CN101461860B - Method for controlling quality of Chinese medicine liquid preparation - Google Patents
Method for controlling quality of Chinese medicine liquid preparation Download PDFInfo
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- CN101461860B CN101461860B CN2008102470114A CN200810247011A CN101461860B CN 101461860 B CN101461860 B CN 101461860B CN 2008102470114 A CN2008102470114 A CN 2008102470114A CN 200810247011 A CN200810247011 A CN 200810247011A CN 101461860 B CN101461860 B CN 101461860B
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Abstract
The invention provides a method for detecting traditional Chinese medicine liquid preparation containing phellodendron barks and teasel roots, which comprises: preparing a sample solution; preparing three reference solutions, including a reference medicinal material solution of the teasel roots, a reference substance solution of Chinese teasel root saponin VI and a reference substance solution ofberberine hydrochloride; adopting thin-layer chromatography, using an upper solution of n-butyl alcohol-acetic acid-water as a developing solvent, and detecting at an ultraviolet wavelength of between 300 and 400 nanometers to observe fluorescent spots displayed on a silica gel G thin-layer plate and the color of the spots; spraying a sulfuric ethanol solution on the silica gel G thin-layer plate, heating the silica gel G thin-layer plate, and observing spots displayed on the silica gel G thin-layer plate and the color of the spots; and using the observed conditions of the spots to identify whether the traditional Chinese medicine liquid preparation contains the phellodendron barks and the teasel roots or not. The method simultaneously identifies two medicinal materials on the same thin-layer plate, and not only simplifies the operation, reduces the experimental time and saves consumptive materials and reagent but also improves the efficiency.
Description
Technical field
The invention provides a kind of method of quality control, it is a kind of method that detects certain traditional Chinese medicine ingredients in the Chinese medicine preparation, refers in particular to adopt a kind of method to detect the method for quality control of two kinds of traditional Chinese medicine ingredients in the Chinese medicine preparation.
Background technology
Existing Chinese medicine preparation; Especially Chinese traditional compound medicine; When its method of quality control was differentiated in compound preparation certain traditional Chinese medicine ingredients more than two kinds, the method that generally adopts was to adopt thin-layer chromatography to inspect different traditional Chinese medicine ingredients respectively, and method repeats, loaded down with trivial details, time and effort consuming.With the Chinese patent drug that contains golden cypress and teasel root simultaneously is example, generally is to differentiate golden cypress and teasel root respectively, has increased operation steps, length consuming time, waste sample and reagent, and also cause too much organic solvent waste, increase and pollute.
Summary of the invention
The purpose of this invention is to provide a kind of detection method that contains the liquid preparation of Chinese medicine of golden cypress and teasel root, this method can detect golden cypress and teasel root simultaneously, has reached the purpose of 1 a plurality of composition of test detection.
The present invention provides a kind of detection method that contains the liquid preparation of Chinese medicine of golden cypress and teasel root, and this method comprises for differentiating the detection method of golden cypress and teasel root:
1. the preparation of need testing solution: sample thief 30-75ml, this sample are the liquid preparation of Chinese medicine that contains golden cypress and teasel root, evaporate to dryness; Residue is dissolved in water (0.4～3 volume that the consumption of water generally can be sample doubly), adds water saturated normal butyl alcohol jolting afterwards, and jolting gets final product for 1-5 time; Get normal butyl alcohol liquid,, use the saturated water washing of normal butyl alcohol again with the sodium hydroxide solution washing of 0.1-5%wt; Washing times is to get final product for 1-5 time, gets normal butyl alcohol liquid, evaporate to dryness; Residue adds methyl alcohol makes its dissolving, and solution is called for short A as need testing solution;
2. preparation reference substance solution is got the teasel root medicinal material, adds alcoholic solution, sonicated; Filter, the 10-20 water doubly that residue adds the teasel root quality of medicinal material makes dissolving, adds water saturated normal butyl alcohol jolting (jolting gets final product for 1-5 time) afterwards, gets normal butyl alcohol liquid; With the sodium hydroxide solution washing of 0.1-5%wt, use the saturated water washing of normal butyl alcohol (washing times is 1-5 time) again, get normal butyl alcohol liquid, evaporate to dryness; Residue adds methyl alcohol makes its dissolving, and solution is the control medicinal material solution of teasel root, is called for short B;
Get asperosaponin VI reference substance, add alcoholic solution and process the solution that contains asperosaponin VI 1mg/1ml reference substance solution, be called for short C as asperosaponin VI;
Get the Berberine hydrochloride reference substance, add alcoholic solution process the about 1mg/1ml of hydrochloric jamaicin solution, as the reference substance solution of Berberine hydrochloride, be called for short D;
The determining alcohol that more than adds in the alcoholic solution is advisable to reach the concentration of analyzing alcohol;
3. adopt thin-layered chromatography to detect; Draw above-mentioned A, B, C and four kinds of solution of D respectively with different suction pipe (capillary syring that thin-layered chromatography is special-purpose); The about 2-10 μ of absorption amount l; With the diverse location of its same level height on same silica gel g thin-layer plate, be designated as A, B, C, D position respectively, be 4 with volume ratio: the upper solution of normal butyl alcohol-acetic acid of 0.1-10: 1-10-water is a developping agent; Under ultraviolet wavelength 300-400nm, carry out ultraviolet detection, observe the fluorescence spot and the spot colors that show on the silica gel g thin-layer plate;
Step 3 is carried out ultraviolet detection under ultraviolet wavelength 300-400nm, above the D position, show a fluorescence spot on the silica gel g thin-layer plate, and it is the characteristic fluorescence spot of Berberine hydrochloride reference substance; On the silica gel g thin-layer plate top of A position and with the identical or approximately uniform position of fluorescence spot level height of Berberine hydrochloride reference substance; If demonstrate the fluorescence spot with the fluorescence spot same color of Berberine hydrochloride reference substance, then prove the effective constituent that contains golden cypress in the sample.Berberine hydrochloride is one of main effective constituent of golden cypress, also is the sign property effective constituent of golden cypress.
4. sulfuring up acid ethanolic solution on silica gel g thin-layer plate heats, and observes the spot and the spot colors that are shown on the silica gel g thin-layer plate.
Step 4 shows spot on the silica gel g thin-layer plate above B, C position after spray on the silica gel g thin-layer plate is with 10% ethanol solution of sulfuric acid and heating, it is the characteristic spot of teasel root control medicinal material and asperosaponin VI reference substance; On the silica gel g thin-layer plate top of A position and with the identical position of spot height of teasel root reference substance and asperosaponin VI reference substance; If the spot of the spot same color of demonstration and teasel root reference substance and asperosaponin VI reference substance then proves and contains teasel root in the sample.
In detection method of the present invention, especially prepare in the step (2) of step 1 and/or preparation reference substance solution of need testing solution, the consumption of described water saturated normal butyl alcohol (volume ml) be the 0.8-1.5 times of sample (ml); The consumption of the sodium hydroxide solution of described 0.1-5%wt (volume ml) is 1-2 a times of sample (ml); Preferred 45-100ml sodium hydroxide solution/50ml sample; More excellent sodium hydroxide solution washed twice with 0.1-5%wt is about 50ml sodium hydroxide solution/50ml sample at every turn; The mass concentration of this sodium hydroxide solution is 0.1-5%wt, is preferably 0.5-3%wt, more preferably 1%wt; The amount of the water that the normal butyl alcohol of described washing usefulness is saturated (volume ml) is 0.8-1.5 a times of sample (ml), preferred 45-100ml/50ml sample, more preferably from about 50ml/50ml sample; The said normal butyl alcohol liquid of getting, evaporate to dryness, residue add methyl alcohol makes its dissolving, and the amount of this methyl alcohol (volume ml) is 0.01-0.1 a times of sample (ml), preferably about 2ml methyl alcohol/50ml sample.
In detection method of the present invention, the described developping agent of step 3 is the upper solution of normal butyl alcohol-acetic acid-water of volume ratio 4: 0.5-5: 5-10.
In a preferred embodiment of the invention, the preferred sample thief of the preparation of test sample (liquid preparation of Chinese medicine that promptly contains golden cypress and teasel root) is concentrated into about 2/5～4/5 volume in water-bath, uses ether (approximately equivalent) jolting to extract again, and ether layer, water layer are subsequent use.Water layer wherein is used for preparing the need testing solution in the detection method of the present invention.
The above-mentioned detection method that contains the liquid preparation of Chinese medicine of golden cypress and teasel root, in the step (2) of preparation reference substance solution, the described alcohol that adds alcoholic solution sonicated teasel root can be methyl alcohol or ethanol, is preferably methyl alcohol; Adding alcohol dissolving asperosaponin VI reference substance and/or adding in the step of alcohol dissolving Berberine hydrochloride reference substance, described alcohol can be methyl alcohol or ethanol, is preferably ethanol.
The above-mentioned detection method that contains the liquid preparation of Chinese medicine of golden cypress and teasel root, in step 3, described developping agent is a volume ratio more preferably 4: the upper solution of normal butyl alcohol-acetic acid of 0.5-5: 5-10-water.
In detection method of the present invention; The preparation method of above-mentioned need testing solution can adopt approximately 50ml of sample (liquid preparation of Chinese medicine that promptly contains golden cypress and teasel root) earlier, extracts the water intaking layer with the ether jolting of 30-60ml; Evaporate to dryness; Residue is dissolved in water, and the consumption of the water of this dissolved residue is about 10-30ml, preferably about 15ml; Extract with water saturated normal butyl alcohol jolting again, the about 15-100ml of the consumption of this water saturated normal butyl alcohol, preferred 20-60ml, more preferably jolting is extracted 3 times, uses the about 20ml of amount of water saturated normal butyl alcohol at every turn; Merge normal butyl alcohol liquid; With the sodium hydroxide solution washing of 0.1-5%wt (mass concentration), the amount of this sodium hydroxide solution is about 30-150ml, preferred 45-100ml; More preferably use the sodium hydroxide solution washed twice of 0.1-5%wt, each sodium hydroxide solution consumption is approximately 50ml; This sodium hydroxide solution mass concentration is preferably 0.5-3%wt, more preferably 1%wt; That is to say, most preferably use 1% sodium hydroxide solution washed twice, the amount of each sodium hydroxide solution is about 50ml; Then, with the saturated water washing of normal butyl alcohol, the saturated water of normal butyl alcohol of washing usefulness is about 30-150ml, preferred 45-100ml, more preferably from about 50ml; Get normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol makes dissolving, and the amount of methyl alcohol is about 1-10ml, preferred 2ml, with the solution that obtains as need testing solution.
In detection method of the present invention, the preparation method of reference substance solution is divided into: one of which, get teasel root control medicinal material 1.0g; Add methanol solution (analyzing alcohol) sonicated; Filter, filtrating volatilizes, and residue adds water 15ml makes dissolving; Prepare the reference substance solution of control medicinal material teasel root with the preparation method of above-mentioned need testing solution, be called for short B.
Its two, other gets asperosaponin VI reference substance, add ethanolic solution (analyze alcohol) and process the solution that contains the about 1mg/1ml of asperosaponin VI, as the reference substance solution of asperosaponin VI, abbreviation C.
Its three, get the Berberine hydrochloride reference substance again, add ethanolic solution (analyze alcohol) process the about 1mg/1ml of hydrochloric jamaicin solution, as the reference substance solution of golden cypress effective constituent, abbreviation D.
In the detection method of the present invention, described thin-layered chromatography detection method is according to thin-layered chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia) test, draws each 5 μ l of above-mentioned four kinds of liquid; Putting respectively on same silica gel g thin-layer plate, is developping agent with the upper solution of normal butyl alcohol-acetic acid-water (the preferred volume ratio is about 4: 1: 5), the volume ratio of developping agent normal butyl alcohol-acetic acid-water preferred 4: 0.5-2: 3-7; More preferably volume ratio 4: 0.7-1.5: 4-6, launch, and take out; Dry, put under the uviol lamp and inspect, detect the preferred 350-380nm of wavelength; In a preferred embodiment of the invention, the wavelength of ultraviolet detection is about 365nm.
In the test sample owing to contain the effective constituent of golden cypress and teasel root, in the test sample chromatogram, with the corresponding position of Berberine hydrochloride reference substance on, the fluorescence spot of apparent same color; Spray the ethanol solution of sulfuric acid with 10% again, it is clear to be heated to spot colour developing at 150 ℃, in the test sample chromatogram, with teasel root control medicinal material, the corresponding position of asperosaponin VI reference substance on, show the spot of same color.
If contain the effective constituent of golden cypress and teasel root in the sample simultaneously, that is, the raw material of sample contains Chinese crude drug golden cypress and teasel root simultaneously, then satisfies simultaneously: on (1) silica gel g thin-layer plate with the fluorescence spot of the apparent same color in the corresponding position of Berberine hydrochloride reference substance; (2) spray is with ethanol solution of sulfuric acid on silica gel g thin-layer plate, and spot colour developing in heating back is clear, and with the corresponding position of the spot of B, C reference substance solution on, show the spot of same color.
The liquid preparation of Chinese medicine that contains golden cypress and teasel root is a lot, for example the strong waist wine of compound eucommia bark, guogong wine, strong bone medicinal liquor etc.Below only to contain the medicinal liquor of golden cypress and teasel root---the strong waist wine of compound eucommia bark is example, specifically describes technical scheme of the present invention.
The strong waist wine of compound eucommia bark be by the bark of eucommia, parasitic loranthus, teasel root, the root of bidentate achyranthes, Psoralea corylifolia, deer horn, turtle shell (vinegar system), Radix Angelicae Sinensis, corydalis tuber, the banksia rose, CORTEX PHELLODENDRI AMURENE etc. ten simply medicinal material boil the health care vina that wine forms.Supernatant liquid for dark brown red; Gas is fragrant, mildly bitter flavor, sweet.Function nourshing kidney tonifying liver restores menstrual flow and invigorates blood circulation.Be used for the pain in the back due to the kidney-yang deficiency, it is unfavorable to change one's position, soreness and weakness of waist and knees, the supplemental treatment of diseases such as lassitude.
When its method of quality control was differentiated in the strong waist wine of compound eucommia bark golden cypress, teasel root, existent method was to adopt thin-layer chromatography to inspect golden cypress and teasel root respectively, and method repeats, loaded down with trivial details, time and effort consuming.The present invention restudies the discrimination method that exploitation makes new advances; Still adopt thin-layer chromatography, the water saturated normal butyl alcohol of samples using extracts, and developping agent adopts normal butyl alcohol-acetic acid-water (the preferred volume ratio is about 4: 1: 5) to launch; Can inspect teasel root and golden cypress simultaneously, inspect respond well.Make two flavor medicinal materials on same thin layer plate, realize differentiating simultaneously, reached 1 test and detected a plurality of compositions, differentiate the purpose of 2 kinds of medicinal materials in this medicinal liquor simultaneously.Both simplified operation, and reduced experimental period, and the result is more clear, also saved consumptive material and reagent simultaneously, improved efficient.
Berberine hydrochloride reference substance (calibrating of Chinese biological goods provides lot number 110713-200208);
Teasel root control medicinal material (calibrating of Chinese biological goods provides lot number 121033-200507);
Asperosaponin VI reference substance (calibrating of Chinese biological goods provides lot number 111685-200401);
Golden cypress, the teasel root negative control is noiseless, and through three lot sample article experimental observations, the affirmation current methods is feasible.
Concrete grammar is:
(1) preparation need testing solution adopts approximately 50ml of sample (liquid preparation of Chinese medicine that promptly contains golden cypress and teasel root) earlier, and water-bath is concentrated into about 30ml, extracts with the ether jolting of about 30-ml again; Water intaking layer, water bath method, residue add the about 15ml dissolving of water, extract 3 times with water saturated normal butyl alcohol jolting; Each 20ml merges normal butyl alcohol liquid, with 1% sodium hydroxide solution washed twice; Each 50ml with the saturated water 50ml washing of normal butyl alcohol, gets normal butyl alcohol liquid again; Evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as need testing solution;
(2) the preparation reference substance solution is got teasel root control medicinal material 1.0g, adds methyl alcohol 20ml, and sonicated 30 minutes filters, and filtrating volatilizes, and residue adds water 15ml makes dissolving, prepares the control medicinal material solution of teasel root according to the described method of above-mentioned steps (1);
Get asperosaponin VI reference substance, add ethanol and process the solution that every 1ml contains 1mg, as the reference substance solution of asperosaponin VI;
Get the Berberine hydrochloride reference substance, add ethanol and process the solution that every 1ml contains 1mg, as the reference substance solution of Berberine hydrochloride;
(3) adopt thin-layered chromatography to detect; According to the thin-layered chromatography of 2005 editions one appendix VI B of Chinese Pharmacopoeia, draw each 5 μ l of reference substance solution of above-mentioned need testing solution and teasel root, asperosaponin VI, Berberine hydrochloride, put the diverse location of same level height on same silica gel g thin-layer plate; Upper solution with normal butyl alcohol-acetic acid of 4: 1: 5 of volume ratio-water is a developping agent; Launch, take out, dry; Put uviol lamp under 365nm, observe the fluorescence spot and the spot colors that are shown on the silica gel g thin-layer plate;
Above a position of Berberine hydrochloride reference substance solution, show the fluorescence spot of Berberine hydrochloride reference substance on the silica gel g thin-layer plate, inspect the position top of a sample and whether show the fluorescence spot with Berberine hydrochloride reference substance fluorescence spot same color in the position identical with the fluorescence spot height of Berberine hydrochloride reference substance; If have, then prove the effective constituent that contains golden cypress in the sample, or contain golden cypress in the raw material of proof sample;
(4) on the silica gel g thin-layer plate of step (3), spray 10% ethanol solution of sulfuric acid again, 150 ℃ are heated to the spot colour developing, observe the spot and the spot colors that are shown on this silica gel g thin-layer plate;
Above the position of the reference substance solution of the reference substance solution of a teasel root and asperosaponin VI, show the spot of teasel root reference substance and asperosaponin VI reference substance on the silica gel g thin-layer plate; The position top of some sample and inspecting the spot that whether shows with the spot same color of teasel root reference substance and asperosaponin VI reference substance with the identical position of spot height of teasel root reference substance and asperosaponin VI reference substance; If have, then can prove the effective constituent that contains teasel root in the sample, perhaps prove in the raw material of sample and contain teasel root.
The prior art that changed said method of the present invention detects the two kinds of detection methods of two kinds of different composition needs that contain simultaneously in a kind of sample and the judging standard of technological means; Make two flavor medicinal materials on same thin layer plate, realize differentiating simultaneously; Only reached that a test can detect a plurality of compositions, differentiated the purpose of two kinds of medicinal materials in this sample (for example medicinal liquor) simultaneously, both simplified operation; Reduced experimental period again; And the result is more clear, has also saved consumptive material and reagent simultaneously, has improved efficient.
Embodiment
Specify the present invention below in conjunction with embodiment, but do not limit practical range of the present invention.
The preparation reference substance solution:
1 gets teasel root control medicinal material 1.0g, adds methyl alcohol 20ml, and sonicated 30 minutes filters; Filtrating volatilizes, and residue adds water 15ml makes dissolving, extracts 3 times with water saturated normal butyl alcohol jolting, each 20ml; Merge normal butyl alcohol liquid, with 1% sodium hydroxide solution washed twice, each 50ml is again with the saturated water 50ml washing of normal butyl alcohol; Get normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as the need testing solution of teasel root control medicinal material.
2 get asperosaponin VI reference substance, add ethanol and process the solution that every 1ml contains 1mg, as the reference substance solution of asperosaponin VI.
3 get the Berberine hydrochloride reference substance, add ethanol and process the solution that every 1ml contains 1mg, as the reference substance solution of Berberine hydrochloride.
The reference substance solution of following examples is all from above-mentioned three kinds of reference substance solution that method prepares.
The detection method of golden cypress and teasel root in embodiment one, the strong waist wine of compound eucommia bark
The strong waist wine of compound eucommia bark be by the bark of eucommia, parasitic loranthus, teasel root, the root of bidentate achyranthes, Psoralea corylifolia, deer horn, turtle shell (vinegar system), Radix Angelicae Sinensis, corydalis tuber, the banksia rose, CORTEX PHELLODENDRI AMURENE etc. ten simply medicinal material boil the health care vina that wine forms.
Detection method is:
1. the preparation need testing solution adopts approximately 50ml of sample (being the strong waist wine of compound eucommia bark) earlier, and water-bath is concentrated into about 30ml, extracts the water intaking layer with the ether jolting of about 30ml; Water bath method, residue add water 15ml dissolving, extract 3 times with water saturated normal butyl alcohol jolting, each 20ml; Merge normal butyl alcohol liquid, with 1% sodium hydroxide solution washed twice, each 50ml is again with the saturated water 50ml washing of normal butyl alcohol; Get normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as need testing solution;
2. preparation reference substance solution: as above;
3. adopt thin-layered chromatography to detect:
3.1 according to the thin-layered chromatography of 2005 editions one appendix VI B of Chinese Pharmacopoeia, draw each 5 μ l of reference substance solution of above-mentioned need testing solution and teasel root, asperosaponin VI, Berberine hydrochloride, put the diverse location of same level height on same silica gel g thin-layer plate; Upper solution with normal butyl alcohol-acetic acid of 4: 1: 5 of volume ratio-water is a developping agent; Launch, take out, dry; Put uviol lamp under 365nm, observe the fluorescence spot and the spot colors that are shown on the silica gel g thin-layer plate;
3.2 above a position of Berberine hydrochloride reference substance solution, show the fluorescence spot of Berberine hydrochloride reference substance on the silica gel g thin-layer plate, the position top of some sample and inspecting the fluorescence spot that shows with the fluorescence spot same color of Berberine hydrochloride reference substance with the identical position of fluorescence spot height of Berberine hydrochloride reference substance; The effective constituent that contains golden cypress in the proof sample;
4. thin-layered chromatography detects:
4.1 on the silica gel g thin-layer plate of step 3, spray 10% ethanol solution of sulfuric acid again, 150 ℃ to be heated to spot colour developing clear, observes the spot and the spot colors that are shown on this silica gel g thin-layer plate;
4.2 above the position of the reference substance solution of the reference substance solution of a teasel root and asperosaponin VI, show the spot of teasel root reference substance and asperosaponin VI reference substance on the silica gel g thin-layer plate; The position top of some sample and inspecting the spot that shows with the spot same color of teasel root reference substance and asperosaponin VI reference substance with the identical position of spot height of teasel root reference substance and asperosaponin VI reference substance; The effective constituent that contains teasel root in the proof sample.
The detection method of golden cypress and teasel root in embodiment two, the guogong wine
1. the preparation need testing solution adopts approximately 50ml of sample (being guogong wine) earlier, and water-bath is concentrated into about 30ml, extracts with the ether jolting of about 30ml; Water intaking layer, water bath method, residue add water 12-18ml dissolving, extract with water saturated normal butyl alcohol 50-80ml jolting; Normal butyl alcohol liquid with the saturated water 40-80ml washing of normal butyl alcohol, is got normal butyl alcohol liquid again with the sodium hydroxide solution 50-100ml washing of 0.5-1.5%; Evaporate to dryness, residue add methyl alcohol 1-5ml makes dissolving, as need testing solution; This sample is a guogong wine;
2. preparation reference substance solution: as above;
3. adopt thin-layered chromatography to detect:
3.1 according to the thin-layered chromatography of 2005 editions one appendix VI B of Chinese Pharmacopoeia, draw each 5 μ l of reference substance solution of above-mentioned need testing solution and teasel root, asperosaponin VI, Berberine hydrochloride, put the diverse location of same level height on same silica gel g thin-layer plate; With volume ratio 3-5: 1: the upper solution of normal butyl alcohol-acetic acid of 4-6-water is a developping agent; Launch, take out, dry; Put uviol lamp under 350-380nm, observe the fluorescence spot and the spot colors that are shown on the silica gel g thin-layer plate;
3.2 above a position of Berberine hydrochloride reference substance solution, show the fluorescence spot of Berberine hydrochloride reference substance on the silica gel g thin-layer plate, the position top of some sample and inspecting the fluorescence spot that shows with the fluorescence spot same color of Berberine hydrochloride reference substance with the identical position of fluorescence spot height of Berberine hydrochloride reference substance; The effective constituent that contains golden cypress in the proof sample (guogong wine);
4. thin-layered chromatography detects:
4.1 on the silica gel g thin-layer plate of step 3, spray the ethanol solution of sulfuric acid of 5-15% again, 100 ℃-200 ℃ to be heated to spot colour developing clear, observes the spot and the spot colors that are shown on this silica gel g thin-layer plate;
4.2 above the position of the reference substance solution of the reference substance solution of a teasel root and asperosaponin VI, show the spot of teasel root reference substance and asperosaponin VI reference substance on the silica gel g thin-layer plate; The position top of some sample and the spot with the spot same color of teasel root reference substance and asperosaponin VI reference substance is arranged in the identical position display of spot height with teasel root reference substance and asperosaponin VI reference substance; The effective constituent that contains teasel root in the proof sample (guogong wine).
The detection method of embodiment three, Comparative Examples
Comparative Examples is to have deleted the strong waist wine of compound eucommia bark of golden cypress and teasel root, its by the bark of eucommia, parasitic loranthus, the root of bidentate achyranthes, Psoralea corylifolia, deer horn, turtle shell (vinegar system), Radix Angelicae Sinensis, corydalis tuber, the banksia rose nine flavor medicinal materials according to ten simply the contrast that forms of the said components content boiling of the strong waist wine of compound eucommia bark formed of Chinese medicine use medicinal liquor.
Detection method is:
1. the preparation need testing solution adopts approximately 50ml of sample (i.e. medicinal liquor is used in contrast) earlier, and water-bath is concentrated into about 30ml, extracts the water intaking layer with the ether jolting of about 30ml; Water bath method, residue add water 15ml dissolving, extract 3 times with water saturated normal butyl alcohol jolting, each 20ml; Merge normal butyl alcohol liquid, with 1% sodium hydroxide solution washed twice, each 50ml is again with the saturated water 50ml washing of normal butyl alcohol; Get normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as need testing solution; This sample is used medicinal liquor for contrast;
2. preparation reference substance solution: as above;
3. adopt thin-layered chromatography to detect:
3.1 according to the thin-layered chromatography of 2005 editions one appendix VI B of Chinese Pharmacopoeia, draw each 5 μ l of reference substance solution of above-mentioned need testing solution and teasel root, asperosaponin VI, Berberine hydrochloride, put the diverse location of same level height on same silica gel g thin-layer plate; Upper solution with normal butyl alcohol-acetic acid of 4: 1: 5 of volume ratio-water is a developping agent; Launch, take out, dry; Put uviol lamp under 365nm, observe the fluorescence spot and the spot colors that are shown on the silica gel g thin-layer plate;
3.2 above a position of Berberine hydrochloride reference substance solution, show the fluorescence spot of Berberine hydrochloride reference substance on the silica gel g thin-layer plate, the position top of some sample and not have to show and the fluorescence spot of the fluorescence spot same color of Berberine hydrochloride reference substance inspecting with the identical position of fluorescence spot height of Berberine hydrochloride reference substance; The effective constituent that does not contain golden cypress in the proof sample (medicinal liquor is used in contrast);
4. thin-layered chromatography detects:
4.1 on the silica gel g thin-layer plate of step 3, spray 10% ethanol solution of sulfuric acid again, 150 ℃ to be heated to spot colour developing clear, observes the spot and the spot colors that are shown on this silica gel g thin-layer plate;
4.2 above the position of the reference substance solution of the reference substance solution of a teasel root and asperosaponin VI, show the spot of teasel root reference substance and asperosaponin VI reference substance on the silica gel g thin-layer plate; The position top of some sample and inspecting the spot of the spot same color that not have demonstration and teasel root reference substance and asperosaponin VI reference substance with the identical position of spot height of teasel root reference substance and asperosaponin VI reference substance; The effective constituent that does not contain teasel root in the proof sample (medicinal liquor is used in contrast).
The actual composition of above-mentioned test result and Comparative Examples coincide, and shows that method of the present invention is definitely feasible.
Claims (2)
1. detection method that contains the liquid preparation of Chinese medicine of golden cypress and teasel root; This detection method is the discrimination method of golden cypress and teasel root in the liquid preparation of Chinese medicine; This liquid preparation of Chinese medicine is the strong waist wine of compound eucommia bark; The strong waist wine of this compound eucommia bark be by the bark of eucommia, parasitic loranthus, teasel root, the root of bidentate achyranthes, Psoralea corylifolia, deer horn, vinegar Carapax Trionycis (processed), Radix Angelicae Sinensis, corydalis tuber, the banksia rose, CORTEX PHELLODENDRI AMURENE ten simply medicinal material boil the vina that wine forms, this method comprises:
(1) preparation need testing solution, sample thief 50ml, this sample are the liquid preparation of Chinese medicine that contains golden cypress and teasel root, extract with the ether jolting of 30-60ml; Water intaking layer, evaporate to dryness, residue add that 10-30ml is water-soluble to be separated, and add the water saturated normal butyl alcohol jolting of 15-100ml afterwards; Get normal butyl alcohol liquid,, use the saturated water washing of 30-150ml normal butyl alcohol again, get normal butyl alcohol liquid with the sodium hydroxide solution washing of 30-150ml 0.1-5%wt; Evaporate to dryness, residue add 1-10ml methyl alcohol makes its dissolving, and solution is need testing solution;
(2) preparation reference substance solution, one of which is got teasel root control medicinal material 1.0g, adds the methanol solution sonicated, filters, and filtrating volatilizes, and residue adds water 15ml makes dissolving, prepares the reference substance solution of control medicinal material teasel root with the preparation method of above-mentioned need testing solution;
Its two, other gets asperosaponin VI reference substance, adds ethanolic solution and processes the solution that contains asperosaponin VI 1mg/1ml, as the reference substance solution of asperosaponin VI;
Its three, get the Berberine hydrochloride reference substance again, add the solution that ethanolic solution is processed hydrochloric jamaicin 1mg/1ml, as the reference substance solution of golden cypress effective constituent;
(3) adopt thin-layered chromatography to detect,, draw each 5 μ l of above-mentioned four kinds of liquid according to the thin-layered chromatography test of 2005 editions one appendix VI B of Chinese Pharmacopoeia; Putting respectively on same silica gel g thin-layer plate, is developping agent with the upper solution of normal butyl alcohol-acetic acid of 4: 1: 5 of volume ratio-water, launches; Take out; Dry, put under the uviol lamp and inspect, detect wavelength 350-380nm;
(4) in the test sample owing to contain the effective constituent of golden cypress and teasel root, in the test sample chromatogram, with the corresponding position of Berberine hydrochloride reference substance on, the fluorescence spot of apparent same color; Spray the ethanol solution of sulfuric acid with 10% again, it is clear to be heated to spot colour developing at 150 ℃, in the test sample chromatogram, with teasel root control medicinal material, the corresponding position of asperosaponin VI reference substance on, show the spot of same color.
2. the detection method that contains the liquid preparation of Chinese medicine of golden cypress and teasel root as claimed in claim 1, this detection method comprises:
(1) preparation need testing solution, sample thief 50ml, water-bath is concentrated into 30ml, extracts the water intaking layer again with the ether jolting of 30ml; Water bath method, residue add water 15ml dissolving, extract 3 times with water saturated normal butyl alcohol jolting, each 20ml; Merge normal butyl alcohol liquid, with 1% sodium hydroxide solution washed twice, each 50ml is again with the saturated water 50ml washing of normal butyl alcohol; Get normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as need testing solution;
(2) the preparation reference substance solution is got teasel root control medicinal material 1.0g, adds methyl alcohol 20ml, and sonicated 30 minutes filters, and filtrating volatilizes, and residue adds water 15ml makes dissolving, prepares the control medicinal material solution of teasel root according to the described method of above-mentioned steps (1);
Get asperosaponin VI reference substance, add ethanol and process the solution that every 1ml contains 1mg, as the reference substance solution of asperosaponin VI;
Get the Berberine hydrochloride reference substance, add ethanol and process the solution that every 1ml contains 1mg, as the reference substance solution of Berberine hydrochloride;
(3) adopt thin-layered chromatography to detect; According to the thin-layered chromatography of 2005 editions one appendix VI B of Chinese Pharmacopoeia, draw each 5 μ l of reference substance solution of above-mentioned need testing solution and teasel root, asperosaponin VI, Berberine hydrochloride, put the diverse location of same level height on same silica gel g thin-layer plate; Upper solution with normal butyl alcohol-acetic acid of 4: 1: 5 of volume ratio-water is a developping agent; Launch, take out, dry; Put uviol lamp under 365nm, observe the fluorescence spot and the spot colors that are shown on the silica gel g thin-layer plate;
Above the position of Berberine hydrochloride reference substance solution, show the fluorescence spot of Berberine hydrochloride reference substance on the silica gel g thin-layer plate, top, the position of sample and inspecting the fluorescence spot that whether shows with the fluorescence spot same color of Berberine hydrochloride reference substance with the identical position of fluorescence spot height of Berberine hydrochloride reference substance;
(4) on the silica gel g thin-layer plate of step (3), spray 10% ethanol solution of sulfuric acid again, 150 ℃ are heated to the spot colour developing, observe the spot and the spot colors that are shown on this silica gel g thin-layer plate;
Above the position of the reference substance solution of the reference substance solution of teasel root and asperosaponin VI, show the spot of teasel root reference substance and asperosaponin VI reference substance on the silica gel g thin-layer plate; Top, the position of sample and inspecting the spot that whether shows with the spot same color of teasel root reference substance and asperosaponin VI reference substance with the identical position of spot height of teasel root reference substance and asperosaponin VI reference substance.
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| 费美玲等.薄层色谱法定性鉴别泌尿宁颗粒中的3味中药.《河北大学学报（自然科学版）》.2007,第27卷(第5期),第497-498，504页. * |
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