dry; Put under the ultraviolet lamp that wavelength is 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
(3) discriminating of balloonflower root
These article of getting 40ml, thin up are to 100ml, and be centrifugal, gets supernatant, through D
101Macroporous adsorptive resins (internal diameter is 15mm, and height is 12cm), it is colourless that water is eluted to eluent, discards water liquid; Use 70% ethanol 100ml wash-out again, collect eluent, evaporate to dryness adds 7% sulfuric acid ethanol: water=1:3 mixed liquor 20ml; Reflux 3 hours is put coldly, extracts 2 times each 20ml with the methenyl choloride jolting; Merge methenyl choloride liquid, add ammonia solution 30ml washing, discard washing lotion, methenyl choloride liquid filters with the filter paper that a small amount of anhydrous sodium sulfate is housed; The filtrating evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets balloonflower root control medicinal material 1g and is ground into meal, adds 7% sulfuric acid ethanol: water=1:3 mixed liquor 20ml, shine medicinal material solution in pairs with legal system; Draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with methenyl choloride: ether=5: 4 is a developping agent; Launch, take out, dry; Put under the ultraviolet lamp that wavelength is 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
(4) discriminating of Radix Glycyrrhizae
These article of getting 10ml, thin up are to 30ml, and be centrifugal, gets supernatant, through D
101Type macroporous adsorptive resins (internal diameter is 15mm, and height is 12cm), it is colourless that water is eluted to eluent, discards water liquid, uses 60% ethanol 60ml wash-out again; Collect eluent, evaporate to dryness, residue add water 10ml makes dissolving, extracts 2 times with water saturated normal butyl alcohol, each 10ml; Merge normal butyl alcohol liquid, with the saturated water washing of normal butyl alcohol 2 times, 10ml discards water liquid at every turn; Obtain normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, gets supernatant as need testing solution; Extracting liquorice control medicinal material 1g adds ethanol 20ml in addition, and reflux 30 minutes filters, and gets filtrating; Evaporate to dryness, residue add water 10ml makes dissolving, extracts 2 times with water saturated normal butyl alcohol, each 10ml; Merge butanol solution, with normal butyl alcohol saturation water washing 2 times, each 10ml discards water liquid; Obtain normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, gets supernatant as reference substance solution; Draw each 8 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate with the preparation of 1% sodium hydroxide solution, with normal butyl alcohol: glacial acetic acid: water=9:2:11 upper strata liquid is developping agent; Launch, take out, dry; Spray is with 10% 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 principal spot of same color.
(5) discriminating of menthol
These article of getting 20ml adds 60～90 ℃ of sherwood oil 40ml joltings and extracts 1 time, gets extract, waves and is dissipated to 1ml, as need testing solution; Other gets the menthol reference substance, adds 60～90 ℃ of sherwood oils and processes the solution that every 1ml contains menthol 2 ㎎, as reference substance solution; Drawing each 6 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developping agent with cyclohexane: ethyl acetate=25:4; Launch, take out, dry; Spray is with 2% vanillic aldehyde sulfuric acid solution: the mixed solution of ethanol=1: 4,105 ℃ of bakings 8 minutes, in the test sample chromatogram; With the corresponding position of reference substance chromatogram on, show the spot of same color.
[
Assay]
The assay of ammonium chloride
These article of getting 20ml puts in the 100ml measuring bottle, adds water 70ml and activated charcoal 2g, places 15 minutes; Jolting constantly adds water to scale, shakes up, and filters with dry filter paper; Discard filtrating just, precision is measured subsequent filtrate 25ml, adds potassium chromate indicator solution 0.5ml; With the titration of 0.1mol/L silver nitrate solution, with among the every 1ml of 0.1mol/L silver nitrate titration liquid with 3.545mg ammonium chloride be standard, can calculate the content of ammonium chloride in these article.
These article chloride calculates content greater than 1.27% (g/ml), less than 1.60% (g/ml), for qualified with total chlorine amount.
Other is with embodiment 1.
Claims (3)
1. a Sufi coughs the detection method of syrup, and this detection method comprises differentiates and the assay project that it is characterized in that: said discriminating comprises the discriminating of the Sufi being coughed ammonium chloride in the syrup; The discriminating of the root bark of white mulberry; The discriminating of balloonflower root, the discriminating of Radix Glycyrrhizae, the discriminating of menthol; Said assay comprises the assay of the Sufi being coughed ammonium chloride in the syrup; Said detection method comprises following:
(1) discriminating of ammonium chloride
These article of getting 1～3ml adds water 5～15ml, after adding nitric acid and making into acidity, adds silver nitrate test solution 1.5～2.5ml, promptly generates the curdy precipitate of white, adds ammonia solution again, and deposition i.e. dissolving; With
/Or
These article of getting 5～15ml, after hydro-oxidation sodium test solution makes alkalize, heating, it is smelly that ammonia promptly takes place, and can make moistening litmus red test paper become blue;
(2) discriminating of the root bark of white mulberry
These article of getting 20～40ml puts and is evaporated to nearly thick paste shape in the water-bath, adds ethanol 30～70ml, and sonicated 15～25 minutes is centrifugal; Get the supernatant evaporate to dryness, add saturated sodium carbonate solution 15～25ml, sonicated 20 minutes filters, and filtrating adds watery hydrochloric acid and regulates pH value to 1～2; Left standstill 20～40 minutes, and filtered, filtrating is extracted 2～3 times with the ethyl acetate jolting, each 5～15ml; Combined ethyl acetate liquid, evaporate to dryness, residue add methyl alcohol 1～2ml makes dissolving, as need testing solution; Other gets root bark of white mulberry control medicinal material 0.5～1.5g and is ground into meal, adds saturated sodium carbonate solution 15～25ml, shines medicinal material solution in pairs with legal system; Draw each 4～8 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with 30～60 ℃ of sherwood oils: ethyl acetate=10～14: 6～8 is developping agent; Launch, take out, dry; Put under the ultraviolet lamp that wavelength is 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
(3) discriminating of balloonflower root
These article of getting 30～50ml, thin up to 80～120ml, centrifugal, get supernatant, through D
101Macroporous adsorptive resins, it is colourless that water is eluted to eluent, discards water liquid, uses 70% ethanol, 80～120ml wash-out again; Collect eluent, evaporate to dryness adds 7% sulfuric acid ethanol: water=0.8～1.2: 2.5～3.5 mixed liquors, 17～23ml, reflux 2～3 hours; Put coldly, extract 2～4 times with the methenyl choloride jolting, each 10～30ml merges methenyl choloride liquid; Add ammonia solution 20～50ml washing, discard washing lotion, methenyl choloride liquid filters with the filter paper that a small amount of anhydrous sodium sulfate is housed; The filtrating evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets balloonflower root control medicinal material 0.5～1.5g and is ground into meal, adds 7% sulfuric acid ethanol: water=0.8～1.2: 2.5～3.5 mixed liquors, 17～23ml, shine medicinal material solution in pairs with legal system; Draw each 4～8 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with methenyl choloride: ether=4.5～5.5: 3.5～4.5 is developping agent; Launch, take out, dry; Put under the ultraviolet lamp that wavelength is 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
(4) discriminating of Radix Glycyrrhizae
These article of getting 8～12ml, thin up to 25～35ml, centrifugal, get supernatant, through D
101The type macroporous adsorptive resins, it is colourless that water is eluted to eluent, discards water liquid, uses 60% ethanol, 40～80ml wash-out again, collects eluent; Evaporate to dryness, residue add water 8～12ml makes dissolving, extracts 2～4 times each 10～30ml with water saturated normal butyl alcohol; Merge normal butyl alcohol liquid, with the saturated water washing of normal butyl alcohol 2～4 times, each 5～15ml discards water liquid; Obtain normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 0.5～1.5ml makes dissolving, gets supernatant as need testing solution; Extracting liquorice control medicinal material 0.8～1.2g adds ethanol 15～25ml in addition, and reflux 25～35 minutes filters, and gets filtrating; Evaporate to dryness, residue add water 7～13ml makes dissolving, extracts 2～4 times each 5～15ml with water saturated normal butyl alcohol; Merge butanol solution, with normal butyl alcohol saturation water washing 2～4 times, each 5～15ml discards water liquid; Obtain normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 0.5～1.5ml makes dissolving, gets supernatant as reference substance solution; Draw each 5～10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate with the preparation of 1% sodium hydroxide solution, with normal butyl alcohol: glacial acetic acid: water=8～10:1.7～2.3:10～12 upper strata liquid are developping agent; Launch, take out, dry; Spray is with 10% 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 principal spot of same color;
(5) discriminating of menthol
These article of getting 15～25ml adds 60～90 ℃ of sherwood oil 30～50ml joltings and extracts 1～2 time, gets extract, waves and is dissipated to 1～2ml, as need testing solution; Other gets the menthol reference substance, adds 60～90 ℃ of sherwood oils and processes the solution that every 1ml contains menthol 2mg, as reference substance solution; Draw each 5～8 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane: ethyl acetate=22～28: 3.5～4.5 is developping agent; Launch, take out, dry; Spray is with 2% vanillic aldehyde sulfuric acid solution: ethanol=0.8～1.2: 3.5～4.5 mixed solution, 105 ℃ of bakings 5～10 minutes, in the test sample chromatogram; With the corresponding position of reference substance chromatogram on, show the spot of same color;
(6) assay of ammonium chloride
These article of getting 15～25ml puts in the 100ml measuring bottle, adds water 50～90ml and activated charcoal 1.5～2.5g, places 10～30 minutes; Jolting constantly adds water to scale, shakes up, and filters with dry filter paper; Discard filtrating just, precision is measured subsequent filtrate 25ml, adds potassium chromate indicator solution 0.5ml; With the titration of 0.1mol/L silver nitrate solution, with among the every 1ml of 0.1mol/L silver nitrate titration liquid with 3.545mg ammonium chloride be standard, can calculate the content of ammonium chloride in these article;
These article chloride calculates with total chlorine amount and should be 1.27～1.60% (g/ml).
2. Sufi according to claim 1 coughs the detection method of syrup, it is characterized in that, detection method comprises following project more specifically:
(1) discriminating of ammonium chloride
These article of getting 2ml adds water 10ml, after adding nitric acid and making into acidity, adds silver nitrate test solution 2ml, promptly generates the curdy precipitate of white, adds ammonia solution again, and deposition i.e. dissolving; With
/Or
These article of getting 10ml, after hydro-oxidation sodium test solution makes alkalize, heating, it is smelly that ammonia promptly takes place, and can make moistening litmus red test paper become blue;
(2) discriminating of the root bark of white mulberry
These article of getting 30ml puts and is evaporated to nearly thick paste shape in the water-bath, adds ethanol 50ml, and sonicated 20 minutes is centrifugal; Get the supernatant evaporate to dryness, add saturated sodium carbonate solution 20ml, sonicated 20 minutes filters, and filtrating adds watery hydrochloric acid and regulates pH value to 1～2; Left standstill 30 minutes, and filtered, filtrating is extracted 2 times with the ethyl acetate jolting, each 10ml; Combined ethyl acetate liquid, evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution; Other gets root bark of white mulberry control medicinal material 1g and is ground into meal, adds saturated sodium carbonate solution 20ml, shines medicinal material solution in pairs with legal system; Draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with 30～60 ℃ of sherwood oils: ethyl acetate=12: 7 is a developping agent; Launch, take out, dry; Put under the ultraviolet lamp that wavelength is 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
(3) discriminating of balloonflower root
These article of getting 40ml, thin up are to 100ml, and be centrifugal, gets supernatant, through D
101Macroporous adsorptive resins, it is colourless that water is eluted to eluent, discards water liquid, uses 70% ethanol 100ml wash-out again, collects eluent; Evaporate to dryness adds 7% sulfuric acid ethanol: water=1:3 mixed liquor 20ml, and reflux 3 hours is put coldly, extracts 2 times with the methenyl choloride jolting; Each 20ml merges methenyl choloride liquid, adds ammonia solution 30ml washing, discards washing lotion; Methenyl choloride liquid filters with the filter paper that a small amount of anhydrous sodium sulfate is housed, the filtrating evaporate to dryness, and residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets balloonflower root control medicinal material 1g and is ground into meal, adds 7% sulfuric acid ethanol: water=1:3 mixed liquor 20ml, shine medicinal material solution in pairs with legal system; Draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with methenyl choloride: ether=5: 4 is a developping agent; Launch, take out, dry; Put under the ultraviolet lamp that wavelength is 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
(4) discriminating of Radix Glycyrrhizae
These article of getting 10ml, thin up are to 30ml, and be centrifugal, gets supernatant, through D
101The type macroporous adsorptive resins, it is colourless that water is eluted to eluent, discards water liquid, uses 60% ethanol 60ml wash-out again, collects eluent; Evaporate to dryness, residue add water 10ml makes dissolving, extracts 2 times with water saturated normal butyl alcohol, each 10ml; Merge normal butyl alcohol liquid, with the saturated water washing of normal butyl alcohol 2 times, 10ml discards water liquid at every turn; Obtain normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, gets supernatant as need testing solution; Extracting liquorice control medicinal material 1g adds ethanol 20ml in addition, and reflux 30 minutes filters, and gets filtrating; Evaporate to dryness, residue add water 10ml makes dissolving, extracts 2 times with water saturated normal butyl alcohol, each 10ml; Merge butanol solution, with normal butyl alcohol saturation water washing 2 times, each 10ml discards water liquid; Obtain normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, gets supernatant as reference substance solution; Draw each 8 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate with the preparation of 1% sodium hydroxide solution, with normal butyl alcohol: glacial acetic acid: water=9:2:11 upper strata liquid is developping agent; Launch, take out, dry; Spray is with 10% 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 principal spot of same color;
(5) discriminating of menthol
These article of getting 20ml adds 60～90 ℃ of sherwood oil 40ml joltings and extracts 1 time, gets extract, waves and is dissipated to 1ml, as need testing solution; Other gets the menthol reference substance, adds 60～90 ℃ of sherwood oils and processes the solution that every 1ml contains menthol 2 ㎎, as reference substance solution; Drawing each 6 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developping agent with cyclohexane: ethyl acetate=25:4; Launch, take out, dry; Spray is with 2% vanillic aldehyde sulfuric acid solution: the mixed solution of ethanol=1: 4,105 ℃ of bakings 8 minutes, in the test sample chromatogram; With the corresponding position of reference substance chromatogram on, show the spot of same color;
(6) assay of ammonium chloride
These article of getting 20ml puts in the 100ml measuring bottle, adds water 70ml and activated charcoal 2g, places 15 minutes; Jolting constantly adds water to scale, shakes up, and filters with dry filter paper; Discard filtrating just, precision is measured subsequent filtrate 25ml, adds potassium chromate indicator solution 0.5ml; With the titration of 0.1mol/L silver nitrate solution, with among the every 1ml of 0.1mol/L silver nitrate titration liquid with 3.545mg ammonium chloride be standard, can calculate the content of ammonium chloride in these article;
These article chloride calculates with total chlorine amount and should be 1.27～1.60% (g/ml).
3. Sufi according to claim 1 and 2 coughs the detection method of syrup, it is characterized in that the D in step (3) and the step (4)
101Type macroporous adsorptive resins internal diameter is 15mm, and height is 12cm.
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Application publication date: 20121031 |