CN1895378A - Quality control for aqueous donkey-hide gelatin and Chinese angelica preparation - Google Patents
Quality control for aqueous donkey-hide gelatin and Chinese angelica preparation Download PDFInfo
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Abstract
A quality control method for the Chinese medicine 'Agui blood-nourishing liquid' includes such areas as discriminating its characteristics, the thin-layer chromatographic discriminating of Chinese angelica root, astragalus root, liquorice root and white peony root, and measuring the content of ferularic acid contained in Chinese angelica root.
Description
Technical field: the present invention relates to a kind of method of quality control of aqueous donkey-hide gelatin and Chinese angelica preparation, belong to the technical field of medicine being carried out quality control.
Background technology: 'Aguiyangxue ' is a kind of Chinese patent medicine of classics, mainly contains effects such as benefiting qi and nourishing blood, is used for deficiency of qi and blood, and shallow complexion is dizzy weak, wasting, amenorrhea, the inferior disease of red and white leukorrhea.Wherein EGUIYANGXUE granule publication is the 12nd of Drug Standard of Ministry of Public Health of the Peoples Republic of China " Chinese traditional patent formulation preparation ", and this granule uses for many years clinically, obtained satisfied therapeutic effect.But find that after deliberation existing 'Aguiyangxue ' exists that method of quality control is simple, the uppity shortcoming of product quality, in process of producing product, can not effectively control the quality of said preparation with this method of quality control, thereby will influence its clinical efficacy.
Summary of the invention:
The objective of the invention is to: the method for quality control that a kind of aqueous donkey-hide gelatin and Chinese angelica preparation is provided, the present invention is directed to simple, the uppity shortcoming of product quality of original EGUIYANGXUE granular mass control criterion, method of quality control to this preparation is studied, the thin layer chromatography that has increased content of ferulic acid mensuration and Radix Angelicae Sinensis in the Radix Angelicae Sinensis, the Radix Astragali, Radix Glycyrrhizae, Radix Paeoniae Alba four Chinese medicine material is differentiated, improve the quality control standard of 'Aguiyangxue ', thereby guaranteed the clinical efficacy of said preparation.
Aqueous donkey-hide gelatin and Chinese angelica preparation of the present invention comprises syrup and oral liquid; Described preparation is according to part by weight, by Radix Angelicae Sinensis 100-300, Radix Codonopsis 5-20, Radix Paeoniae Alba 5-20, Radix Glycyrrhizae (processed with honey) 2-10, Poria 5-20, Radix Astragali 5-20, Radix Rehmanniae Preparata 5-20, Rhizoma Chuanxiong 2-10 and Colla Corii Asini 5-20 make, its preparation method is: get Radix Angelicae Sinensis, Radix Codonopsis, the Radix Paeoniae Alba, Radix Glycyrrhizae, Poria, the Radix Astragali, Radix Rehmanniae Preparata becomes coarse powder with Rhizoma Chuanxiong eight flavor pulverizing medicinal materials, mixing, according to the percolation under Chinese Pharmacopoeia fluid extract and the extractum item, make solvent with 40-85% ethanol, flooded 12-60 hour, slowly percolation is collected the liquid of filtering, and reclaims ethanol, concentrate, after the placement, collect the grease of come-up, device is preserved in addition; Medicinal residues decoct with water, and filter, and filtrate is left standstill.Merge above-mentioned two kinds of medicinal liquids, add the Colla Corii Asini solution after adjuvant and water dissolve, stir evenly, add above-mentioned grease, boiled 10-60 minute, filter, add water and adjust total amount to 1000ml, promptly.
Method of quality control of the present invention mainly comprise in character, discriminating, inspection and the assay project partly or entirely; Wherein differentiate the thin layer chromatography discriminating that comprises Radix Angelicae Sinensis, the Radix Astragali, Radix Glycyrrhizae and white Peony Root in the preparation; Assay is that the contained content of ferulic acid of Radix Angelicae Sinensis in the preparation is measured.
The discrimination method of Radix Angelicae Sinensis is to be contrast with the ferulic acid reference substance, and with 60-90 ℃ of petroleum ether: ethyl acetate: glacial acetic acid=5-20: 1-10: 0.1-2 is the thin layer chromatography of developing solvent.
The discrimination method of the Radix Astragali, Radix Glycyrrhizae is to be contrast with astragaloside reference substance, Radix Glycyrrhizae control medicinal material, and with chloroform: lower floor's solution of methanol or acetonitrile: water=5-20: 1-10: 0.5-5 is the thin layer chromatography of developing solvent.
The discrimination method of the Radix Paeoniae Alba is to be contrast with the peoniflorin reference substance, and with chloroform: ethyl acetate: methanol or acetonitrile: formic acid=30-50: 1-10: 5-20: 0.1-1 is the thin layer chromatography of developing solvent.
Concrete discrimination method comprises the part or all of of following project:
(1) get this preparation 2-10ml, add methanol 2-20ml, shake up, add petroleum ether 1-10ml again, jolting is extracted, and divides and gets petroleum ether liquid, volatilizes, and residue adds 1～10 of 1% vanillin sulfuric acid solution, shows pale brown color, after the placement, fades to reddish violet;
(2) get this preparation 2-20ml, extract 1-6 time with the ether jolting, merge ether solution, extract 1-5 time, merge alkali liquor with the jolting of 1-10% sodium bicarbonate solution, regulate pH value to 1～6 with dilute hydrochloric acid, the jolting of reuse ether is extracted 1-5 time, merges ether solution, evaporate to dryness, residue adds ethanol 0.5-5ml makes dissolving, as need testing solution; Other gets the ferulic acid reference substance, adds ethanol and makes the solution that every 1ml contains 0.5-3mg, in contrast product solution; Draw each 5-25 μ l of need testing solution and reference substance solution respectively, according to the test of Chinese Pharmacopoeia thin layer chromatography, put respectively in same be the silica gel G of adhesive with the sodium carboxymethyl cellulose
254On the lamellae, with 60-90 ℃ of petroleum ether: ethyl acetate: glacial acetic acid=5-20: 1-10: 0.1-2 is developing solvent, launches, and takes out, and dries, and spray is with phosphomolybdic acid sulphuric acid test solution, and it is clear that hot blast blows to the speckle colour developing, inspects under the daylight; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(3) get this preparation 10-50ml, the 10-100ml jolting that adds diethyl ether is extracted, and divides the water intaking layer, add water saturated n-butyl alcohol jolting and extract 1-5 time, merge n-butyl alcohol liquid, wash with water 1-5 time, n-butyl alcohol liquid evaporate to dryness, add dissolve with methanol, by the neutral alumina post, with 20-80% methanol solution eluting, collect eluent, evaporate to dryness, residue add methanol 0.2-3ml makes dissolving, as need testing solution; Extracting liquorice control medicinal material 0.1-0.5g extracts 1-5 time with the n-butyl alcohol jolting, merges n-butyl alcohol liquid, washes with water 1-5 time, and n-butyl alcohol liquid evaporate to dryness adds methanol 0.5-3ml and makes dissolving, in contrast medical material solution; Other gets the astragaloside reference substance, adds methanol and makes the solution that every 1ml contains 0.5-5mg, in contrast product solution; Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 1-20 μ l of need testing solution, reference substance solution and control medicinal material solution respectively, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform: lower floor's solution of methanol or acetonitrile: water=5-20: 1-10: 0.5-5 is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃, inspects under the daylight; In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
(4) get this preparation 10-40ml, add ethyl acetate extraction 1-5 time, discard ethyl acetate layer, water layer merges n-butanol layer with water saturated n-butanol extraction 1-5 time, with the saturated washing of n-butyl alcohol 1-5 time, get n-butanol layer and volatilize, residue is with methanol 0.2-2ml dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 0.5-5mg, in contrast product solution; Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 5-20 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform: ethyl acetate: methanol or acetonitrile: formic acid=30-50: 1-10: 5-20: 0.1-1 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
The content of ferulic acid assay method is to be contrast with the ferulic acid reference substance in the Radix Angelicae Sinensis, and fine with methanol or second: 0.05-0.2% phosphoric acid solution=10-90: 90-10 is the high performance liquid chromatography of mobile phase.
Concrete content assaying method is:
According to the Chinese Pharmacopoeia high effective liquid chromatography for measuring:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Methanol or second are fine: 0.05-0.2% phosphoric acid solution=10-90: 90-10 is a mobile phase; The detection wavelength is 324nm; Number of theoretical plate must not calculate with the ferulic acid peak and is lower than 5000;
The preparation of reference substance solution: it is an amount of to get the ferulic acid reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 5-20 μ g, in contrast product solution;
The preparation of need testing solution: precision is measured this preparation 1-10ml, puts in the 25ml measuring bottle, adds methanol to scale, shakes up, and with the microporous filter membrane filtration of 0.45 μ m, gets subsequent filtrate, promptly;
Algoscopy: accurate respectively reference substance solution and each 5-25 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
In this preparation, the every 1ml of syrup contains Radix Angelicae Sinensis with ferulic acid C
10H
10O
4Meter must not be less than 0.020mg; The every 1ml of oral liquid contains Radix Angelicae Sinensis with ferulic acid C
10H
10O
4Meter must not be less than 0.010mg.
Described method of quality control comprises:
Character:
For syrup: be auburn thick liquid; Feeble QI perfume (or spice), distinguish the flavor of sweet, puckery, little hardship, suffering;
For oral liquid: be the liquid of brown; Feeble QI perfume (or spice), distinguish the flavor of sweet, puckery, little hardship, suffering;
Differentiate: (1) gets this preparation 2-10ml, adds methanol 2-20ml, shakes up, and adds petroleum ether 1-10ml again, and jolting is extracted, and divides and gets petroleum ether liquid, volatilizes, and residue adds 1～10 of 1% vanillin sulfuric acid solution, shows pale brown color, after the placement, fades to reddish violet;
(2) get this preparation 2-20ml, extract 1-6 time with the ether jolting, merge ether solution, extract 1-5 time, merge alkali liquor with the jolting of 1-10% sodium bicarbonate solution, regulate pH value to 1～6 with dilute hydrochloric acid, the jolting of reuse ether is extracted 1-5 time, merges ether solution, evaporate to dryness, residue adds ethanol 0.5-5ml makes dissolving, as need testing solution; Other gets the ferulic acid reference substance, adds ethanol and makes the solution that every 1ml contains 0.5-3mg, in contrast product solution; Draw each 5-25 μ l of need testing solution and reference substance solution respectively, according to the test of Chinese Pharmacopoeia thin layer chromatography, put respectively in same be the silica gel G of adhesive with the sodium carboxymethyl cellulose
254On the lamellae, with 60-90 ℃ of petroleum ether: ethyl acetate: glacial acetic acid=5-20: 1-10: 0.1-2 is developing solvent, launches, and takes out, and dries, and spray is with phosphomolybdic acid sulphuric acid test solution, and it is clear that hot blast blows to the speckle colour developing, inspects under the daylight; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(3) get this preparation 10-50ml, the 10-100ml jolting that adds diethyl ether is extracted, and divides the water intaking layer, add water saturated n-butyl alcohol jolting and extract 1-5 time, merge n-butyl alcohol liquid, wash with water 1-5 time, n-butyl alcohol liquid evaporate to dryness, add dissolve with methanol, by the neutral alumina post, with 20-80% methanol solution eluting, collect eluent, evaporate to dryness, residue add methanol 0.2-3ml makes dissolving, as need testing solution; Extracting liquorice control medicinal material 0.1-0.5g extracts 1-5 time with the n-butyl alcohol jolting, merges n-butyl alcohol liquid, washes with water 1-5 time, and n-butyl alcohol liquid evaporate to dryness adds methanol 0.5-3ml and makes dissolving, in contrast medical material solution; Other gets the astragaloside reference substance, adds methanol and makes the solution that every 1ml contains 0.5-5mg, in contrast product solution; Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 1-20 μ l of need testing solution, reference substance solution and control medicinal material solution respectively, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform: lower floor's solution of methanol or acetonitrile: water=5-20: 1-10: 0.5-5 is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃, inspects under the daylight; In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
(4) get this preparation 10-40ml, add ethyl acetate extraction 1-5 time, discard ethyl acetate layer, water layer merges n-butanol layer with water saturated n-butanol extraction 1-5 time, with the saturated washing of n-butyl alcohol 1-5 time, get n-butanol layer and volatilize, residue is with methanol 0.2-2ml dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 0.5-5mg, in contrast product solution; Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 5-20 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform: ethyl acetate: methanol or acetonitrile: formic acid=30-50: 1-10: 5-20: 0.1-1 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Check: relative density is got syrup 5-20g, add water 10-50ml dilution after, measure according to Chinese Pharmacopoeia relative density algoscopy, should be not less than 1.09;
Other should meet every regulation relevant under Chinese Pharmacopoeia syrup or the oral liquid item;
Assay: shine the Chinese Pharmacopoeia high effective liquid chromatography for measuring:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Methanol or second are fine: 0.05-0.2% phosphoric acid solution=10-90: 90-10 is a mobile phase; The detection wavelength is 324nm; Number of theoretical plate must not calculate with the ferulic acid peak and is lower than 5000;
The preparation of reference substance solution: it is an amount of to get the ferulic acid reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 5-20 μ g, in contrast product solution;
The preparation of need testing solution: precision is measured this preparation 1-10ml, puts in the 25ml measuring bottle, adds methanol to scale, shakes up, and with the microporous filter membrane filtration of 0.45 μ m, gets subsequent filtrate, promptly;
Algoscopy: accurate respectively reference substance solution and each 5-25 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
In this preparation, the every 1ml of syrup contains Radix Angelicae Sinensis with ferulic acid C
10H
10O
4Meter must not be less than 0.020mg; The every 1ml of oral liquid contains Radix Angelicae Sinensis with ferulic acid C
10H
10O
4Meter must not be less than 0.010mg.
In order to ensure method of quality control science of the present invention, reasonable, feasible, Radix Angelicae Sinensis, the Radix Paeoniae Alba, the Radix Astragali, Radix Glycyrrhizae etc. have carried out the thin layer chromatography Study on Identification among the applicant the other side, have determined discrimination method; And increased the contained content of ferulic acid mensuration of Radix Angelicae Sinensis medical material in the preparation, specifically test as follows:
One, ferulaic acid content study on determination method
1, need testing solution preparation method research:
Get this preparation 5ml, put in the 25ml measuring bottle, add methanol to scale, shake up, with the microporous filter membrane filtration of 0.45 μ m, get subsequent filtrate, measure its ferulaic acid content, measurement result sees the following form.
Different influences (n=3) of extracting solvent to ferulaic acid content mensuration
| Solvent | Ethanol | Methanol | |
| Oral liquid | Average content (mg/g) | 0.0549 | 0.0704 |
| RSD(％) | 1.20 | 0.95 | |
| Syrup | Average content (mg/g) | 0.0892 | 0.1005 |
| RSD(％) | 1.17 | 0.83 | |
Result of the test shows, uses methanol extraction, and ferulic acid extracts comparatively complete.
2, the selection of mobile phase:
Mobile phase 1: the mixed solution with methanol, phosphoric acid solution different proportion is a mobile phase;
Mobile phase 2: the mixed solution with acetonitrile, phosphoric acid solution different proportion is a mobile phase;
Mobile phase 3: the mixed solution with acetonitrile, water different proportion is a mobile phase;
Mobile phase 4: the mixed solution with methanol, water, glacial acetic acid different proportion is a mobile phase;
Result: fine with methanol or second: 0.05-0.2% phosphoric acid solution=10-90: 90-10 is a mobile phase, and the negative sample chromatogram is at non-false positive peak, place, ferulic acid peak position; The ferulic acid peak separates fully (separating degree＞1.5) with close impurity peaks.Optimal flow is mutually: acetonitrile: 0.085% phosphoric acid solution=16: 84.
3, repeatability test
Accurate this preparation 3ml that draws, the preparation method by test liquid under the assay item among the present invention prepares 5 parts of test liquids respectively, and sample introduction is measured peak area, and the ferulic acid average content is 0.1017mg/ml, and RSD is 0.98%.Show that repeatability is good, the results are shown in following table.
The replica test of ferulic acid in the preparation test sample
| The sample introduction number of times | 1 | 2 | 3 | 4 | 5 | Meansigma methods | RSD(％) |
| Peak area | 0.1006 | 0.1021 | 0.1018 | 0.1031 | 0.1009 | 0.1017 | 0.98 |
4, precision test
Accurate ferulic acid reference substance solution (10.42 μ g/ml) the 10 μ l that draw inject chromatograph of liquid, measure peak area, repeat sample introduction 5 times, and average peak area is 498354, and RSD is 1.25%.Show that precision is good, the results are shown in following table.
The test of ferulic acid reference substance solution precision
| The sample introduction number of times | 1 | 2 | 3 | 4 | 5 | Meansigma methods | RSD(％) |
| Peak area | 509147 | 497875 | 495844 | 493887 | 495015 | 498354 | 1.25 |
5, recovery test
Adopt the application of sample absorption method, accurate respectively this preparation (average content is 0.1017mg/ml) of drawing is put in the tool plug conical flask, (with methanol is solvent to accurate adding ferulic acid reference substance, make that to contain ferulic acid be 32.44 μ g/ml) solution 5ml, press the quality standard draft, make test liquid.The accurate respectively 10 μ l of absorption inject chromatograph of liquid, and the record chromatogram is measured content, and calculate recovery rate sees the following form.Average recovery rate is 99.64%, and RSD is 0.69%, proves that this method is feasible.
Ferulic acid is measured recovery test in the need testing solution
| Experiment number | Sample size (ml) | Contain ferulic acid (mg) | Add ferulic acid (mg) | The amount of recording (mg) | The response rate (%) | Average recovery rate (%) | RSD (％) |
| 1 | 1 | 0.15255 | 0.1622 | 0.3119 | 99.09 | 99.64 | 0.69 |
| 2 | 1 | 0.15255 | 0.3133 | 99.54 | |||
| 3 | 1 | 0.15255 | 0.3138 | 99.70 | |||
| 4 | 1 | 0.15255 | 0.3119 | 99.09 | |||
| 5 | 1 | 0.15255 | 0.3172 | 100.78 |
Two, Radix Angelicae Sinensis thin layer Study on Identification
With Radix Angelicae Sinensis medical material in the ferulic acid reference substance discriminating side.
The thing of getting it filled extracts 3 times with the ether jolting, merges ether solution, with 5% sodium bicarbonate solution jolting extraction 3 times, merge alkali liquor, regulate pH value to 2～3 with dilute hydrochloric acid, the jolting of reuse ether is extracted 3 times, merges ether solution, evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution.Get the negative test sample that lacks Radix Angelicae Sinensis, get negative need testing solution with legal system.Other gets the ferulic acid reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution.According to Chinese Pharmacopoeia thin layer chromatography test, draw above-mentioned need testing solution, negative need testing solution and reference substance solution, put respectively in samely with the sodium carboxymethyl cellulose be on the adhesive silica gel g thin-layer plate, silica gel G
254On, respectively with the mixed solution of benzene, methanol, glacial acetic acid different proportion; Mixed solution with petroleum ether (60-90 ℃), ethyl acetate, glacial acetic acid different proportion is developing solvent.
With benzene, methanol, glacial acetic acid is developing solvent, feminine gender have mostly disturb or the speckle separating degree bad.With 60-90 ℃ of petroleum ether: ethyl acetate: glacial acetic acid=5-20: 1-10: 0.1-2 is developing solvent, put on same silica gel g thin-layer plate, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color, but speckle is fuzzyyer; Point is in same silica gel G
254On the lamellae, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, the speckle that shows same color, and good separating effect, clear spot, negative control is noiseless, the method favorable reproducibility, and best developing solvent is a 60-90 ℃ of petroleum ether: ethyl acetate: glacial acetic acid=12: 5: 0.6.
Three, the Radix Astragali, Radix Glycyrrhizae thin layer Study on Identification
With licorice medicinal materials in Milkvetch Root, the Radix Glycyrrhizae control medicinal material discriminating side in the astragaloside reference substance discriminating side.
The thing of getting it filled, the jolting that adds diethyl ether is extracted, and divides the water intaking layer, add water saturated n-butyl alcohol jolting and extract 2 times, merge n-butyl alcohol liquid, wash with water 2 times, n-butyl alcohol liquid evaporate to dryness adds dissolve with methanol, by neutral alumina post (100～120 orders, 5g, internal diameter 10mm), with 40% methanol solution 100ml eluting, collect eluent, evaporate to dryness, residue add methanol 0.5ml makes dissolving, as need testing solution; Get scarce Radix Glycyrrhizae negative sample, make scarce Radix Glycyrrhizae negative control test liquid with method; Other gets Radix Astragali negative sample, makes with method to lack Radix Astragali negative control test liquid; The extracting liquorice control medicinal material extracts 3 times with the n-butyl alcohol jolting again, merges n-butyl alcohol liquid, washes with water 2 times, each 20ml, and n-butyl alcohol liquid evaporate to dryness adds methanol 1ml and makes dissolving, in contrast medical material solution; Get the astragaloside reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution.Test according to the Chinese Pharmacopoeia thin layer chromatography, draw need testing solution respectively, lack Radix Astragali negative control solution, lack the Radix Glycyrrhizae negative control solution each, reference substance solution and control medicinal material solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, respectively with the mixed solution of ethyl acetate, formic acid, glacial acetic acid, water different proportion; Mixed solution with chloroform, acetonitrile, water different proportion; Mixed solution with chloroform, methanol, water different proportion is expansion.
Result: with chloroform: lower floor's solution of methanol or acetonitrile: water=5-20: 1-10: 0.5-5 is developing solvent, spray is with 10% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing at 105 ℃, put respectively under the daylight and inspect, inspect under the ultraviolet light 365nm, in the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color, but it is a little less than the spot intensity, unintelligible; Under daylight, inspect, in the test sample chromatograph, with reference substance, the corresponding position of control medicinal material chromatograph on, show the speckle of same color, clear spot, separating degree is good, negative noiseless, repeatability is good.Best developing solvent is a chloroform: methanol: lower floor's solution of water=13: 6: 2.
Four, Radix Paeoniae Alba thin layer Study on Identification
With white Peony Root in the peoniflorin reference substance discriminating side.
Need testing solution preparation method one, the thing of getting it filled, evaporate to dryness added the ethanol jolting 5 minutes, filtered, and filtrate evaporate to dryness, residue add ethanol makes dissolving, as need testing solution; Get the negative test sample that lacks the Radix Paeoniae Alba, get negative need testing solution with legal system.
Need testing solution preparation method two, the thing of getting it filled are used extracted with diethyl ether 3 times, abandon ether layer, water layer merges n-butanol layer with water saturated n-butanol extraction 2 times, with the saturated washing of n-butyl alcohol 2 times, get the n-butanol layer evaporate to dryness, the residue dissolve with ethanol is as need testing solution; Get the negative test sample that lacks the Radix Paeoniae Alba, get negative need testing solution with legal system.
Need testing solution preparation method three, the thing of getting it filled add ethyl acetate extraction 3 times, abandon the ethyl acetate layer, water layer merges n-butanol layer with water saturated n-butanol extraction 3 times, with the saturated washing of n-butyl alcohol 3 times, get n-butanol layer and volatilize, the residue dissolve with methanol is as need testing solution.Get the peoniflorin reference substance, add ethanol and make every 1ml and contain 1mg solution, in contrast product solution.
According to Chinese Pharmacopoeia thin layer chromatography test, draw each 10 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, respectively with the mixed solution of chloroform, ethyl acetate, methanol, formic acid different proportion; Mixed solution with chloroform, ethyl acetate, acetonitrile, formic acid different proportion is developing solvent, launches, and takes out, and dries, and spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing, and daylight is inspected.
The result shows that the test sample speckled background disturbs greatly in the method one, and speckle is unintelligible; The method two speckled background disturbs big, and speckle is unintelligible, and feminine gender has interference; Method three clear spots, the good feminine gender of separating degree is noiseless, favorable reproducibility.Developing solvent preferably is: chloroform: ethyl acetate: methanol or acetonitrile: formic acid=30-50: 1-10: 5-20: 0.1-1; Best developing solvent is a chloroform: ethyl acetate: methanol: formic acid=40: 5: 10: 0.2.
Compared with prior art, method of quality control of the present invention has increased the thin layer chromatography of content of ferulic acid mensuration and Radix Angelicae Sinensis in the Radix Angelicae Sinensis, the Radix Astragali, Radix Glycyrrhizae, Radix Paeoniae Alba four Chinese medicine material and has differentiated, the method precision height that is adopted, favorable reproducibility, good stability, response rate height has improved the quality control standard of 'Aguiyangxue ', thereby has guaranteed the clinical efficacy of said preparation.
Further specify the present invention by the following examples, but not as limitation of the present invention.
The specific embodiment:
Embodiments of the invention 1: the method for quality control of described syrup comprises:
Character: this preparation is auburn thick liquid; Feeble QI perfume (or spice), distinguish the flavor of sweet, puckery, little hardship, suffering;
Differentiate: (1) gets this preparation 5ml, adds methanol 5ml, shakes up, and adds petroleum ether 5ml again, and jolting is extracted, and divides and gets petroleum ether liquid, volatilizes, and residue adds 1～2 of 1% vanillin sulfuric acid solution, shows pale brown color, after the placement, fades to reddish violet;
(2) get this preparation 10ml, extract 3 (15ml, 10ml with the ether jolting, 10ml), merge ether solution, extract 3 times with 5% sodium bicarbonate solution jolting, each 15ml merges alkali liquor, regulates pH value to 2～3 with dilute hydrochloric acid, the jolting of reuse ether is extracted 3 times, each 15ml merges ether solution, evaporate to dryness, residue adds ethanol 1ml makes dissolving, as need testing solution; Other gets the ferulic acid reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Draw test sample 8 μ l, reference substance solution 5 μ l, according to the test of Chinese Pharmacopoeia thin layer chromatography, put respectively in same be the silica gel G of adhesive with the sodium carboxymethyl cellulose
254On the lamellae, with 60-90 ℃ of petroleum ether: ethyl acetate: glacial acetic acid=12: 5: 0.6 is developing solvent, launches, and takes out, and dries, and spray is with phosphomolybdic acid sulphuric acid test solution, and it is clear that hot blast blows to the speckle colour developing, inspects under the daylight; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(3) get this preparation 40ml, the 30ml jolting that adds diethyl ether is extracted, and divides the water intaking layer, add water saturated n-butyl alcohol jolting and extract 2 times, each 20ml merges n-butyl alcohol liquid, wash each 20ml, n-butyl alcohol liquid evaporate to dryness with water 2 times, add dissolve with methanol, by the neutral alumina post of 100～120 orders, 5g, internal diameter 10mm, with 40% methanol solution 100ml eluting, collect eluent, evaporate to dryness, residue add methanol 0.5ml makes dissolving, as need testing solution; Extracting liquorice control medicinal material 0.2g extracts 3 times with the n-butyl alcohol jolting, and each 15ml merges n-butyl alcohol liquid, washes with water 2 times, each 20ml; N-butyl alcohol liquid evaporate to dryness adds methanol 1ml and makes dissolving, in contrast medical material solution; Other gets the astragaloside reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 2 μ l of need testing solution 10 μ l, reference substance solution and control medicinal material solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform: methanol: lower floor's solution of water=13: 6: 2 is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃, inspects under the daylight; In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
(4) get this preparation 25ml, add ethyl acetate extraction 3 times, each 25ml discards ethyl acetate layer, water layer is with water saturated n-butanol extraction 3 times, each 20ml merges n-butanol layer, uses the saturated washing of n-butyl alcohol 3 times, each 10ml, get n-butanol layer and volatilize, residue is with methanol 0.5ml dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform: ethyl acetate: methanol: formic acid=40: 5: 10: 0.2 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Check: relative density is got this preparation 10g, add water 20ml dilution after, measure according to Chinese Pharmacopoeia relative density algoscopy, should be not less than 1.09;
Other should meet every regulation relevant under the Chinese Pharmacopoeia syrup item;
Assay: shine the Chinese Pharmacopoeia high effective liquid chromatography for measuring:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Second is fine: 0.085% phosphoric acid solution=16: 84 is a mobile phase; The detection wavelength is 324nm; Number of theoretical plate must not calculate with the ferulic acid peak and is lower than 5000;
The preparation of reference substance solution: it is an amount of to get the ferulic acid reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 10 μ g, in contrast product solution;
The preparation of need testing solution: precision is measured this preparation 3ml, puts in the 25ml measuring bottle, adds methanol to scale, shakes up, and with the microporous filter membrane filtration of 0.45 μ m, gets subsequent filtrate, promptly;
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
The every 1ml of syrup contains Radix Angelicae Sinensis with ferulic acid C
10H
10O
4Meter must not be less than 0.040mg.
Embodiments of the invention 2: the method for quality control of described syrup comprises:
Character: be auburn thick liquid; Feeble QI perfume (or spice), distinguish the flavor of sweet, puckery, little hardship, suffering;
Differentiate: (1) gets syrup 10ml, adds methanol 20ml, shakes up, and adds petroleum ether 10ml again, and jolting is extracted, and divides and gets petroleum ether liquid, volatilizes, and residue adds 10 of 1% vanillin sulfuric acid solutions, shows pale brown color, after the placement, fades to reddish violet;
(2) get syrup 20ml, extract 6 times, merge ether solution, extract 1 time with 10% sodium bicarbonate solution jolting with the ether jolting, alkali liquor is regulated pH value to 6 with dilute hydrochloric acid, and the jolting of reuse ether is extracted 5 times, merges ether solution, evaporate to dryness, residue add ethanol 5ml makes dissolving, as need testing solution; Other gets the ferulic acid reference substance, adds ethanol and makes the solution that every 1ml contains 3mg, in contrast product solution; Draw each 5 μ l of need testing solution and reference substance solution respectively, according to the test of Chinese Pharmacopoeia thin layer chromatography, put respectively in same be the silica gel G of adhesive with the sodium carboxymethyl cellulose
254On the lamellae, with 60-90 ℃ of petroleum ether: ethyl acetate: glacial acetic acid=20: 1: 0.1 is developing solvent, launches, and takes out, and dries, and spray is with phosphomolybdic acid sulphuric acid test solution, and it is clear that hot blast blows to the speckle colour developing, inspects under the daylight; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(3) get syrup 50ml, the 100ml jolting that adds diethyl ether is extracted, and divides the water intaking layer, add water saturated n-butyl alcohol jolting and extract 5 times, merge n-butyl alcohol liquid, wash with water 5 times, n-butyl alcohol liquid evaporate to dryness, add dissolve with methanol, by the neutral alumina post, with 80% methanol solution eluting, collect eluent, evaporate to dryness, residue add methanol 3ml makes dissolving, as need testing solution; Extracting liquorice control medicinal material 0.5g extracts 5 times with the n-butyl alcohol jolting, merges n-butyl alcohol liquid, washes with water 5 times, and n-butyl alcohol liquid evaporate to dryness adds methanol 3ml and makes dissolving, in contrast medical material solution; Other gets the astragaloside reference substance, adds methanol and makes the solution that every 1ml contains 5mg, in contrast product solution; Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 1 μ l of need testing solution, reference substance solution and control medicinal material solution respectively, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform: methanol: lower floor's solution of water=5: 10: 0.5 is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃, inspects under the daylight; In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
(4) get syrup 40ml, add ethyl acetate extraction 5 times, discard ethyl acetate layer, water layer merges n-butanol layer with water saturated n-butanol extraction 5 times, with the saturated washing of n-butyl alcohol 5 times, get n-butanol layer and volatilize, residue is with methanol 2ml dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 5mg, in contrast product solution; Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 20 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform: ethyl acetate: methanol: formic acid=30: 1: 20: 1 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Check: relative density is got syrup 20g, add water 50ml dilution after, measure according to Chinese Pharmacopoeia relative density algoscopy, should be not less than 1.09;
Other should meet every regulation relevant under the Chinese Pharmacopoeia syrup item;
Assay: shine the Chinese Pharmacopoeia high effective liquid chromatography for measuring:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Methanol: 0.2% phosphoric acid solution=90: 10 is a mobile phase; Detecting wavelength and be the 324nm number of theoretical plate must not calculate with the ferulic acid peak and is lower than 5000;
The preparation of reference substance solution: it is an amount of to get the ferulic acid reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 20 μ g, in contrast product solution;
The preparation of need testing solution: precision is measured syrup 10ml, puts in the 25ml measuring bottle, adds methanol to scale, shakes up, and with the microporous filter membrane filtration of 0.45 μ m, gets subsequent filtrate, promptly;
Algoscopy: accurate respectively reference substance solution and each 25 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
The every 1ml of syrup contains Radix Angelicae Sinensis with ferulic acid C
10H
10O
4Meter must not be less than 0.020mg.
Embodiments of the invention 3: the method for quality control of described oral liquid comprises:
Character: be the liquid of brown; Feeble QI perfume (or spice), distinguish the flavor of sweet, puckery, little hardship, suffering;
Differentiate: (1) gets oral liquid 2ml, adds methanol 2ml, shakes up, and adds petroleum ether 1ml again, and jolting is extracted, and divides and gets petroleum ether liquid, volatilizes, and residue adds 1 of 1% vanillin sulfuric acid solution, shows pale brown color, after the placement, fades to reddish violet;
(2) get oral liquid 2ml, extract 1 time, merge ether solution, extract 5 times with 1% sodium bicarbonate solution jolting with the ether jolting, merge alkali liquor, regulate pH value to 1 with dilute hydrochloric acid, the jolting of reuse ether is extracted 1 time, ether solution evaporate to dryness, residue add ethanol 0.5ml makes dissolving, as need testing solution; Other gets the ferulic acid reference substance, adds ethanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; Draw each 25 μ l of need testing solution and reference substance solution respectively, according to the test of Chinese Pharmacopoeia thin layer chromatography, put respectively in same be the silica gel G of adhesive with the sodium carboxymethyl cellulose
254On the lamellae, with 60-90 ℃ of petroleum ether: ethyl acetate: glacial acetic acid=5: 10: 2 is developing solvent, launches, and takes out, and dries, and spray is with phosphomolybdic acid sulphuric acid test solution, and it is clear that hot blast blows to the speckle colour developing, inspects under the daylight; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(3) get oral liquid 10ml, the 10ml jolting that adds diethyl ether is extracted, and divides the water intaking layer, adding water saturated n-butyl alcohol jolting extracts 1 time, n-butyl alcohol liquid washes with water 1 time, and n-butyl alcohol liquid evaporate to dryness adds dissolve with methanol, by the neutral alumina post, with 20% methanol solution eluting, collect eluent, evaporate to dryness, residue adds methanol 0.2ml makes dissolving, as need testing solution; Extracting liquorice control medicinal material 0.1g extracts 1 time with the n-butyl alcohol jolting, and n-butyl alcohol liquid washes with water 1 time, and n-butyl alcohol liquid evaporate to dryness adds methanol 0.5ml and makes dissolving, in contrast medical material solution; Other gets the astragaloside reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 1 μ l of need testing solution, reference substance solution and control medicinal material solution respectively, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform: acetonitrile: lower floor's solution of water=20: 1: 5 is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃, inspects under the daylight; In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
(4) get oral liquid 10ml, add ethyl acetate extraction 1 time, discard ethyl acetate layer, water layer is with water saturated n-butanol extraction 1 time, and n-butanol layer is got n-butanol layer and volatilized with the saturated washing of n-butyl alcohol 1 time, and residue is with methanol 0.2ml dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform: ethyl acetate: acetonitrile: formic acid=50: 10: 5: 0.1 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Check: should meet every regulation relevant under the Chinese Pharmacopoeia oral liquid item;
Assay: shine the Chinese Pharmacopoeia high effective liquid chromatography for measuring:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Second is fine: 0.05% phosphoric acid solution=10: 90 is a mobile phase; The detection wavelength is 324nm; Number of theoretical plate must not calculate with the ferulic acid peak and is lower than 5000;
The preparation of reference substance solution: it is an amount of to get the ferulic acid reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 5 μ g, in contrast product solution;
The preparation of need testing solution: precision is measured oral liquid 1ml, puts in the 25ml measuring bottle, adds methanol to scale, shakes up, and with the microporous filter membrane filtration of 0.45 μ m, gets subsequent filtrate, promptly;
Algoscopy: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
The every 1ml of oral liquid contains Radix Angelicae Sinensis with ferulic acid C
10H
10O
4Meter must not be less than 0.010mg.
Embodiments of the invention 4: the method for quality control of described oral liquid can comprise:
Character: be the liquid of brown; Feeble QI perfume (or spice), distinguish the flavor of sweet, puckery, little hardship, suffering;
Differentiate:
(1) gets this preparation 15ml, extract 2 times, merge ether solution, extract 2 times with 6% sodium bicarbonate solution jolting with the ether jolting, merge alkali liquor, regulate pH value to 3 with dilute hydrochloric acid, the jolting of reuse ether is extracted 2 times, merges ether solution, evaporate to dryness, residue add ethanol 2ml makes dissolving, as need testing solution; Other gets the ferulic acid reference substance, adds ethanol and makes the solution that every 1ml contains 2mg, in contrast product solution; Draw each 10 μ l of need testing solution and reference substance solution respectively, according to the test of Chinese Pharmacopoeia thin layer chromatography, put respectively in same be the silica gel G of adhesive with the sodium carboxymethyl cellulose
254On the lamellae, with 60-90 ℃ of petroleum ether: ethyl acetate: glacial acetic acid=15: 5: 0.8 is developing solvent, launches, and takes out, and dries, and spray is with phosphomolybdic acid sulphuric acid test solution, and it is clear that hot blast blows to the speckle colour developing, inspects under the daylight; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(2) get this preparation 15ml, add ethyl acetate extraction 4 times, discard ethyl acetate layer, water layer merges n-butanol layer with water saturated n-butanol extraction 4 times, with the saturated washing of n-butyl alcohol 4 times, get n-butanol layer and volatilize, residue is with methanol 1ml dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform: ethyl acetate: acetonitrile: formic acid=35: 8: 10: 0.7 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Check: should meet every regulation relevant under the Chinese Pharmacopoeia oral liquid item.
Embodiments of the invention 5: the method for quality control of described syrup can comprise:
Character: be auburn thick liquid; Feeble QI perfume (or spice), distinguish the flavor of sweet, puckery, little hardship, suffering;
Check: relative density is got syrup 5-20g, add water 10-50ml dilution after, measure according to Chinese Pharmacopoeia relative density algoscopy, should be not less than 1.09;
Other should meet every regulation relevant under the Chinese Pharmacopoeia syrup item;
Assay: shine the Chinese Pharmacopoeia high effective liquid chromatography for measuring:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Second is fine: 0.1% phosphoric acid solution=65: 35 is a mobile phase; The detection wavelength is 324nm; Number of theoretical plate must not calculate with the ferulic acid peak and is lower than 5000;
The preparation of reference substance solution: it is an amount of to get the ferulic acid reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 10 μ g, in contrast product solution;
The preparation of need testing solution: precision is measured this preparation 5ml, puts in the 25ml measuring bottle, adds methanol to scale, shakes up, and with the microporous filter membrane filtration of 0.45 μ m, gets subsequent filtrate, promptly;
Algoscopy: accurate respectively reference substance solution and each 15 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
The every 1ml of syrup contains Radix Angelicae Sinensis with ferulic acid C
10H
10O
4Meter must not be less than 0.020mg.
Claims (8)
1. the method for quality control of an aqueous donkey-hide gelatin and Chinese angelica preparation, described liquid preparation comprises syrup and oral liquid, it is characterized in that: described method of quality control mainly comprise in character, discriminating, inspection and the assay project partly or entirely; Wherein differentiate the thin layer chromatography discriminating that comprises Radix Angelicae Sinensis, the Radix Astragali, Radix Glycyrrhizae and white Peony Root in the preparation; Assay is that the contained content of ferulic acid of Radix Angelicae Sinensis in the preparation is measured.
2. according to the method for quality control of the described aqueous donkey-hide gelatin and Chinese angelica preparation of claim 1, it is characterized in that: the discrimination method of Radix Angelicae Sinensis is to be contrast with the ferulic acid reference substance, and with 60-90 ℃ of petroleum ether: ethyl acetate: glacial acetic acid=5-20: 1-10: 0.1-2 is the thin layer chromatography of developing solvent.
3. according to the method for quality control of the described aqueous donkey-hide gelatin and Chinese angelica preparation of claim 1, it is characterized in that: the discrimination method of the Radix Astragali, Radix Glycyrrhizae is to be contrast with astragaloside reference substance, Radix Glycyrrhizae control medicinal material, and with chloroform: lower floor's solution of methanol or acetonitrile: water=5-20: 1-10: 0.5-5 is the thin layer chromatography of developing solvent.
4. according to the method for quality control of the described aqueous donkey-hide gelatin and Chinese angelica preparation of claim 1, it is characterized in that: the discrimination method of the Radix Paeoniae Alba is to be contrast with the peoniflorin reference substance, and with chloroform: ethyl acetate: methanol or acetonitrile: formic acid=30-50: 1-10: 5-20: 0.1-1 is the thin layer chromatography of developing solvent.
5. according to the method for quality control of claim 1,2,3 or 4 described aqueous donkey-hide gelatin and Chinese angelica preparations, it is characterized in that: concrete discrimination method comprises the part or all of of following project:
(1) get this preparation 2-10ml, add methanol 2-20ml, shake up, add petroleum ether 1-10ml again, jolting is extracted, and divides and gets petroleum ether liquid, volatilizes, and residue adds 1～10 of 1% vanillin sulfuric acid solution, shows pale brown color, after the placement, fades to reddish violet;
(2) get this preparation 2-20ml, extract 1-6 time with the ether jolting, merge ether solution, extract 1-5 time, merge alkali liquor with the jolting of 1-10% sodium bicarbonate solution, regulate pH value to 1～6 with dilute hydrochloric acid, the jolting of reuse ether is extracted 1-5 time, merges ether solution, evaporate to dryness, residue adds ethanol 0.5-5ml makes dissolving, as need testing solution; Other gets the ferulic acid reference substance, adds ethanol and makes the solution that every 1ml contains 0.5-3mg, in contrast product solution; Draw each 5-25 μ l of need testing solution and reference substance solution respectively, test according to the Chinese Pharmacopoeia thin layer chromatography, put respectively in same be on silica gel G 254 lamellaes of adhesive with the sodium carboxymethyl cellulose, with 60-90 ℃ of petroleum ether: ethyl acetate: glacial acetic acid=5-20: 1-10: 0.1-2 is developing solvent, launches, and takes out, dry, spray is with phosphomolybdic acid sulphuric acid test solution, and it is clear that hot blast blows to the speckle colour developing, inspects under the daylight; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(3) get this preparation 10-50ml, the 10-100ml jolting that adds diethyl ether is extracted, and divides the water intaking layer, add water saturated n-butyl alcohol jolting and extract 1-5 time, merge n-butyl alcohol liquid, wash with water 1-5 time, n-butyl alcohol liquid evaporate to dryness, add dissolve with methanol, by the neutral alumina post, with 20-80% methanol solution eluting, collect eluent, evaporate to dryness, residue add methanol 0.2-3ml makes dissolving, as need testing solution; Extracting liquorice control medicinal material 0.1-0.5g extracts 1-5 time with the n-butyl alcohol jolting, merges n-butyl alcohol liquid, washes with water 1-5 time, and n-butyl alcohol liquid evaporate to dryness adds methanol 0.5-3ml and makes dissolving, in contrast medical material solution; Other gets the astragaloside reference substance, adds methanol and makes the solution that every 1ml contains 0.5-5mg, in contrast product solution; Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 1-20 μ l of need testing solution, reference substance solution and control medicinal material solution respectively, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform: lower floor's solution of methanol or acetonitrile: water=5-20: 1-10: 0.5-5 is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃, inspects under the daylight; In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
(4) get this preparation 10-40ml, add ethyl acetate extraction 1-5 time, discard ethyl acetate layer, water layer merges n-butanol layer with water saturated n-butanol extraction 1-5 time, with the saturated washing of n-butyl alcohol 1-5 time, get n-butanol layer and volatilize, residue is with methanol 0.2-2ml dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 0.5-5mg, in contrast product solution; Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 5-20 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform: ethyl acetate: methanol or acetonitrile: formic acid=30-50: 1-10: 5-20: 0.1-1 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
6. according to the method for quality control of the described aqueous donkey-hide gelatin and Chinese angelica preparation of claim 1, it is characterized in that: the content of ferulic acid assay method is to be contrast with the ferulic acid reference substance in the Radix Angelicae Sinensis, and fine with methanol or second: 0.05-0.2% phosphoric acid solution=10-90: 90-10 is the high performance liquid chromatography of mobile phase.
7. according to the method for quality control of claim 1 or 6 described aqueous donkey-hide gelatin and Chinese angelica preparations, it is characterized in that: described content assaying method is:
According to the Chinese Pharmacopoeia high effective liquid chromatography for measuring:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Methanol or second are fine: 0.05-0.2% phosphoric acid solution=10-90: 90-10 is a mobile phase; The detection wavelength is 324nm; Number of theoretical plate must not calculate with the ferulic acid peak and is lower than 5000;
The preparation of reference substance solution: it is an amount of to get the ferulic acid reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 5-20 μ g, in contrast product solution;
The preparation of need testing solution: precision is measured this preparation 1-10ml, puts in the 25ml measuring bottle, adds methanol to scale, shakes up, and with the microporous filter membrane filtration of 0.45 μ m, gets subsequent filtrate, promptly;
Algoscopy: accurate respectively reference substance solution and each 5-25 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
In this preparation, the every 1ml of syrup contains Radix Angelicae Sinensis in ferulic acid C10H10O4, must not be less than 0.020mg; The every 1ml of oral liquid contains Radix Angelicae Sinensis in ferulic acid C10H10O4, must not be less than 0.010mg.
8. according to the method for quality control of the described aqueous donkey-hide gelatin and Chinese angelica preparation of claim 1, it is characterized in that: described method of quality control comprises:
Character:
For syrup: be auburn thick liquid; Feeble QI perfume (or spice), distinguish the flavor of sweet, puckery, little hardship, suffering;
For oral liquid: be the liquid of brown; Feeble QI perfume (or spice), distinguish the flavor of sweet, puckery, little hardship, suffering;
Differentiate: (1) gets this preparation 2-10ml, adds methanol 2-20ml, shakes up, and adds petroleum ether 1-10ml again, and jolting is extracted, and divides and gets petroleum ether liquid, volatilizes, and residue adds 1～10 of 1% vanillin sulfuric acid solution, shows pale brown color, after the placement, fades to reddish violet;
(2) get this preparation 2-20ml, extract 1-6 time with the ether jolting, merge ether solution, extract 1-5 time, merge alkali liquor with the jolting of 1-10% sodium bicarbonate solution, regulate pH value to 1～6 with dilute hydrochloric acid, the jolting of reuse ether is extracted 1-5 time, merges ether solution, evaporate to dryness, residue adds ethanol 0.5-5ml makes dissolving, as need testing solution; Other gets the ferulic acid reference substance, adds ethanol and makes the solution that every 1ml contains 0.5-3mg, in contrast product solution; Draw each 5-25 μ l of need testing solution and reference substance solution respectively, test according to the Chinese Pharmacopoeia thin layer chromatography, put respectively in same be on silica gel G 254 lamellaes of adhesive with the sodium carboxymethyl cellulose, with 60-90 ℃ of petroleum ether: ethyl acetate: glacial acetic acid=5-20: 1-10: 0.1-2 is developing solvent, launches, and takes out, dry, spray is with phosphomolybdic acid sulphuric acid test solution, and it is clear that hot blast blows to the speckle colour developing, inspects under the daylight; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(3) get this preparation 10-50ml, the 10-100ml jolting that adds diethyl ether is extracted, and divides the water intaking layer, add water saturated n-butyl alcohol jolting and extract 1-5 time, merge n-butyl alcohol liquid, wash with water 1-5 time, n-butyl alcohol liquid evaporate to dryness, add dissolve with methanol, by the neutral alumina post, with 20-80% methanol solution eluting, collect eluent, evaporate to dryness, residue add methanol 0.2-3ml makes dissolving, as need testing solution; Extracting liquorice control medicinal material 0.1-0.5g extracts 1-5 time with the n-butyl alcohol jolting, merges n-butyl alcohol liquid, washes with water 1-5 time, and n-butyl alcohol liquid evaporate to dryness adds methanol 0.5-3ml and makes dissolving, in contrast medical material solution; Other gets the astragaloside reference substance, adds methanol and makes the solution that every 1ml contains 0.5-5mg, in contrast product solution; Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 1-20 μ l of need testing solution, reference substance solution and control medicinal material solution respectively, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform: lower floor's solution of methanol or acetonitrile: water=5-20: 1-10: 0.5-5 is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃, inspects under the daylight; In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
(4) get this preparation 10-40ml, add ethyl acetate extraction 1-5 time, discard ethyl acetate layer, water layer merges n-butanol layer with water saturated n-butanol extraction 1-5 time, with the saturated washing of n-butyl alcohol 1-5 time, get n-butanol layer and volatilize, residue is with methanol 0.2-2ml dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 0.5-5mg, in contrast product solution; Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 5-20 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform: ethyl acetate: methanol or acetonitrile: formic acid=30-50: 1-10: 5-20: 0.1-1 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Check: relative density is got syrup 5-20g, add water 10-50ml dilution after, measure according to Chinese Pharmacopoeia relative density algoscopy, should be not less than 1.09;
Other should meet every regulation relevant under Chinese Pharmacopoeia syrup or the oral liquid item;
Assay: shine the Chinese Pharmacopoeia high effective liquid chromatography for measuring:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Methanol or second are fine: 0.05-0.2% phosphoric acid solution=10-90: 90-10 is a mobile phase; The detection wavelength is 324nm; Number of theoretical plate must not calculate with the ferulic acid peak and is lower than 5000;
The preparation of reference substance solution: it is an amount of to get the ferulic acid reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 5-20 μ g, in contrast product solution;
The preparation of need testing solution: precision is measured this preparation 1-10ml, puts in the 25ml measuring bottle, adds methanol to scale, shakes up, and with the microporous filter membrane filtration of 0.45 μ m, gets subsequent filtrate, promptly;
Algoscopy: accurate respectively reference substance solution and each 5-25 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
In this preparation, the every 1ml of syrup contains Radix Angelicae Sinensis in ferulic acid C10H10O4, must not be less than 0.020mg; The every 1ml of oral liquid contains Radix Angelicae Sinensis in ferulic acid C10H10O4, must not be less than 0.010mg.
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| CNB2006102005768A CN100559180C (en) | 2006-06-16 | 2006-06-16 | The detection method of aqueous donkey-hide gelatin and Chinese angelica preparation |
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| CNB2006102005768A CN100559180C (en) | 2006-06-16 | 2006-06-16 | The detection method of aqueous donkey-hide gelatin and Chinese angelica preparation |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101085060B (en) * | 2007-06-08 | 2010-09-29 | 于洪文 | Vein-relaxing capsule for treating desquamation of the hands |
| CN102288708A (en) * | 2011-08-09 | 2011-12-21 | 南京中山制药有限公司 | Method for detecting quality of capsules used for promoting blood circulation and stopping pain |
| CN102944641A (en) * | 2012-12-06 | 2013-02-27 | 杨清兰 | Method for detecting medicinal material of Ranunculaceae plant radix paeoniae alba |
| CN109157582A (en) * | 2018-11-28 | 2019-01-08 | 江西济民可信金水宝制药有限公司 | A kind of Aguiyanxue Syrup and preparation method thereof |
-
2006
- 2006-06-16 CN CNB2006102005768A patent/CN100559180C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101085060B (en) * | 2007-06-08 | 2010-09-29 | 于洪文 | Vein-relaxing capsule for treating desquamation of the hands |
| CN102288708A (en) * | 2011-08-09 | 2011-12-21 | 南京中山制药有限公司 | Method for detecting quality of capsules used for promoting blood circulation and stopping pain |
| CN102288708B (en) * | 2011-08-09 | 2013-05-01 | 南京中山制药有限公司 | Method for detecting quality of capsules used for promoting blood circulation and stopping pain |
| CN102944641A (en) * | 2012-12-06 | 2013-02-27 | 杨清兰 | Method for detecting medicinal material of Ranunculaceae plant radix paeoniae alba |
| CN109157582A (en) * | 2018-11-28 | 2019-01-08 | 江西济民可信金水宝制药有限公司 | A kind of Aguiyanxue Syrup and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN100559180C (en) | 2009-11-11 |
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