CN109085284A - A kind of quick thin-layer identification method of multiple medicine taste of Ershiwuwei zhenzhu wan - Google Patents
A kind of quick thin-layer identification method of multiple medicine taste of Ershiwuwei zhenzhu wan Download PDFInfo
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Abstract
The present invention relates to a kind of quick thin-layer identification methods of multiple medicine taste of Ershiwuwei zhenzhu wan.It is characterized by: obtain test sample and control medicinal material solution with simple, fast pre-treating method, using same test solution, on seven blocks of lamellaes, authenticated 12 taste medicinal materials, it is different inspect under the conditions of, inspect different traditional Chinese medicine ingredients；Each clear spot, intersects, but the ingredient of different levels, and does not interfere with each other.Rate of revising and enlarging will be identified in the compound preparation of 25-component Chinese medicinal composition by average 12%, is increased to 48%.Completing these identifications only needs sample 3g, Extraction solvent and solvent 126ml, time 4 hours.Method is easy, quick, efficient, and rate height is revised and enlarged in identification, and report method does not have at present.Wherein double medicinal materials of 10 taste medicinal materials identify simultaneously to report for the first time.It feeds intake for the supervision of Ershiwuwei zhenzhu wan, provides quick thin-layer identification method.
Description
Technical field
The present invention relates to a kind of quick thin-layer identification methods of multiple medicine taste of Ershiwuwei zhenzhu wan.The quick thin layer mirror of multiple medicine taste
Other method refers to that using thin-layer identification method, the cultured ox gallstone, muscone, will in prescription reach Sa increasing, Cuminum celery, cloves, wood
Perfume, agalloch eaglewood, Long Pepper, Fructus Malvae Vertillatae, dalbergia wood, safflower and west safflower, 12 taste Chinese medicines have carried out thin layer identification.Completing these identifications only needs
Sample 3g, Extraction solvent and solvent 126ml, time 4 hours.Method is easy, quick, efficient, and it is current that rate height is revised and enlarged in identification
Report method does not have.
Background technique
In compound Chinese medicinal preparation, the especially compound preparation of the above prescription of 25-component, since flavour of a drug are more, each flavour of a drug
Dosage is low, and numerous micro effective component interferes with each other, and thin layer resolution is low, and quantitative determination index was few, with version China in 2015
For pharmacopeia one, the compound preparation more than 25-component recorded shares 32 kinds, and it is highest that rate is recorded in thin layer identification
Be the net brain piece of cow-bezoar be 28%, minimum is that YANGHE JIENING GAO is zero, average out to 11%.That is in 20 eight traditional chinese medicines
In the preparation of prescription, only 3 taste medicinal materials can identify it whether there is or not feeding intake, and numerous medicinal materials is to be unable to control its situation that feeds intake
, inspecting for quality standard is horizontal too low, can not provide strong support to quality surveillance.
Even if revising and enlarging in the highest kind of rate in thin layer identification, it is a kind that thin layer, which identifies also mostly, is identified if any N,
N kind test solution will be prepared, n times are unfolded in N block lamellae, identify traditional differential mode of N taste medicinal material.For exclusive PCR,
The pre-treatment program of sample is how complicated, loaded down with trivial details, need to use a large amount of organic reagent purification process repeatedly, it is laborious, time-consuming, take reagent,
Environment is polluted, harm is healthy, and detection cycle is long.In this way, a quality mark identified containing 6~7 thin layers with binomial assay
Quasi- detection is completed, and the time of Fei Yizhou is commonly taken up, and such as retrial, the time is double, and detection speed seriously restricts the Chinese medicine modern times
Change speed of production.So finding simple, fast detection method, improving detection efficiency, reduce testing cost and traditional Chinese medicine quality
Control the difficulty that must be broken through.By taking the net brain piece of the highest cow-bezoar of rate is recorded in Chinese Pharmacopoeia one thin layer identification of version in 2015 as an example
Dissect: the kind has been recorded 7 thin layers and has been identified by 28 taste Chinese medicinal compositions under normal term.The specific method is as follows:
[identification] (1) takes this product 2, and coating tablet removes coating, and finely ground, add diethyl ether 10ml, is ultrasonically treated 10 minutes, filters, filter
Liquid is evaporated, and residue adds methanol 1ml to make to dissolve, as test solution.Borneol reference substance separately is taken, adds methanol that every 1ml is made containing 1mg
Solution, as reference substance solution.It is tested according to thin-layered chromatography (general rule 502), draws each 10 μ l of above two solution, respectively point
In on same silica gel g thin-layer plate, with toluene-ethyl acetate (10: 1) for solvent, it is unfolded, takes out, dry, spray with 5% vanillic aldehyde
It is clear to be heated to spot development at 105 DEG C for sulfuric acid solution.In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, show
Same color spot.
(2) this product 10 are taken, coating tablet removes coating, and it is finely ground, add methanol 20ml, is ultrasonically treated 30 minutes, filtration, filtrate
It is evaporated, residue adds water 10ml to make to dissolve, and adds hydrochloric acid 0.5ml, sets heating hydrolysis 30 minutes in water-bath, cools down, shaken immediately with ether
Extraction 2 times, each 10ml is shaken, merges ether solution, is evaporated, residue adds methanol 1ml to make to dissolve, as test solution.It separately takes big
Yellow control medicinal material 0.5g, is made in the same way of control medicinal material solution.Rheum emodin, Chrysophanol reference substance are taken again, add methanol that every 1ml is made each
Solution containing 1mg, as reference substance solution.It is tested according to thin-layered chromatography (general rule 502), draws above-mentioned each 5 μ l of three kinds of solution, point
In on same silica gel g thin-layer plate, the upper solution with petroleum ether (60~90 DEG C)-acetic ether-methanoic acid (15: 5: 1) is other point
Solvent is unfolded, and takes out, dries, set and inspect under ultraviolet lamp 365nm.In sample chromatogram, corresponding to reference medicine chromatography
Position on, show identical orange-yellow fluorescence spot；It sets after being smoked in ammonia steam, spot becomes red.
(3) this product 5 are taken, coating tablet removes coating, and it is finely ground, add methanol 10ml, is ultrasonically treated 30 minutes, filtration, filtrate
It is concentrated into about 1ml, is added on neutral alumina column (100~200 mesh, 2g, internal diameter 1cm), is eluted with methanol 20ml, collection is washed
De- liquid, is evaporated, residue adds methanol 1ml to make to dissolve, as test solution.Coptis control medicinal material 50mg separately is taken, is made in the same way of pair
According to medicinal material solution.Berberine hydrochloride reference substance is taken again, adds methanol that solution of every 1ml containing 0.05mg is made, as reference substance solution.
It is tested according to thin-layered chromatography (general rule 502), draws above-mentioned each 5 μ l of three kinds of solution, put respectively on same silica gel g thin-layer plate, with
Toluene-ethyl acetate-isopropanol-methanol-water (12: 6: 3: 3: 0.6) is solvent, in the expansion cylinder for setting ammonia saturated with vapor, exhibition
It opens, takes out, dry, set and inspected under ultraviolet lamp 365nm.In sample chromatogram, on position corresponding with reference medicine chromatography,
The fluorescence principal spot of aobvious same color；At the position corresponding to the chromatogram of the reference substance, the fluorescence spot of same color is shown.
(4) this product 15 are taken, coating tablet removes coating, and it is finely ground, add methanol 30ml, is ultrasonically treated 30 minutes, filtration, filtrate
It is evaporated, residue adds water 20ml to make to dissolve, and adds dilute hydrochloric acid to adjust pH value about to 2, is extracted 2 times with ether shaking, each 20ml is discarded
Ether solution, then extracted 2 times, each 20ml with chloroform, merge chloroform liquid (aqueous solution is spare), is evaporated, residue adds first
Alcohol 1ml makes to dissolve, as test solution.Forsythin reference substance is taken, adds methanol that solution of every 1ml containing 1mg is made, as control
Product solution.It is tested according to thin-layered chromatography (general rule 502), draws each 10 μ l of above two solution, put respectively in same silica G thin layer
On plate, with chloroform-methanol-glacial acetic acid (14: 2: 0.2) for solvent, it is unfolded, takes out, dry, spray with 10% sulfuric acid ethyl alcohol
It is clear to be heated to spot development at 105 DEG C for solution.In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, show identical
The spot of color.
(5) the spare aqueous solution under [identification] (4) item is taken, is extracted 2 times, each 20ml with ethyl acetate shaking, merges second
Acetoacetic ester liquid (aqueous solution is spare), is evaporated, and residue adds 1 ml of ethyl acetate to make to dissolve, as test solution.Separately take chlorogenic acid
Reference substance adds methanol that solution of every 1ml containing 1mg is made, as reference substance solution.It tests, inhales according to thin-layered chromatography (general rule 502)
Each 2 μ l of above two solution is taken, is put respectively on same polyamide film, is with acetate-methanol-formic acid (10: 1: 1.5)
Solvent is unfolded, and takes out, dries, set and inspect under ultraviolet lamp 365nm.In sample chromatogram, corresponding with reference substance chromatography
On position, the fluorescence spot of same color is shown.
(6) the spare aqueous solution under [identification] (5) item is taken, is adjusted to neutrality with ammonia solution, extracts 2 with ethyl acetate shaking
Secondary, each 20ml discards acetic acid ethyl fluid, then is saturated with water n-butanol shaking and extracts 2 times, each 20ml, merges n-butanol liquid,
It is evaporated, residue adds 1 ml of methanol to make to dissolve, as test solution.Separately take Puerarin reference substance, Gardenoside reference substance, respectively plus
Solution of every 1ml containing 1mg is made in methanol, as reference substance solution.It is tested according to thin-layered chromatography (general rule 502), draws above-mentioned three
Kind each 5 μ l of solution puts respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (14: 5: 0.5) for solvent, opens up
It opens, takes out, dry, set and inspected under ultraviolet lamp 365nm.In sample chromatogram, in position corresponding with Puerarin reference substance chromatography
It sets, shows the fluorescence spot of same color；It is clear to be heated to spot development at 105 DEG C with 5% vanillin-sulfuric acid solution for spray.For examination
In product chromatography, on position corresponding with Gardenoside reference substance chromatography, the spot of same color is shown.
6 thin layers in above-mentioned example identify, and authenticated 7 taste Chinese medicines, and only time for sample pretreatment is it is necessary to spending 12
Hour, 32, sample, organic extraction solvent 404ml, in addition 90 ml of solvent and duration of run 4 hours, the thin layer of 1 batch of sample
Identify it is necessary to spend whole 2 days time and 494 ml organic solvents.It is all to use that its premise, which will also have the identification of gomi herbs,
Reference substance compares, and such as according to control medicinal material, the solvent of sample processing time and cost can be more, and reference substance compares,
Information content is single, is unfavorable for quality surveillance.
Such as retrial, detection time and organic reagent will be double, and detection speed can not be with mechanization mass production phase
Match.The method of quality control of compound Chinese medicinal preparation as dissecting example can be found everywhere, or even also more cumbersome, more multiple than example
Miscellaneous, the solvent of cost and time are more.So improving detection efficiency, reducing testing cost, reduce environmental pollution, at detection people
The very urgent objective of the struggle of member, we are exactly to record 25-component for one pharmacopeia of version in 2015 under the background condition
Pearl Pill, thin layer identification only authenticated 2 taste Chinese medicines, and quantitative detection only determines crocin I status, is unable to control said preparation
The situation that feeds intake, so special topic revise and enlarge raising research to the identification of its thin layer.
Its composition and preparation method be shown under Chinese Pharmacopoeia version one Ershiwuwei zhenzhu wan item recorded in 2015, no
It repeats again.
Summary of the invention
Each control medicinal material supernatant using same test solution and methanol ultrasound is established, on seven blocks of lamellaes,
Authenticated 12 taste medicinal materials, it is different inspect under the conditions of, inspect different traditional Chinese medicine ingredients；Each clear spot, intersects, but different
The ingredient of level, and do not interfere with each other.Rate of revising and enlarging will be identified in the compound preparation of 25-component Chinese medicinal composition by average 11%, improved
To 48%.Completing these identifications only needs sample 3g, Extraction solvent and solvent 126ml, time 4 hours.Method is easy, quick, high
Rate height is revised and enlarged in effect, identification, and report method does not have at present.Not only had and broken through conventional novelty, but also had and improve
Detection efficiency saves testing cost, the practicability to reduce environmental pollution.
The present invention solves scheme used by its technical problem are as follows:
(1) this product 3g is taken, it is finely ground, add methanol 5ml, be ultrasonically treated 20 minutes, filtration, filtrate is as test solution；Separately take training
Induced bezoar and each 0.05g of muscone's control medicinal material, respectively plus 2 ml of methanol, ultrasonic treatment 20 minutes, supernatant are used as control
Medicinal material solution；Control medicinal material solution and each 5~6 μ l of test solution are drawn, is put respectively in same silica G F254On lamellae, with
Cyclohexane-ethyl acetate-glacial acetic acid-methanol-water of volume ratio 8.5: 8.5: 1: 1: 0.5 is solvent, is unfolded, and is taken out, hot wind
Drying is sprayed with 10% ethanol solution of sulfuric acid, and 105 DEG C to be heated to spot development clear, is set and is inspected under ultraviolet lamp 365nm, test sample
In chromatography, on position corresponding with cultured ox gallstone reference medicine chromatography, show 2 identical blue-fluorescence principal spots, with musk deer
On the fragrant corresponding position of reference medicine chromatography, an identical faint yellow fluorescence principal spot is shown, is verified through blank, blank sample
(sample without cultured ox gallstone or muscone) is noiseless, identifies exclusive；
(2) it takes will to increase control medicinal material and each 0.1g of Cuminum celery control medicinal material up to Sa, respectively plus 2 ml of methanol, is ultrasonically treated 20 points
Clock, supernatant is as control medicinal material solution；It draws control medicinal material solution and identifies each 6~8 μ l of test solution under (1) item, point
On not same silica gel g thin-layer plate, using cyclohexane-ethyl acetate-acetone of volume ratio 7: 2: 1 as solvent, it is unfolded, takes out, heat
Wind is dry, sets and inspects under ultraviolet lamp 365nm, in sample chromatogram, is increasing the corresponding position of reference medicine chromatography up to Sa with will
On, 3 identical red fluorescence principal spots are at least shown, on position corresponding with Cuminum celery reference medicine chromatography, aobvious 2 are identical
Bright blue fluorescence principal spot；It is verified through blank, blank sample (sample that Sa increasing or Cuminum celery are reached without will) is noiseless, identifies
It is exclusive；
(3) cloves 0.1g, 0.2 g of radix aucklandiae control medicinal material are taken, respectively plus 2 ml of methanol, is ultrasonically treated 20 minutes, as comparison medicine
Material solution；It draws control medicinal material solution and identifies each 6~8 μ l of test solution under (1) item, put respectively in same silica G thin layer
On plate, using hexamethylene-ethyl acetate-formic acid of volume ratio 8: 2: 0.2 as solvent, it is unfolded, takes out, hot blast drying, spray with 10%
Ethanol solution of sulfuric acid, 105 DEG C to be heated to spot development clear, sets and inspects under ultraviolet lamp 365nm, in sample chromatogram, with
On the corresponding position of cloves reference medicine chromatography, an identical orange-yellow fluorescence spot is shown；It is inspected under daylight, sample chromatogram
In, on position corresponding with cloves and radix aucklandiae reference medicine chromatography, same color principal spot is shown respectively；It is verified through blank, it is empty
White sample (sample without cloves or radix aucklandiae) is noiseless, identifies exclusive；
(4) agalloch eaglewood control medicinal material and each 0.1g of Long Pepper control medicinal material are taken, respectively plus 2 ml of methanol, is ultrasonically treated 20 minutes, as
Control medicinal material solution；It draws control medicinal material solution and identifies each 6~8 μ l of test solution under (1) item, put respectively in same silica gel
GF254On lamellae, using cyclohexane-ethyl acetate-acetone of volume ratio 7: 2: 1 as solvent, it is unfolded, takes out, hot blast drying,
It sets and is inspected under ultraviolet lamp 254nm, in sample chromatogram, on position corresponding with agalloch eaglewood and Long Pepper reference medicine chromatography, point
It Xian not same color principal spot；Spray is with 10% ethanol solution of sulfuric acid, and 105 DEG C to be heated to spot development clear, sets ultraviolet lamp
It is inspected under 365nm, in sample chromatogram, on position corresponding with agalloch eaglewood reference medicine chromatography, shows two identical sapphirines
Fluorescence principal spot shows two identical glassy yellow fluorescence principal spots, through sky on position corresponding with Long Pepper reference medicine chromatography
White verifying, blank sample (sample without agalloch eaglewood or Long Pepper) is noiseless, identifies exclusive；
(5) it takes caffeic acid reference substance appropriate, adds methanol that solution of every 1ml containing 1mg is made, as reference substance solution；Draw control
5 μ l of product solution, identify 6~8 μ l of test solution under (1) item, put respectively in same silica G F254On lamellae, with volume ratio 6:
4: 0.5 cyclohexane-ethyl acetate-formic acid is solvent, is unfolded, and is taken out, and hot blast drying is set and inspected under ultraviolet lamp 254nm,
In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, same color principal spot is shown；It sprays with 10% ethanol solution of sulfuric acid,
105 DEG C to be heated to spot development clear, inspects under daylight, in sample chromatogram, at the position corresponding to the chromatogram of the reference substance, shows
Same color spot, is verified through blank, and blank sample (sample without Fructus Malvae Vertillatae) is noiseless, is identified exclusive；
(6) 0.2 g of dalbergia wood control medicinal material is taken, 2 ml of methanol is added, is ultrasonically treated 20 minutes, supernatant is as control medicinal material solution；
It draws control medicinal material solution and identifies each 6~8 μ l of test solution under (1) item, put respectively on same silica gel g thin-layer plate, with
2: 1.5 cyclohexane-ethyl acetate of volume ratio is solvent, is unfolded, and takes out, dries, set and inspect under ultraviolet lamp 365nm, for examination
In product chromatography, on position corresponding with reference medicine chromatography, same color fluorescence principal spot is shown；It is sprayed again with 10% sulfuric acid ethyl alcohol
Solution, 105 DEG C to be heated to spot development clear, then sets and inspect under ultraviolet lamp 365nm, in sample chromatogram, with comparison medicine
Wood color is composed on corresponding position, and the fluorescence principal spot of at least aobvious 3 same colors is verified, blank sample (is free of dalbergia wood through blank
Sample) it is noiseless, identify it is exclusive；
(7) 0.2 g of safflower control medicinal material, 0.04 g of west safflower control medicinal material are taken, respectively plus 2 ml of methanol, is ultrasonically treated 20 points
Clock, supernatant is as control medicinal material solution；It draws control medicinal material solution and identifies each 6~8 μ l of test solution under (1) item, point
Other point is on same silica gel g thin-layer plate, using acetic ether-methanoic acid-water-methanol of volume ratio 10:2:2.1:0.5 as solvent,
Expansion takes out, dries, set and inspect under daylight, in sample chromatogram, on position corresponding with west safflower reference medicine chromatography,
Show 3 identical yellow principal spots；Set and inspected under ultraviolet lamp 365nm, in sample chromatogram, with safflower reference medicine chromatography
On corresponding position, 1 identical fluorescence principal spot is shown, is verified through blank, the blank sample (sample without safflower or west safflower
Product) it is noiseless, identify exclusive.
The principle of the present invention is as follows:
It is different according to the chemical structure of each effective component of Chinese medicine and polarity, with the movement of solvent, absorption on lamellae,
The ability of desorption and it is different, so that the spot of each effective component is separated.Again by each compositional polarity size, polarity is chosen
Different under the conditions of inspecting, respectively different spot colors are presented in approximate effective component, overlapped, but are not done mutually
It disturbs, detects several medicinal materials, same test solution, for multinomial identification application simultaneously on same lamellae.
It innovative point of the invention and has the beneficial effect that:
(1) breaching a herbal species has N to identify it is necessary to prepare N kind test solution, and n times, mirror is unfolded in N block lamellae
Traditional identification method of other N taste medicinal material.Each control medicinal material supernatant using same test solution and methanol ultrasound is established,
On seven blocks of lamellaes, authenticated 12 taste medicinal materials, it is different inspect under the conditions of, inspect different traditional Chinese medicine ingredients；Each clear spot,
It intersects, but the ingredient of different levels, and does not interfere with each other.Rate is revised and enlarged by identifying in the compound preparation of 25-component Chinese medicinal composition
By average 11%, it is increased to 48%.Completing these identifications only needs sample 3g, Extraction solvent and solvent 126ml, time 4 hours.Side
Method is easy, quick, efficient, and rate height is revised and enlarged in identification, and report method does not have at present.Both have and break through conventional innovation
Property, and have and improve detection efficiency, save testing cost, the practicability to reduce environmental pollution.
(2) on same lamellae, while cultured ox gallstone and muscone being detected；Will increases up to Sa and Cuminum celery；Cloves
And radix aucklandiae；Agalloch eaglewood and Long Pepper；Discrimination method while safflower and 2 medicinal material of plate for west safflower yet there are no identical report, tool innovation
Property and practicability.
(3) after dalbergia wood thin-layer developing, the fluorescence spot that presentation is inspected under ultraviolet lamp 365nm, then 10% sulfuric acid by spraying are first set
Ethanol solution colour developing after, inspect increase fluorescence spot, although being all fluorescence spot, colour developing front and back, not only the intensity of fluorescence and
Color is different, is formed there are also new fluorescence spot, and the information content of detection increases, and facilitates quality surveillance, is prime report.
(4) medicine of the invention compared with the thin-layer identification method of the Chinese materia medica preparation of the current above prescription of 25 taste, not only detected
Taste is significantly promoted, and also improves 5 times of detection efficiency or more, saves detection time 70%, reduces testing cost 80%, and it is dirty to reduce environment
Dye 90% forms a set of easy, quick, efficient, low consumption, low pollution, multiple medicine taste, the quick thin-layer identification method of multi information.
Detailed description of the invention
After Fig. 1 is spraying 10% ethanol solution of sulfuric acid colour developing, the cultured ox gallstone inspected under ultraviolet lamp 365nm and artificial is set
The TLC of Moschus schemes.
Fig. 2 is that the will inspected at ultraviolet lamp 365nm increases up to Sa and the TLC of Cuminum celery schemes.
Fig. 3 is to set the cloves TLC figure inspected under ultraviolet lamp 365nm after spraying 10% ethanol solution of sulfuric acid develops the color.
Fig. 4 is after spraying 10% ethanol solution of sulfuric acid develops the color, and the radix aucklandiae TLC inspected under daylight schemes.
Fig. 5 is the TLC figure of the agalloch eaglewood and Long Pepper inspected at ultraviolet lamp 254nm.
Fig. 6 is after spraying 10% ethanol solution of sulfuric acid develops the color, to set the TLC of the agalloch eaglewood and Long Pepper inspected under ultraviolet lamp 365nm
Figure.
Fig. 7 is the caffeic acid TLC figure inspected at ultraviolet lamp 254nm.
Fig. 8 is after spraying 10% ethanol solution of sulfuric acid develops the color, and the caffeic acid TLC inspected under daylight schemes.
Fig. 9 is the dalbergia wood TLC figure inspected at ultraviolet lamp 365nm.
Figure 10 is after spraying 10% ethanol solution of sulfuric acid develops the color, and the dalbergia wood TLC inspected under ultraviolet lamp 365nm schemes.
Figure 11 is the west safflower TLC figure inspected under daylight.
Figure 12 is the safflower TLC figure inspected at ultraviolet lamp 365nm.
In Fig. 1,1 cultured ox gallstone control medicinal material, 2. cultured ox gallstone blank 3.4.5 sample, 6. muscone's blank 7.
Muscone's control medicinal material.
In Fig. 2,1. will increase 2. Cuminum celery control medicinal material 3. of control medicinal material up to Sa and lack the sky that will reaches Sa increasing and Cuminum celery
It is white
4.5.6.7 sample.
Fig. 3,4 are same lamellae, and chromatogram under the conditions of difference is inspected, in figure, 1. cloves control medicinal material, 2. cloves is empty
White 6. radix aucklandiae blank of 3.4.5 sample, 7. radix aucklandiae control medicinal material.
Fig. 5,6 are same lamellae, and chromatogram under the conditions of difference is inspected, in figure, 1. agalloch eaglewood control medicinal material, 2. agalloch eaglewood is empty
White 6. Long Pepper blank of 3.4.5 sample, 7. Long Pepper control medicinal material.
Fig. 7,8 are same lamellae, chromatogram under the conditions of difference is inspected, in figure, 1. caffeic acid reference substance, 2. Fructus Malvae Vertillatae
Blank 3.4.5 sample.
Fig. 9,10 are same lamellae, chromatogram under the conditions of difference is inspected, in figure, the control of 4. dalbergia wood of 1.2.3 sample
5. blank of medicinal material.
Figure 11,12 are same lamellae, and chromatogram under the conditions of difference is inspected, in figure, 1. safflower control medicinal materials 2. are red
Flower 3. west safflower control medicinal material of blank, 4. west safflower blank 5.6.7 sample.
The specific embodiment of the invention is as follows:
(1) this product 3g is taken, it is finely ground, add methanol 5ml, be ultrasonically treated 20 minutes, filtration, filtrate is as test solution；Separately take training
Induced bezoar and each 0.05g of muscone's control medicinal material, respectively plus 2 ml of methanol, ultrasonic treatment 20 minutes, supernatant are used as control
Medicinal material solution；Control medicinal material solution and each 5~6 μ l of test solution are drawn, is put respectively in same silica G F254On lamellae, with
Cyclohexane-ethyl acetate-glacial acetic acid-methanol-water of volume ratio 8.5: 8.5: 1: 1: 0.5 is solvent, is unfolded, and is taken out, hot wind
Drying is sprayed with 10% ethanol solution of sulfuric acid, and 105 DEG C to be heated to spot development clear, is set and is inspected under ultraviolet lamp 365nm, test sample
In chromatography, on position corresponding with cultured ox gallstone reference medicine chromatography, show 2 identical fluorescence principal spots blue, with musk deer
On the fragrant corresponding position of reference medicine chromatography, an identical faint yellow fluorescence principal spot is shown；
(2) it takes will to increase control medicinal material and each 0.1g of Cuminum celery control medicinal material up to Sa, respectively plus 2 ml of methanol, is ultrasonically treated 20 points
Clock, supernatant is as control medicinal material solution；It draws control medicinal material solution and identifies each 6~8 μ l of test solution under (1) item, point
Other point is on same silica gel g thin-layer plate, and using cyclohexane-ethyl acetate-acetone of volume ratio 7: 2: 1 as solvent, expansion is taken
Out, hot blast drying is set and is inspected under ultraviolet lamp 365nm, corresponding increasing reference medicine chromatography up to Sa with will in sample chromatogram
On position, 3 identical red fluorescence principal spots are at least shown, on position corresponding with Cuminum celery reference medicine chromatography, show 2
Identical bright blue fluorescence principal spot；
(3) cloves 0.1g, 0.2 g of radix aucklandiae control medicinal material are taken, respectively plus 2 ml of methanol, is ultrasonically treated 20 minutes, as comparison medicine
Material solution；It draws control medicinal material solution and identifies each 6~8 μ l of test solution under (1) item, put respectively in same silica G thin layer
On plate, using hexamethylene-ethyl acetate-formic acid of volume ratio 8: 2: 0.2 as solvent, it is unfolded, takes out, hot blast drying, spray with 10%
Ethanol solution of sulfuric acid, 105 DEG C to be heated to spot development clear, sets and inspects under ultraviolet lamp 365nm, in sample chromatogram, with
On the corresponding position of cloves reference medicine chromatography, an identical orange-yellow fluorescence spot is shown；It is inspected under daylight, sample chromatogram
In, on position corresponding with cloves and radix aucklandiae reference medicine chromatography, same color principal spot is shown respectively；
(4) agalloch eaglewood control medicinal material and each 0.1g of Long Pepper control medicinal material are taken, respectively plus 2 ml of methanol, is ultrasonically treated 20 minutes, as
Control medicinal material solution；It draws control medicinal material solution and identifies each 6~8 μ l of test solution under (1) item, put respectively in same silica gel
GF254On lamellae, using cyclohexane-ethyl acetate-acetone of volume ratio 7: 2: 1 as solvent, it is unfolded, takes out, hot blast drying,
It sets and is inspected under ultraviolet lamp 254nm, in sample chromatogram, on position corresponding with agalloch eaglewood and Long Pepper reference medicine chromatography, point
It Xian not same color principal spot；Spray is with 10% ethanol solution of sulfuric acid, and 105 DEG C to be heated to spot development clear, sets ultraviolet lamp
It is inspected under 365nm, in sample chromatogram, on position corresponding with agalloch eaglewood reference medicine chromatography, shows two identical sapphirines
Fluorescence principal spot shows two identical glassy yellow fluorescence principal spots on position corresponding with Long Pepper reference medicine chromatography；
(5) it takes caffeic acid reference substance appropriate, adds methanol that solution of every 1ml containing 1mg is made, as reference substance solution；Draw control
5 μ l of product solution, identify 6~8 μ l of test solution under (1) item, put respectively in same silica G F254On lamellae, with volume ratio 6:
4: 0.5 cyclohexane-ethyl acetate-formic acid is solvent, is unfolded, and is taken out, and hot blast drying is set and inspected under ultraviolet lamp 254nm,
In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, same color principal spot is shown；It sprays with 10% ethanol solution of sulfuric acid,
105 DEG C to be heated to spot development clear, inspects under daylight, in sample chromatogram, at the position corresponding to the chromatogram of the reference substance, shows
Same color spot；
(6) 0.2 g of dalbergia wood control medicinal material is taken, 2 ml of methanol is added, is ultrasonically treated 20 minutes, supernatant is as control medicinal material solution；
It draws control medicinal material solution and identifies each 6~8 μ l of test solution under (1) item, put respectively on same silica gel g thin-layer plate, with
2: 1.5 cyclohexane-ethyl acetate of volume ratio is solvent, is unfolded, and takes out, dries, set and inspect under ultraviolet lamp 365nm, for examination
In product chromatography, on position corresponding with reference medicine chromatography, same color fluorescence principal spot is shown；It is sprayed again with 10% sulfuric acid ethyl alcohol
Solution, 105 DEG C to be heated to spot development clear, then sets and inspect under ultraviolet lamp 365nm, in sample chromatogram, with comparison medicine
Wood color is composed on corresponding position, the fluorescence principal spot of at least aobvious 3 same colors；
(7) 0.2 g of safflower control medicinal material, 0.04 g of west safflower control medicinal material are taken, respectively plus 2 ml of methanol, is ultrasonically treated 20 points
Clock, supernatant is as control medicinal material solution；It draws control medicinal material solution and identifies each 6~8 μ l of test solution under (1) item, point
Other point is on same silica gel g thin-layer plate, using acetic ether-methanoic acid-water-methanol of volume ratio 10:2:2.1:0.5 as solvent,
Expansion takes out, dries, set and inspect under daylight, in sample chromatogram, on position corresponding with west safflower reference medicine chromatography,
Show 3 identical yellow principal spots；Set and inspected under ultraviolet lamp 365nm, in sample chromatogram, with safflower reference medicine chromatography
On corresponding position, 1 identical fluorescence principal spot is shown.
Claims (2)
1. a kind of quick thin-layer identification method of multiple medicine taste of Ershiwuwei zhenzhu wan, it is characterised in that:
(1) Ershiwuwei zhenzhu wan 3g is taken, it is finely ground, add methanol 5ml, be ultrasonically treated 20 minutes, filter, filtrate is molten as test sample
Liquid；Cultured ox gallstone and each 0.05g of muscone's control medicinal material separately are taken, respectively plus 2 ml of methanol, is ultrasonically treated 20 minutes, supernatant
As control medicinal material solution；Control medicinal material solution and each 5~6 μ l of test solution are drawn, is put respectively in same silica G F254It is thin
On laminate, using cyclohexane-ethyl acetate-glacial acetic acid-methanol-water of volume ratio 8.5: 8.5: 1: 1: 0.5 as solvent, expansion,
It takes out, hot blast drying, sprays with 10% ethanol solution of sulfuric acid, 105 DEG C to be heated to spot development clear, sets and examines under ultraviolet lamp 365nm
Depending on position corresponding with cultured ox gallstone reference medicine chromatography, showing 2 identical main spots of blue-fluorescence in sample chromatogram
Point shows an identical faint yellow fluorescence principal spot on position corresponding with Moschus reference medicine chromatography；
(2) it takes will to increase control medicinal material and each 0.1g of Cuminum celery control medicinal material up to Sa, respectively plus 2 ml of methanol, is ultrasonically treated 20 points
Clock, supernatant is as control medicinal material solution；It draws control medicinal material solution and identifies each 6~8 μ l of test solution under (1) item, point
Other point is on same silica gel g thin-layer plate, and using cyclohexane-ethyl acetate-acetone of volume ratio 7: 2: 1 as solvent, expansion is taken
Out, hot blast drying is set and is inspected under ultraviolet lamp 365nm, corresponding increasing reference medicine chromatography up to Sa with will in sample chromatogram
On position, 3 identical red fluorescence principal spots are at least shown, on position corresponding with Cuminum celery reference medicine chromatography, show 2
Identical bright blue fluorescence principal spot；
(3) cloves 0.1g, 0.2 g of radix aucklandiae control medicinal material are taken, respectively plus 2 ml of methanol, is ultrasonically treated 20 minutes, as comparison medicine
Material solution；It draws control medicinal material solution and identifies each 6~8 μ l of test solution under (1) item, put respectively in same silica G thin layer
On plate, using hexamethylene-ethyl acetate-formic acid of volume ratio 8: 2: 0.2 as solvent, it is unfolded, takes out, hot blast drying, spray with 10%
Ethanol solution of sulfuric acid, 105 DEG C to be heated to spot development clear, sets and inspects under ultraviolet lamp 365nm, in sample chromatogram, with
On the corresponding position of cloves reference medicine chromatography, an identical orange-yellow fluorescence spot is shown；It is inspected under daylight, sample chromatogram
In, on position corresponding with cloves and radix aucklandiae reference medicine chromatography, same color principal spot is shown respectively；
(4) agalloch eaglewood control medicinal material and each 0.1g of Long Pepper control medicinal material are taken, respectively plus 2 ml of methanol, is ultrasonically treated 20 minutes, as
Control medicinal material solution；It draws control medicinal material solution and identifies each 6~8 μ l of test solution under (1) item, put respectively in same silica gel
GF254On lamellae, using cyclohexane-ethyl acetate-acetone of volume ratio 7: 2: 1 as solvent, it is unfolded, takes out, hot blast drying,
It sets and is inspected under ultraviolet lamp 254nm, in sample chromatogram, on position corresponding with agalloch eaglewood and Long Pepper reference medicine chromatography, point
It Xian not same color principal spot；Spray is with 10% ethanol solution of sulfuric acid, and 105 DEG C to be heated to spot development clear, sets ultraviolet lamp
It is inspected under 365nm, in sample chromatogram, on position corresponding with agalloch eaglewood reference medicine chromatography, shows two identical sapphirines
Fluorescence principal spot shows two identical glassy yellow fluorescence principal spots on position corresponding with Long Pepper reference medicine chromatography；
(5) it takes caffeic acid reference substance appropriate, adds methanol that solution of every 1ml containing 1mg is made, as reference substance solution；Draw control
5 μ l of product solution, identify 6~8 μ l of test solution under (1) item, put respectively in same silica G F254On lamellae, with volume ratio 6:
4: 0.5 cyclohexane-ethyl acetate-formic acid is solvent, is unfolded, and is taken out, and hot blast drying is set and inspected under ultraviolet lamp 254nm,
In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, same color principal spot is shown；It sprays with 10% ethanol solution of sulfuric acid,
105 DEG C to be heated to spot development clear, inspects under daylight, in sample chromatogram, at the position corresponding to the chromatogram of the reference substance, shows
Same color spot；
(6) 0.2 g of dalbergia wood control medicinal material is taken, 2 ml of methanol is added, is ultrasonically treated 20 minutes, supernatant is as control medicinal material solution；
It draws control medicinal material solution and identifies each 6~8 μ l of test solution under (1) item, put respectively on same silica gel g thin-layer plate, with
2: 1.5 cyclohexane-ethyl acetate of volume ratio is solvent, is unfolded, and takes out, dries, set and inspect under ultraviolet lamp 365nm, for examination
In product chromatography, on position corresponding with reference medicine chromatography, same color fluorescence principal spot is shown；It is sprayed again with 10% sulfuric acid ethyl alcohol
Solution, 105 DEG C to be heated to spot development clear, then sets and inspect under ultraviolet lamp 365nm, in sample chromatogram, with comparison medicine
Wood color is composed on corresponding position, the fluorescence principal spot of at least aobvious 3 same colors；
(7) 0.2 g of safflower control medicinal material, 0.04 g of west safflower control medicinal material are taken, respectively plus 2 ml of methanol, is ultrasonically treated 20 points
Clock, supernatant is as control medicinal material solution；It draws control medicinal material solution and identifies each 6~8 μ l of test solution under (1) item, point
Other point is on same silica gel g thin-layer plate, using acetic ether-methanoic acid-water-methanol of volume ratio 10:2:2.1:0.5 as solvent,
Expansion takes out, dries, set and inspect under daylight, in sample chromatogram, on position corresponding with west safflower reference medicine chromatography,
Show 3 identical yellow principal spots；Set and inspected under ultraviolet lamp 365nm, in sample chromatogram, with safflower reference medicine chromatography
On corresponding position, 1 identical fluorescence principal spot is shown.
2. a kind of quick thin-layer identification method of Ershiwuwei zhenzhu wan multiple medicine taste according to claim 1, it is characterised in that
The multiple medicine taste, which refers to, is authenticated flavour of a drug more than ten tastes；Quick thin-layer identification method refers to the thin layer mirror of ten pleasant impression medicinal materials
Not, always the time is spent not exceed 5 hours.
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