CN110031588A - An a kind of quick thin-layer identification method of plate multiple medicine taste of livestock and poultry antiviral granule - Google Patents
An a kind of quick thin-layer identification method of plate multiple medicine taste of livestock and poultry antiviral granule Download PDFInfo
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Abstract
The present invention relates to an a kind of quick thin-layer identification methods of plate multiple medicine taste of livestock and poultry antiviral granule.It is characterized by: obtaining test sample and control medicinal material solution with simple, fast pre-treating method, using same test solution, on four blocks of lamellaes, it authenticated 10 taste medicinal materials.It is different inspect under the conditions of, inspect different traditional Chinese medicine ingredients, though each ingredient intersects, on different levels, do not interfere with each other, clearly colored speckles or fluorescence spot can be showed.Completing these identifications only needs sample 4g, each 0.1~0.3g of control medicinal material, Extraction solvent and solvent 90ml, the time 3 hours.Easy, quick, efficient, report method does not have at present.Supervision for livestock and poultry antiviral granule feeds intake, and provides method for quick identification.And sulfuric acid colour developing after rhizoma anemarrhenae, fritillaria thunbergii increasing fluorescence spot, the punctation of dried orange peel；The new diagnostic characteristics point of folium isatidis and Radix Isatidis is to report for the first time.
Description
Technical field
The present invention relates to an a kind of quick thin-layer identification methods of plate multiple medicine taste of livestock and poultry antiviral granule.Multiple medicine taste is quickly thin
Layer discrimination method refers to using thin-layer identification method, to the Radix Glycyrrhizae in prescription, dried orange peel, rheum officinale, rhizoma anemarrhenae, honeysuckle, fritillaria thunbergii, bavin
Recklessly, Radix Salviae Miltiorrhizae, folium isatidis, 10 taste Chinese medicine of Radix Isatidis have carried out thin layer identification.It is characterized in that a plate multiple medicine taste means one piece of thin layer
Identify 2-3 taste medicinal material on plate；Quick thin-layer identification method refer to every identification simply medicinal material the spent time be averaged less than 20 minutes,
The reagent of consumption is no more than 10ml.
Background technique
In compound Chinese medicinal preparation, the water of the above prescription of especially 18 tastes extracts compound preparation, since flavour of a drug are more, each medicine
Taste is all again that water extracts, and according to the extraction principle of similar compatibility, liposoluble constituent has not existed substantially, and extraction is all water
Dissolubility or inclined water soluble ingredient, the ingredient humble for some contents, since the ingredient in extraction process polymerize, decomposition, destroys,
Substantially also it is difficult to detect again.So thin layer identification is caused to be revised and enlarged, rate is low, and quantitative determination index is few.Version China in 2015 is consulted
Pharmacopeia one, it is seldom that traditional water more than ten Six-elements recorded extracts compound preparation, has the similar formulations of comparativity to have 6 kinds, that is,
Wushicha granules are made of 19 taste medicinal materials, are control with aurantiamarin, forsythin, enoxolone, and thin layer authenticated 3 taste medicinal materials, reflect
Not revising and enlarging rate is 15.8%；Yunkang capsule is by 23 taste Chinese medicinal compositions, with Astragaloside IV, Radix Angelicae Sinensis, Paeoniflorin, scutelloside, psoralea corylifolia
Element is control, authenticated 5 taste medicinal materials, it is 21.7% that rate is revised and enlarged in identification；The logical holy particle of radix saposhnikoviae is made of 17 taste medicinal materials, with 5-0- first
Base visamminol glycosides, ephedrine hydrochloride, rheum officinale, Gardenoside, campanulaceae, Radix Angelicae Sinensis, Rhizoma Chuanxiong, scutelloside, Radix Glycyrrhizae are control, be authenticated
9 taste medicinal materials, it is 52.9% that rate is revised and enlarged in identification；Wangbi granules are made of 17 taste medicinal materials, with Radix Angelicae Pubescentis, cinnamic acid, Paeoniflorin, chinaroot greenbrier soap
Aglycon is control, authenticated 4 taste medicinal materials, it is 23.5% that rate is revised and enlarged in identification；Resolving stagnation for tranquilization particle is made of 16 taste medicinal materials, with remote
Will, radix bupleuri, Radix Glycyrrhizae are control, authenticated 3 taste medicinal materials, it is 18.8% that rate is revised and enlarged in identification；Sweet dreams capsule is made of 17 taste medicinal materials, with
Wilsonii, Astragaloside IV, fructus lycii, icariin, aurantiamarin are control, authenticated 5 as medicinal material, identify the rate of revising and enlarging and are
29.4%；Rate average out to 27.0%, that is, a system being made of 18 taste medicinal materials are revised and enlarged in the thin layer identification that 6 kinds of water extract preparation
Agent, only about 1/4 medicinal material can identify it whether there is or not feeding intake, and numerous medicinal materials is unable to control its situation that feeds intake, quality mark
Quasi- inspecting 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, one is identified by 7~8 taste medicinal material thin layers and is formed with binomial assay
Quality standard detect complete, commonly take up the time of Fei Yizhou, such as retrial, the time is double, detect speed seriously restrict
Modernization of Chinese medicine speed of production.So find simple, fast detection method, improve detection efficiency, reduce testing cost, just at
Traditional Chinese medicine quality detects the difficulty that must be broken through.Just by taking the logical holy particle of the highest radix saposhnikoviae of rate is revised and enlarged in the identification of above-mentioned thin layer as an example, cut open
Analyse that the specific method is as follows:
[identification] (1) takes this product 6g, finely ground, adds methanol 30ml, is ultrasonically treated 30 minutes, and filtration, filtrate is evaporated, and residue adds
Water 20ml dissolution is extracted 2 times, each 20ml with ethyl acetate shaking, then the n-butanol being saturated with water extracts 2 times, each 20ml,
Merge n-butanol extracting liquid, is evaporated, residue adds methanol 2ml to make to dissolve, as test solution.Separately take 5-0- methyl Wei Sia meter
Alcohol glycosides reference substance adds methanol that solution of every 1ml containing 1mg is made, as reference substance solution.It is tried according to thin-layered chromatography (general rule 502)
It tests, draws 6 μ l of test solution, 2 μ l of reference substance solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol
(4: 1) it is solvent, is unfolded, take out, dry, spray is heated about 3 minutes, ultraviolet lamp with 10% ethanol solution of sulfuric acid at 105 DEG C
It is inspected under 365nm.In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, same color fluorescence spot is shown.
(2) this product 6g is taken, it is finely ground, add methanol 30ml, be ultrasonically treated 30 minutes, filtration, filtrate is evaporated, and residue adds water 10ml
Dissolution adjusts pH value to 10 with 1mol/L sodium hydroxide solution, is extracted 2 times, each 20ml with chloroform shaking, merge trichlorine
Methane extracting solution, low temperature are evaporated, and residue adds methanol 2ml to make to dissolve, as test solution.Ephedrine hydrochloride reference substance separately is taken,
Add methanol that solution of every 1ml containing 1mg is made, as reference substance solution.It tests, is drawn for examination according to thin-layered chromatography (general rule 502)
4~8 μ l of product solution, 5 μ l of reference substance solution are put respectively on same silica gel g thin-layer plate, with chloroform-methanol-strong ammonia solution
(4: 1: 0.1) it is solvent, is unfolded, take out, dry, with ninhydrin solution, it is clear to be heated to spot development at 105 DEG C for spray, day
It is inspected under light.In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, same color spot is shown.
(3) this product 6g is taken, it is finely ground, add hydrochloric acid solution (3 → 20) 10ml, mixes, add chloroform 30ml, be heated to reflux 1
Hour, divide and take chloroform liquid, is evaporated, residue adds methanol 2ml to make to dissolve, as test solution.Separately take rheum officinale control medicinal material
0.5g is made in the same way of control medicinal material solution.It is tested according to thin-layered chromatography (general rule 502), draws above-mentioned each 5 μ l of two kinds of solution, point
Other point is on same silica gel g thin-layer plate, with toluene-Ethyl formate-methyl alcohol-formic acid-water (6: 2: 0.4: 0.1: 1) upper solution
For solvent, it is unfolded, takes out, dry, set and inspected under ultraviolet lamp 365nm.In sample chromatogram, with reference medicine chromatography phase
On the position answered, the orange-yellow fluorescence spot of same color is shown；It sets after being smoked in ammonia, spot becomes red.
(4) take the test solution under [identification] (2) item as test solution.Gardenoside reference substance separately is taken, adds methanol
Solution of every 1ml containing 1mg is made, as reference substance solution.It is tested according to thin-layered chromatography (general rule 502), draws test solution 5
μ l, 2 μ l of reference substance solution are put respectively on same silica gel g thin-layer plate, with 10 DEG C of chloroform-methanol-water (13: 7: 2) or less
Lower layer's solution of placement is solvent, is unfolded, and takes out, dries, and sprays with 5% vanillin-sulfuric acid solution, is heated to spot at 105 DEG C
Colour developing is clear, inspects under daylight.In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, same color spot is shown.
(5) this product 15g is taken, it is finely ground, add the mixed solution 40ml of 7% ethanol solution of sulfuric acid-water (1: 3), it is small to be heated to reflux 3
When, it lets cool, is extracted 2 times, each 20ml with chloroform shaking, merge chloroform extracting solution, washed with water 30ml, discard water
Washing lotion, the chloroform funnel filtration for being covered with anhydrous sodium sulfate, filtrate are evaporated, and residue adds methanol 1ml to make to dissolve, as examination
Product solution.Campanulaceae control medicinal material 1g separately is taken, is made in the same way of control medicinal material solution.It tests, draws according to thin-layered chromatography (general rule 502)
Above-mentioned each 10 μ l of two kinds of solution puts respectively on same silica gel g thin-layer plate, with chloroform-ether (1: 1) for solvent, opens up
It opens, takes out, dry, with 10% ethanol solution of sulfuric acid, it is clear to be heated to spot development at 105 DEG C for spray, inspects in the sunlight, for examination
In product chromatography, on position corresponding with reference medicine chromatography, the spot of same color is shown.
(6) this product 20g is taken, finely ground, add diethyl ether 100ml, is heated to reflux 1 hour, filters, and filtrate recycling design is residual to dry
Slag adds methanol 1ml to make to dissolve, as test solution.Radix Angelicae Sinensis control medicinal material, each 0.5g of Rhizoma Chuanxiong control medicinal material separately are taken, respectively same method
Control medicinal material solution is made.It is tested according to thin-layered chromatography (general rule 502), draws 20 μ l of test solution, control medicinal material solution each 4
μ l is put respectively on same silica gel g thin-layer plate, and with petroleum ether (30~60 DEG C)-ethyl acetate (9: 1) for solvent, expansion is taken
Out, it dries, is inspected at ultraviolet lamp 365nm.In sample chromatogram, on position corresponding with reference medicine chromatography, phase is shown
With the fluorescence spot of color.
(7) this product 5g is taken, it is finely ground, add methanol 30ml, be ultrasonically treated 30 minutes, filtration, filtrate is evaporated, and residue adds water 15ml
Dissolution is extracted 2 times, each 15ml with ether shaking, discards ether solution, and aqueous solution dilute hydrochloric acid adjusts pH value to 1~2, uses second
Acetoacetic ester shaking is extracted 2 times, each 10ml, and combined ethyl acetate extracting solution is evaporated, and residue adds methanol 1ml to make to dissolve, as confession
Test sample solution.Scutelloside reference substance separately is taken, adds methanol that solution of every 1ml containing 1mg is made, as reference substance solution.According to thin layer color
Spectrometry (general rule 502) test, draws each 5 μ l of above two solution, is put respectively on same silica gel g thin-layer plate, with ethyl acetate-
Butanone-formic acid-water (5: 3: 1: 1) is solvent, is unfolded, and takes out, dries, and is sprayed with 2% ferric trichloride ethanol solution, in the sunlight
It inspects.In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, same color spot is shown.
(8) this product 1.5g is taken, it is finely ground, add 0.5mol/L hydrochloric acid solution 5ml, shake 10 minutes, centrifugation, residue adds 50% second
Alcohol 30ml adjusts pH value to 7, heating and refluxing extraction 1 hour with sodium carbonate liquor, and filtration, filtrate concentration is close dry, and residue adds 50%
Ethyl alcohol 2ml makes to dissolve, as test solution.Another extracting liquorice control medicinal material 0.3g, is made in the same way of control medicinal material solution.According to thin layer
Chromatography (general rule 502) test, draws each 5 μ l of above two solution, is put respectively on same silica gel g thin-layer plate, with acetic acid second
Ester-formic acid-glacial acetic acid-water (15: 1: 1: 2) is solvent, is unfolded, and takes out, dries, and is sprayed with 10% ethanol solution of sulfuric acid, 105
It is clear DEG C to be heated to spot development, is inspected at ultraviolet lamp 365nm.In sample chromatogram, corresponding to reference medicine chromatography
Position on, show same color fluorescence spot.
8 thin layers in above-mentioned example identify, and authenticated 9 taste medicinal materials, that is, with 5-0- methyl visamminol glycosides are control
Radix saposhnikoviae, the radix scutellariae that ephedrine hydrochloride is the Chinese ephedra of control, Gardenoside is the cape jasmine of control, scutelloside is control, there are also with right
It is the rheum officinale compareed, campanulaceae, Radix Angelicae Sinensis, Rhizoma Chuanxiong, Radix Glycyrrhizae according to medicinal material, only time for sample pretreatment is it is necessary to spend 20 hours, sample
60g, organic extraction solvent 755ml, in addition solvent 120ml and duration of run 6 hours, the thin layer of 1 batch of sample identifies it is necessary to flower
Remove about 4 days times and 875ml organic solvents.Its premise still has the identification of four traditional Chinese medicine material all and is the reference substance used to do pair
According to, such as according to control medicinal material, the solvent of sample processing time and cost can be more, and reference substance compares, and information content is single,
It 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.Chinese medicine tradition water as dissecting example extracts the method for quality control of compound preparation, because a large amount of fat-soluble low with content
The loss of micro- ingredient, test solution require be enriched with and purify, or even have than example also than it is more cumbersome, complicated, cost
Solvent and time are more.So improving detection efficiency, reducing testing cost, reduce environmental pollution, carves and do not allow at testing staff
The slow objective of the struggle, we are exactly under the background condition, are research pair with a kind of livestock and poultry antiviral granule that traditional water extracts
As having carried out easy, quick, low cost, high efficiency thin-layer identification method discussion, and obtain success.
The composition and preparation process of a kind of livestock and poultry antiviral granule are as follows:
Prescription: 12~14 parts of Radix Isatidis, 10~12 parts of gypsum, 10~12 parts of folium isatidis, 10~12 parts of cornu bubali
10~12 parts of honeysuckle, 5~6 parts of rhizoma anemarrhenae, 10~12 parts of 10~12 parts of Radix Glehniae Radix Ophiopogonis of 10~12 parts of fritillaria thunbergii is old
10~12 portions of skin, 12~14 portions of eupatorium, 5~6 portions of the leaf of bamboo, 5~6 portions of Rheum palmatum (processed with wine), 5~6 portions of Radix Salviae Miltiorrhizae, 5~6 parts of Radix Glycyrrhizae
5~6 parts of radix bupleuri, 5~6 parts of coloured malt of 5~6 parts of stir-baked FRUCTUS CRATAEGI
Preparation process: after dried orange peel, honeysuckle add water distillating extracting oil in prescription, other medicinal materials such as the dregs of a decoction and folium isatidis
Merge, decoction is secondary, and 1.5 hours every time, collecting decoction filtered, and filtrate is concentrated into the medicinal extract of relative density 1.3~1.35；It takes
4 parts of 1 part of medicinal extract plus cane sugar powder, 1 part of dextrin be uniformly mixed, particle is made, it is dry, spray into volatile oil, bored profit mixes, packaging,
To obtain the final product.
Summary of the invention
Establish an a kind of quick thin-layer identification method of plate multiple medicine taste of livestock and poultry antiviral granule.That is, with simple, fast
Pre-treating method obtains test sample and control medicinal material solution, authenticated 10 on four blocks of lamellaes using same test solution
Taste medicinal material.Under the conditions of inspecting, different traditional Chinese medicine ingredients are inspected different, though each ingredient intersects, in different levels
On, it does not interfere with each other, clearly color or fluorescence spot can be showed.Completing these identifications only needs sample 4g, each control medicinal material
0.1~0.3g, Extraction solvent and the total 90ml of solvent, the time 3 hours.It is easy, quick, efficiently, it is that report method is all at present
Do not have.Supervision for livestock and poultry antiviral granule feeds intake, and provides method for quick identification.And rhizoma anemarrhenae, bulb of thunberg fritillary after sulfuric acid colour developing
Female fluorescence spot, the punctation of dried orange peel；The new diagnostic characteristics point of folium isatidis and Radix Isatidis is to report for the first time.
The present invention solves scheme used by its technical problem are as follows:
(1) the thin layer identification of Radix Glycyrrhizae, dried orange peel and rheum officinale takes livestock and poultry antiviral granule 4g, finely ground, adds methanol 15ml, at ultrasound
Reason 15 minutes, filtration, filtrate are evaporated, and residue adds methanol 1ml to make to dissolve, as test solution；Another extracting liquorice control medicinal material
0.1g, dried orange peel control medicinal material 0.2g, finely ground, respectively plus methanol 2ml is ultrasonically treated 15 minutes, takes supernatant as Radix Glycyrrhizae and dried orange peel
Control medicinal material solution；Rheum officinale control medicinal material 0.2g is taken again, adds water 40ml, small fire decocts 30 minutes, and cotton filtration, filtrate is evaporated,
Residue adds methanol 1ml to make to dissolve, as rheum officinale control medicinal material；Draw each 5~6 μ l of above-mentioned control medicinal material solution, test solution 5
μ l is put respectively in same silica G F254On lamellae, with the dense ammonia examination of chlorofonn-ethylacetate-methanol-of volume ratio 8: 2: 4: 0.5
Liquid is solvent, is unfolded, and is taken out, and hot blast drying is set and inspected under ultraviolet lamp 365nm, in sample chromatogram, with Radix Glycyrrhizae and old
On the corresponding position of skin reference medicine chromatography, show identical bright blue fluorescence principal spot respectively, with rheum officinale reference medicine chromatography
On corresponding position, at least show an identical red fluorescence spot (see Fig. 1)；5% vanillic aldehyde for being 1: 6 with volume ratio is sprayed again
The mixed solution of sulfuric acid solution and ethyl alcohol, it is clear to be heated to spot development at 105 DEG C, inspects under daylight, in sample chromatogram,
On position corresponding with dried orange peel reference medicine chromatography, show identical red principal spot (see Fig. 2)；
(2) rhizoma anemarrhenae and the thin layer of honeysuckle identification takes rhizoma anemarrhenae control medicinal material 0.2g, honeysuckle control medicinal material 0.3g, respectively plus
Methanol 2ml is ultrasonically treated 15 minutes, and supernatant is as respective control medicinal material solution；3~5 μ l of control medicinal material solution is drawn,
(1) 5~6 μ l of test solution under item, puts respectively in same silica G F254It is 3.1: 1: 1 just with volume ratio on lamellae
Butanol-glacial acetic acid-water is solvent, is unfolded, and is taken out, and hot blast drying is set and inspected under ultraviolet lamp 365nm, in sample chromatogram,
On position corresponding with honeysuckle reference medicine chromatography, show the fluorescence principal spot of same color (see Fig. 3)；It is sprayed again with 10% sulphur
Sour ethanol solution, 105 DEG C to be heated to spot development clear, then sets and inspect under ultraviolet lamp 365nm, in sample chromatogram, with
On the corresponding position of rhizoma anemarrhenae reference medicine chromatography, show identical brilliant blue green fluorescence principal spot (see Fig. 4)；
(3) thin layer of fritillaria thunbergii and radix bupleuri identification takes fritillaria thunbergii control medicinal material 0.3g, radix bupleuri 0.2g, respectively plus methanol 2ml,
Ultrasonic treatment 15 minutes, supernatant is as control medicinal material solution.The test solution drawn under control medicinal material solution and (1) item is each
5~8 μ l put the chloroform-ethyl acetate-first for being 10: 4: 3: 0.5 with volume ratio on same silica gel g thin-layer plate respectively
Alcohol-strong ammonia solution is solvent, is unfolded, and is taken out, and hot blast drying is set and inspected under ultraviolet lamp 365nm, in sample chromatogram,
On position corresponding with radix bupleuri reference medicine chromatography, show the fluorescence spot of a same color (see Fig. 5)；Spray is with 10% sulfuric acid
Ethanol solution, 105 DEG C to be heated to spot development clear, sets and inspects under ultraviolet lamp 365nm, in sample chromatogram, with bulb of thunberg fritillary
On female corresponding position of reference medicine chromatography, show identical brilliant blue purple fluorescence principal spot (see Fig. 6)；It is set in darkroom again through lamp
Light is inspected, and in sample chromatogram, on position corresponding with fritillaria thunbergii and radix bupleuri reference medicine chromatography, shows identical brown respectively
Color principal spot (see Fig. 7)；
(4) the thin layer identification of Radix Salviae Miltiorrhizae, folium isatidis, Radix Isatidis takes folium isatidis control medicinal material 0.2g, Radix Isatidis control medicinal material
0.3g is ultrasonically treated 15 minutes, supernatant is as folium isatidis and Radix Isatidis control medicinal material solution respectively plus methanol 2ml；Separately take pellet
To join control medicinal material 0.3g, adds water 40ml, small fire decocts 30 minutes, and cotton filtration, filtrate is evaporated, and residue adds methanol 1ml to make to dissolve,
As Radix Salviae Miltiorrhizae control medicinal material solution；Draw folium isatidis and each 5~6 μ l of Radix Isatidis control medicinal material solution, Radix Salviae Miltiorrhizae control medicinal material solution
12 μ l of test solution under 10 μ l, (1) item, puts respectively in same silica G F254On lamellae, with volume ratio for 6: 4.5: 0.1
Cyclohexane-ethyl acetate-formic acid be solvent, be unfolded, take out, hot blast drying sets and inspect under ultraviolet lamp 254nm, for examination
In product chromatography, on position corresponding with Radix Salviae Miltiorrhizae reference medicine chromatography, show same color principal spot (see Fig. 8)；Spray is with volume ratio
For the mixed solution of 1: 6 5% vanillin-sulfuric acid solution and ethyl alcohol, it is clear to be heated to spot development at 105 DEG C, sets in darkroom thoroughly
It crosses light to inspect, in sample chromatogram, on position corresponding with folium isatidis and Radix Isatidis reference medicine chromatography, show respectively identical
Color principal spot (see Fig. 9).
The principle of the invention is as follows:
According to the chemical structure of each effective component of Chinese medicine and polarity difference, with the movement of solvent, on lamellae
The attached ability of Adsorption and desorption and it is different, so that the spot of each effective component is separated.Again by each compositional polarity size, choosing
The approximate effective component of polarity is taken, different under the conditions of inspecting, respectively different colored speckles are presented, though it is overlapped,
It does not interfere with each other again, 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) compound Chinese medicinal preparation that a traditional water extracts is breached, there are N identifications molten it is necessary to prepare N kind test sample
N times are unfolded in liquid, N block lamellae, identify traditional identification method of N taste medicinal material.It establishes using same test solution, methanol
After ultrasound or water decoct, each control medicinal material solution of methanol constant volume authenticated 10 taste medicinal materials on four blocks of lamellaes, different
Under the conditions of inspecting, different traditional Chinese medicine ingredients are inspected；Each clear spot, intersects, but the ingredient of different levels, and does not do mutually
It disturbs.The identification that traditional water extracts the livestock and poultry antiviral granule of preparation is revised and enlarged into rate by average 27.0%, is increased to 55.6%.This Shen
10 taste medicinal materials please identify each detection for completing a collection of sample compared with 9 taste medicinal materials in the logical holy particle of radix saposhnikoviae identify, the application
Only need sample 4g, each 0.1~0.3g of control medicinal material, Extraction solvent and the total 90ml of solvent, 4 pieces of lamellae, 3 hours time；And
The logical holy particle of radix saposhnikoviae then needs sample 60g, 26 hours time, solvent 875ml, 8 pieces of lamellae.In contrast, this Shen is shown
Please it is easy, quick, efficient and higher identification revise and enlarge rate, be currently report method do not have.Both have and break through
Conventional novelty, and have and improve detection efficiency, save testing cost, the practicability to reduce environmental pollution.
(2) on same lamellae, the bright blue fluorescence spot of honeysuckle is directly detected under ultraviolet lamp 365nm, and
The clear chartreuse fluorescence spot of rhizoma anemarrhenae blur margin is not interfered (see Fig. 3), after spraying 10% ethanol solution of sulfuric acid colour developing, sample
Other original fluorescence spots all disappear, and the very high brilliant blue green fluorescence spot of rhizoma anemarrhenae sensitivity is only presented (see Fig. 4).It is different
Inspect under the conditions of inspect different medicinal materials, effectively increase the clarity and specificity of identification.
(3) the fritillaria thunbergii thin layer that document records at present identifies, and is mostly the colored speckles meeting alkaloid reagent and developing the color identified,
The amount of required fritillaria thunbergii will reach 5g, be converted to water and extract this preparation, even if converting by 50% recovery rate, also want 200g sample,
Sampling amount is big, can not be identified.So having invented using the means for increasing fluorescence, taking for fritillaria thunbergii is considerably reduced
Sample amount only needs control medicinal material 0.3g, i.e., the 1/17 of 5g.Fritillaria thunbergii is at ultraviolet lamp 365nm, and directly detection is that nothing is appointed
(see 1 in Fig. 5) of what information spot, but after spraying 10% ethanol solution of sulfuric acid colour developing, then set and examined under ultraviolet lamp 365nm
Depending on fritillaria thunbergii control medicinal material presents 4 bluish violet fluorescence spots, other original fluorescence spots of sample all disappear, and is only in
Reveal five bluish violet fluorescence spots with sulfuric acid reaction, wherein 2 exclusive spots for fritillaria thunbergii, 2 are to share spot, 1
A spot (see Fig. 6) presented for other medicinal materials eliminates the original numerous fluorescence spot interference of sample, it is glimmering to obtain fritillaria thunbergii increasing
New diagnostic characteristics point after light.Identify for the fritillaria thunbergii that water decocts, provides highly sensitive, simple, fast thin layer identification side
Method is prime report.
(4) thin layer of dried orange peel identifies, and is to be detected with dried orange peel glycosides for control under one dried orange peel item of Chinese Pharmacopoeia.It needs
Match two kinds of different solvents, after carrying out second outspread, spray is inspected under ultraviolet lamp 365nm with alchlor test solution.This
Application is with dried orange peel medicinal material for control, with alkaline developers, the dense ammonia of chlorofonn-ethylacetate-methanol-of volume ratio 8: 2: 4: 0.5
After test solution expansion, directly sets and inspected under ultraviolet lamp 365nm, test sample is in position corresponding with Radix Glycyrrhizae and dried orange peel reference medicine chromatography
Set, show identical bright blue fluorescence principal spot respectively, spray with volume ratio be 1: 6 5% vanillin-sulfuric acid solution and ethyl alcohol it is mixed
Close solution colour developing after, inspected under daylight, on test sample position corresponding with dried orange peel reference medicine chromatography, present respectively one it is old
The distinctive punctation of skin；The different colours spot that dried orange peel is presented under the conditions of two kinds of differences are inspected, further enhances thin layer
The specificity of identification, to report for the first time.
(5) it is well known that Radix Isatidis and folium isatidis are same plants, i.e. different parts of cruciferae isatis,
Folium isatidis is its leaf portion, and Radix Isatidis is its root.Folium isatidis is all with indigo red and indigo for control, progress thin layer identification；Plate
Blue root is then to be accused with amino acid (arginine) and (R, S)-according to spring reference substance for control, the amino acid face of detection and ninhydrin colour developing
Color spot point and at ultraviolet lamp 254nm directly inspects (R, S)-and accuses colored speckles according to the spring.Indigo red and it is indigo belong to it is miscellaneous
Cycle compound is inclined liposoluble constituent, and content is again low, is that substantially can't detect it after water decoction about 0.02% in crude drug
Spot information；And the colored speckles presented under the amino acids and ultraviolet lamp 254nm of Radix Isatidis, it is not exclusive spot,
It is all existing in a variety of medicinal materials；So interference of the livestock and poultry antiviral granule being made of 18 taste medicinal materials because of blank, Wu Fajin
Row identifies.Inquired into repeatedly find it is a kind of neither amino acids, do not presented again at ultraviolet lamp 254nm spot (see Fig. 8 kind
9), and the chemical component that the very high folium isatidis of content and Radix Isatidis all have, that is, the 5% vanillic aldehyde sulphur for being 1: 6 with volume ratio
The spot of the mixed solution of acid solution and ethyl alcohol presentation color (see 5 and 9 in Fig. 9).Though belong to it is partially fat-soluble, because of content
Height, folium isatidis control medicinal material only need 0.2g, Radix Isatidis only to need 0.3g, are dissolved in 2ml methanol respectively, and 5 μ l of point sample can be presented
Dense colored speckles out cook agent and provide new diagnostic characteristics point, to report for the first time for folium isatidis and Radix Isatidis decocting.Tool
Innovation and practicality.
(6) the application is compared with the thin-layer identification method that current prescription cooks agent with Chinese medicine decocting that preparation process is similar,
The flavour of a drug not only detected are most, and the time spent and organic reagent are minimum, and environmental pollution is low, form a set of easy, fast
Prompt, efficient, low consumption, low pollution, multiple medicine taste, the quick thin-layer identification method of multi information.
Detailed description of the invention
The punctation TLC of Radix Glycyrrhizae, dried orange peel bright blue fluorescence principal spot and the rheum officinale inspected under Fig. 1 ultraviolet lamp 365nm
Figure.
After Fig. 2 is sprayed the colour developing of vanillin-sulfuric acid ethanol solution, the punctation TLC for the dried orange peel inspected under daylight schemes.
The honeysuckle bright blue fluorescence spot TLC figure inspected under Fig. 3 ultraviolet lamp 365nm.
After Fig. 4 is sprayed the colour developing of 10% ethanol solution of sulfuric acid, the rhizoma anemarrhenae brilliant blue green fluorescence spot inspected under ultraviolet lamp 365nm
Point TLC figure.
The campanulaceae blue-fluorescence spot TLC figure inspected under Fig. 5 ultraviolet lamp 365nm.
After Fig. 6 is sprayed the colour developing of 10% ethanol solution of sulfuric acid, the fritillaria thunbergii bluish violet spot inspected under ultraviolet lamp 365nm
TLC figure.
Fig. 7 is the campanulaceae and fritillaria thunbergii sepia spot TLC inspected through light after the colour developing of 10% ethanol solution of sulfuric acid
Figure.
The Radix Salviae Miltiorrhizae sepia spot TLC figure inspected under Fig. 8 ultraviolet lamp 254nm.
After Fig. 9 is sprayed the colour developing of vanillin-sulfuric acid ethanol solution, the Radix Isatidis inspected through light and folium isatidis brownish red master
Spot TLC figure.
Fig. 1,2 are same lamellae, difference inspect under the conditions of chromatogram, in figure, 1. Radix Glycyrrhizae control medicinal materials；2. Radix Glycyrrhizae
Blank；3.6.7 sample；4. rheum officinale blank；5. rheum officinale；8. dried orange peel blank；9. dried orange peel control medicinal material.
Fig. 3,4 are same lamellae, difference inspect under the conditions of chromatogram, in figure, 1.2.3 sample；4. honeysuckle is empty
It is white；5. honeysuckle control medicinal material；6. rhizoma anemarrhenae；7. rhizoma anemarrhenae blank.
Fig. 5,6,7 are same lamellae, difference inspect under the conditions of chromatogram, in figure, 1. fritillaria thunbergii control medicinal materials；2.
Fritillaria thunbergii blank；3.4.5 sample；6. radix bupleuri blank；7. radix bupleuri control medicinal material.
Fig. 8,9 are same lamellae, difference inspect under the conditions of chromatogram, in figure, 1. Radix Salviae Miltiorrhizae control medicinal materials；2. Radix Salviae Miltiorrhizae
Blank；3.4.6.7 sample；5. folium isatidis；8. folium isatidis and Radix Isatidis blank；9. Radix Isatidis control medicinal material.
The specific embodiment of the invention is as follows:
(1) the thin layer identification of Radix Glycyrrhizae, dried orange peel and rheum officinale takes livestock and poultry antiviral granule 4g, finely ground, adds methanol 15ml, at ultrasound
Reason 15 minutes, filtration, filtrate are evaporated, and residue adds methanol 1ml to make to dissolve, as test solution；Another extracting liquorice control medicinal material
0.1g, dried orange peel control medicinal material 0.2g, finely ground, respectively plus methanol 2ml is ultrasonically treated 15 minutes, takes supernatant as Radix Glycyrrhizae and dried orange peel
Control medicinal material solution；Rheum officinale control medicinal material 0.2g is taken again, adds water 40ml, small fire decocts 30 minutes, and cotton filtration, filtrate is evaporated,
Residue adds methanol 1ml to make to dissolve, as rheum officinale control medicinal material；Draw each 5~6 μ l of above-mentioned control medicinal material solution, test solution 5
μ l is put respectively in same silica G F254On lamellae, with the dense ammonia examination of chlorofonn-ethylacetate-methanol-of volume ratio 8: 2: 4: 0.5
Liquid is solvent, is unfolded, and is taken out, and hot blast drying is set and inspected under ultraviolet lamp 365nm, in sample chromatogram, with Radix Glycyrrhizae and old
On the corresponding position of skin reference medicine chromatography, show identical bright blue fluorescence principal spot respectively, with rheum officinale reference medicine chromatography
On corresponding position, an identical red fluorescence spot is at least shown；It is molten that 5% vanillin-sulfuric acid for being 1: 6 with volume ratio is sprayed again
The mixed solution of liquid and ethyl alcohol, it is clear to be heated to spot development at 105 DEG C, inspects under daylight, in sample chromatogram, with dried orange peel
On the corresponding position of reference medicine chromatography, identical red principal spot is shown；
(2) rhizoma anemarrhenae and the thin layer of honeysuckle identification takes rhizoma anemarrhenae control medicinal material 0.2g, honeysuckle control medicinal material 0.3g, respectively plus
Methanol 2ml is ultrasonically treated 15 minutes, and supernatant is as respective control medicinal material solution；3~5 μ l of control medicinal material solution is drawn,
(1) 5~6 μ l of test solution under item, puts respectively in same silica G F254It is 3.1: 1: 1 just with volume ratio on lamellae
Butanol-glacial acetic acid-water is solvent, is unfolded, and is taken out, and hot blast drying is set and inspected under ultraviolet lamp 365nm, in sample chromatogram,
On position corresponding with honeysuckle reference medicine chromatography, the fluorescence principal spot of same color 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 rhizoma anemarrhenae pair
According on the corresponding position of medicinal material chromatography, identical brilliant blue green fluorescence principal spot is shown；
(3) thin layer of fritillaria thunbergii and radix bupleuri identification takes fritillaria thunbergii control medicinal material 0.3g, radix bupleuri 0.2g, respectively plus methanol 2ml,
Ultrasonic treatment 15 minutes, supernatant is as control medicinal material solution.The test solution drawn under control medicinal material solution and (1) item is each
5~8 μ l put the chloroform-ethyl acetate-first for being 10: 4: 3: 0.5 with volume ratio on same silica gel g thin-layer plate respectively
Alcohol-strong ammonia solution is solvent, is unfolded, and is taken out, and hot blast drying is set and inspected under ultraviolet lamp 365nm, in sample chromatogram,
On position corresponding with radix bupleuri reference medicine chromatography, the fluorescence spot of a same color is shown；It sprays molten with 10% sulfuric acid ethyl alcohol
Liquid, 105 DEG C to be heated to spot development clear, sets and inspects under ultraviolet lamp 365nm, in sample chromatogram, compares with fritillaria thunbergii
On the corresponding position of medicinal material chromatography, identical brilliant blue purple fluorescence principal spot is shown；It sets in darkroom and is inspected through light again, test sample
In chromatography, on position corresponding with fritillaria thunbergii and radix bupleuri reference medicine chromatography, identical sepia principal spot is shown respectively；
(4) the thin layer identification of Radix Salviae Miltiorrhizae, folium isatidis, Radix Isatidis takes folium isatidis control medicinal material 0.2g, Radix Isatidis control medicinal material
0.3g is ultrasonically treated 15 minutes, supernatant is as folium isatidis and Radix Isatidis control medicinal material solution respectively plus methanol 2ml；Separately take pellet
To join control medicinal material 0.3g, adds water 40ml, small fire decocts 30 minutes, and cotton filtration, filtrate is evaporated, and residue adds methanol 1ml to make to dissolve,
As Radix Salviae Miltiorrhizae control medicinal material solution；Draw folium isatidis and 5~6 μ l of Radix Isatidis control medicinal material solution, 10 μ of Radix Salviae Miltiorrhizae control medicinal material solution
L, the 12 μ l of test solution under (1) item, puts respectively in same silica G F254It is 6: 4.5: 0.1 with volume ratio on lamellae
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, test sample
In chromatography, on position corresponding with Radix Salviae Miltiorrhizae reference medicine chromatography, same color principal spot is shown；Spray is with 5% that volume ratio is 1: 6
The mixed solution of vanillin-sulfuric acid solution and ethyl alcohol, it is clear to be heated to spot development at 105 DEG C, sets in darkroom and examines through light
Depending on position corresponding with folium isatidis and Radix Isatidis reference medicine chromatography, showing the main spot of same color respectively in sample chromatogram
Point.
Claims (2)
1. an a kind of quick thin-layer identification method of plate multiple medicine taste of livestock and poultry antiviral granule, it is characterised in that:
(1) the thin layer identification of Radix Glycyrrhizae, dried orange peel and rheum officinale takes livestock and poultry antiviral granule 4g, finely ground, adds methanol 15ml, is ultrasonically treated
15 minutes, filtration, filtrate was evaporated, and residue adds methanol 1ml to make to dissolve, as test solution；Another extracting liquorice control medicinal material 0.1g,
Dried orange peel control medicinal material 0.2g, finely ground, respectively plus methanol 2ml is ultrasonically treated 15 minutes, and supernatant is taken to compare as Radix Glycyrrhizae and dried orange peel
Medicinal material solution；Rheum officinale control medicinal material 0.2g is taken again, adds water 40ml, and small fire decocts 30 minutes, and cotton filtration, filtrate is evaporated, residue
Methanol 1ml is added to make to dissolve, as rheum officinale control medicinal material；Each 5~6 μ l of above-mentioned control medicinal material solution, 5 μ l of test solution are drawn,
It is put respectively in same silica G F254On lamellae, it is with chlorofonn-ethylacetate-methanol-strong ammonia solution of volume ratio 8: 2: 4: 0.5
Solvent, be unfolded, take out, hot blast drying is set and is inspected under ultraviolet lamp 365nm, in sample chromatogram, with Radix Glycyrrhizae and dried orange peel pair
According on the corresponding position of medicinal material chromatography, identical bright blue fluorescence principal spot is shown respectively, corresponding to rheum officinale reference medicine chromatography
Position on, at least show an identical red fluorescence spot；Spray again with volume ratio be 1: 6 5% vanillin-sulfuric acid solution with
The mixed solution of ethyl alcohol, it is clear to be heated to spot development at 105 DEG C, inspects under daylight, in sample chromatogram, compares with dried orange peel
On the corresponding position of medicinal material chromatography, identical red principal spot is shown；
(2) rhizoma anemarrhenae and the identification of the thin layer of honeysuckle take rhizoma anemarrhenae control medicinal material 0.2g, honeysuckle control medicinal material 0.3g, respectively plus first
Alcohol 2ml is ultrasonically treated 15 minutes, and supernatant is as respective control medicinal material solution；Draw 3~5 μ l of control medicinal material solution, (1)
5~6 μ l of test solution under, puts respectively in same silica G F264On lamellae, the positive fourth for being 3.1: 1: 1 with volume ratio
Alcohol-glacial acetic acid-water is solvent, is unfolded, and is taken out, and hot blast drying is set and inspected under ultraviolet lamp 365nm, in sample chromatogram,
On position corresponding with honeysuckle reference medicine chromatography, the fluorescence principal spot of same color is shown；It sprays again molten with 10% sulfuric acid ethyl alcohol
Liquid, 105 DEG C to be heated to spot development clear, then sets and inspect under ultraviolet lamp 365nm, in sample chromatogram, compares with rhizoma anemarrhenae
On the corresponding position of medicinal material chromatography, identical brilliant blue green fluorescence principal spot is shown；
(3) thin layer of fritillaria thunbergii and radix bupleuri identification takes fritillaria thunbergii control medicinal material 0.3g, radix bupleuri 0.2g, respectively plus methanol 2ml, surpasses
Sonication 15 minutes, supernatant was as control medicinal material solution.Draw the test solution each 5 under control medicinal material solution and (1) item
~8 μ l put the chloroform-acetate-methanol-for being 10: 4: 3: 0.5 with volume ratio on same silica gel g thin-layer plate respectively
Strong ammonia solution is solvent, be unfolded, take out, hot blast drying is set and is inspected under ultraviolet lamp 365nm, in sample chromatogram, with bavin
On the corresponding position of Hu reference medicine chromatography, the fluorescence spot of a same color is shown；It sprays 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 fritillaria thunbergii control medicinal material
On the corresponding position of chromatography, identical brilliant blue purple fluorescence principal spot is shown；It sets in darkroom and is inspected through light again, sample chromatogram
In, on position corresponding with two reference medicine chromatographies, identical sepia principal spot is shown respectively；
(4) the thin layer identification of Radix Salviae Miltiorrhizae, folium isatidis, Radix Isatidis takes folium isatidis control medicinal material 0.2g, Radix Isatidis control medicinal material 0.3g,
Respectively plus methanol 2ml, it is ultrasonically treated 15 minutes, supernatant is as folium isatidis and Radix Isatidis control medicinal material solution；Separately take Radix Salviae Miltiorrhizae pair
According to medicinal material 0.3g, adding water 40ml, small fire decocts 30 minutes, and cotton filtration, filtrate is evaporated, and residue adds methanol 1ml to make to dissolve, as
Radix Salviae Miltiorrhizae control medicinal material solution；Draw folium isatidis and each 5~6 μ l of Radix Isatidis control medicinal material solution, 10 μ l of Radix Salviae Miltiorrhizae control medicinal material solution,
(1) the 12 μ l of test solution under item, puts respectively in same silica G F254On lamellae, the ring for being 6: 4.5: 0.1 with volume ratio
Hexane-ethylacetate-formic acid is solvent, is unfolded, and is taken out, and hot blast drying is set and inspected under ultraviolet lamp 254nm, test sample color
In spectrum, on position corresponding with Radix Salviae Miltiorrhizae reference medicine chromatography, same color principal spot is shown；Spray is with 5% perfume that volume ratio is 1: 6
The mixed solution of oxalaldehyde sulfuric acid solution and ethyl alcohol, it is clear to be heated to spot development at 105 DEG C, sets in darkroom and inspects through light,
In sample chromatogram, on position corresponding with folium isatidis and Radix Isatidis reference medicine chromatography, same color principal spot is shown respectively.
2. an a kind of quick thin-layer identification method of plate multiple medicine taste of livestock and poultry antiviral granule according to claim 1, special
Sign is that a plate multiple medicine taste means identification 2-3 taste medicinal material on one block of lamellae；Quick thin-layer identification method refers to every identification simply
Medicinal material the spent time, the average reagent less than 20 minutes, consumption was no more than 10ml.
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| CN110954645B (en) * | 2019-09-09 | 2020-09-29 | 山东琪康生物技术有限公司 | Detection method of high-quality Sihuang dysentery stopping granules |
| CN110412184A (en) * | 2019-09-10 | 2019-11-05 | 江西倍肯药业有限公司 | A kind of detection method of quickly allaying infantile fever particle |
| CN111830187A (en) * | 2020-06-02 | 2020-10-27 | 鉴甄检测技术（上海）有限公司 | Rapid thin-layer identification method for multiple medicines in small radix bupleuri granule finished product |
| CN111735901A (en) * | 2020-07-09 | 2020-10-02 | 四川大学 | Gradient full-information thin-layer identification method for multi-source rhubarb medicinal material |
| CN113567610A (en) * | 2021-07-13 | 2021-10-29 | 数源汇通（北京）医药科技有限公司 | Thin-layer chromatography identification method for shalian stomach harmonizing capsules |
| CN118130694A (en) * | 2024-05-08 | 2024-06-04 | 中国中医科学院中药研究所 | Quality control method of modified Sixisan granules |
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