CN108956842A - A kind of quick thin-layer identification method of the full taste medicinal material of Danggui Jianzhong Tang freeze-dried powder - Google Patents
A kind of quick thin-layer identification method of the full taste medicinal material of Danggui Jianzhong Tang freeze-dried powder Download PDFInfo
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Abstract
The present invention relates to a kind of quick thin-layer identification methods of the full taste medicinal material of Danggui Jianzhong Tang freeze-dried powder.It is characterized by: obtain test sample and control medicinal material solution with simple, fast pre-treating method, using same test solution, on 4 blocks of lamellaes, 4 kinds different inspect under the conditions of, authenticated 6 taste medicinal materials, inspected more than 10 traditional Chinese medicine ingredients spots;Each clear spot, they intersect, but the ingredient of different levels, and do not interfere with each other.It is 100% that the water, which extracts thin layer identification in preparation and revises and enlarges rate,.All identifying only needs sample 0.5g, Extraction solvent and solvent 67ml, time 3 hours.Easy, quick, the efficient full flavour of a drug thin layer of method identifies, and yet there are no identical report.It is controlled for the quality of Danggui Jianzhong Tang freeze-dried powder, provides simple, fast thin-layer identification method.
Description
Technical field
The present invention relates to a kind of quick thin-layer identification methods of the full taste medicinal material of Danggui Jianzhong Tang freeze-dried powder.
Background technique
In compound Chinese medicinal preparation, the compound preparation that especially traditional water decoction is boiled is made according to the extraction principle of similar compatibility
Fat-soluble ingredient is largely it is difficult to extract arriving in agent, and water soluble ingredient extracts more, interferes with each other serious, and water extracts
Later, identified under crude drug item with the thin layer of liposoluble constituent, some can not use, it is necessary to find the identification of water soluble ingredient
Characteristic point is limited to the difficulty of technology, so the thin layer identification that its water extracts preparation is revised and enlarged, rate is low, and quantitative determination index is few.With
The yiganning granules that the water recorded decocts only have revised and enlarged 4 by 13 taste Chinese medicinal compositions for version Chinese Pharmacopoeia one within 2015
The thin layer of taste medicinal material identifies.Not only it is low to revise and enlarge rate for identification, and discrimination method is also very cumbersome, complicated, and the completions of 4 identifications need
Sample 85g or 15g (containing lactose), only pre-treatment solvent 386ml, time 10~12 hours.4 identifications will prepare 4 kinds of test samples
Solution, on 4 blocks of lamellaes, 4 expansion are completed;The Erding granules recorded are made of 4 taste medicinal materials, have only revised and enlarged a thin layer
Identify.Its pre-treatment needs sample 15g or 3g (containing lactose), processing solvent 82ml, time 2 h;The Er'bao granule recorded, by
Ten simply medicinal material form, revised and enlarged 4 taste medicinal materials thin layer identify.And discrimination method is also very cumbersome, complicated, 4 identifications will make
Standby 3 kinds of test solutions, on 4 blocks of lamellaes, 4 expansion are completed.Need altogether sample 80g, only pre-treatment solvent 295ml, when
Between 8 hours.If the total organic solvent of cost and time are with regard to more in addition solvent and duration of run.Etc., similar example
It is too numerous to mention.
To sum up, thin layer identification is substantially a kind, identifies if any N it is necessary to prepare N kind test solution, N block is thin
N times are unfolded in laminate, identify traditional differential mode of N taste medicinal material.For exclusive PCR, the pre-treatment program of sample is how complicated, tired
It is trivial, it need to use a large amount of organic reagent purification process repeatedly, it is laborious, time-consuming, take reagent, pollution environment, harm health, detection cycle
It is long.In this way, one identifies to detect with the quality standard of binomial assay containing 6~7 thin layers and complete, commonly take up Fei Yizhou's
Time, such as retrial, the time is double, and detection speed seriously restricts modernization of Chinese medicine speed of production.So finding water extracts system
The simplicity of agent, improves detection efficiency, reduces testing cost rapid detection method, is the difficulty that traditional Chinese medicine quality control must be broken through.
Danggui Jianzhong Tang is the classics recipe that State Administration of Traditional Chinese Medicine announces, by Radix Angelicae Sinensis, ramulus cinnamomi, Radix Glycyrrhizae, Radix Paeoniae Alba, ginger
With jujube Six-element medicinal material, prescription is matched and extraction process is as follows:
Prescription: four liang of Radix Angelicae Sinensis, three liang of osmanthus heart, two liang of Radix Glycyrrhizae (toast), six liang of Chinese herbaceous peony, three liang of ginger, 12 pieces of jujube (thumb).
Preparation method: right Six-element,Nozzle, it is a pipeful of with water, it boils and takes three liters, take to boil and take liquid, be concentrated, freeze-drying obtains freeze-dried powder (name
Word is explained: the right side refers to by ancient times from right to left, format write from the top down, by the medicinal material in the prescription of right side, the meaning smashed to pieces,Nozzle refers to the meaning smashed to pieces).
For the quality for ensuring preparation, thin layer is carried out to Danggui Jianzhong Tang and has identified research.
Summary of the invention
The present invention identifies if any N aiming at the previous kind of mesh it is necessary to prepare N kind test solution, N block thin layer
N times are unfolded in plate, identify traditional differential mode of N taste medicinal material.Pass through the various combination of solvent and its ratio, color developing agent, thin layer
The parameter studies such as carrier and testing conditions are created using same test solution, on 4 blocks of lamellaes, 4 kinds of different inspections
Depending under the conditions of, it authenticated 6 taste medicinal materials, the survey for having inspected more than 10 traditional Chinese medicine ingredients spots comments thin layer to identify new model more.Each spot
Point is clear, they intersect, but the ingredient of different levels, and do not interfere with each other.The thin layer identification rate of revising and enlarging is in this preparation
100%.
The present invention solves scheme used by its technical problem are as follows:
A. Danggui Jianzhong Tang freeze-dried powder 0.5g is taken, methanol 2ml is added, is ultrasonically treated 10 minutes, centrifugation, supernatant is used as examination
Product solution;Rhizoma zingiberis control medicinal material 0.1g separately is taken, adds water 30ml, small fire decocts 20 minutes, and filtration, filtrate is concentrated to dryness, and residue adds
Methanol 1ml makes to dissolve, as control medicinal material solution;It takes 6-gingerol reference substance appropriate again, adds methanol to be configured to every 1ml and contain
The solution of 0.5mg, as reference substance solution;Draw 5~6 μ l of control medicinal material solution, 2~3 μ l of reference substance solution, test solution
8~10 μ l are put respectively in same silica G F254On lamellae, with the dense ammonia examination of the chlorofonn-ethylacetate-of volume ratio 5: 3.5: 0.5
Liquid is solvent, is unfolded, and is taken out, hot blast drying, is sprayed molten with 5% vanillin-sulfuric acid solution-ethyl alcohol mixing of volume ratio 1: 8
Liquid, 105 DEG C are heated to rhizoma zingiberis clear spot, set in darkroom and inspect through light, in sample chromatogram, with reference substance and compare
On the corresponding position of medicinal material chromatography, same color principal spot (Fig. 1) is shown respectively;
B. Radix Paeoniae Alba control medicinal material 0.2g is taken, methanol 2ml is added, is ultrasonically treated 20 minutes, supernatant is as control medicinal material solution;
It separately takes Paeoniflorin reference substance appropriate, adds methanol that every 1ml solution containing 1mg is made, as reference substance solution;Draw 5 μ of reference substance solution
L, 5~8 μ l of control medicinal material solution, 8~10 μ l of test solution under A, put respectively in same silica G F254On lamellae, with
Ethyl acetate-butanone-formic acid-water of volume ratio 12.5: 2.2: 1: 0.3 is solvent, is unfolded, and is taken out, hot blast drying, is sprayed with body
Product compares 1: 8 5% vanillin-sulfuric acid solution-ethyl alcohol mixed solution, and 105 DEG C to be heated to spot development clear, under daylight or
It is inspected in darkroom through light, in sample chromatogram, on position corresponding with reference substance and reference medicine chromatography, shows phase respectively
Same color principal spot (Fig. 2,3);
C. Radix Angelicae Sinensis control medicinal material 0.1g is taken, adds methanol 4ml to be ultrasonically treated 20 minutes, takes supernatant molten as control medicinal material
Liquid;Ramulus cinnamomi 0.3g separately is taken, adds water 30ml, small fire decocts 20 minutes, and filtration, filtrate is concentrated to dryness, and residue adds methanol 0.5ml, makes
Dissolution, as ramulus cinnamomi control medicinal material solution;Draw 2~3 μ l of Radix Angelicae Sinensis control medicinal material solution, 15 μ l of ramulus cinnamomi control medicinal material, under A
10~12 μ l of test solution, puts respectively in same silica G F254On lamellae, with hexamethylene-acetic acid of volume ratio 8: 4: 0.1
Ethyl ester-formic acid be solvent, be unfolded, take out, hot blast drying is set and is inspected under ultraviolet lamp 365nm, in sample chromatogram, with
On the corresponding position of Radix Angelicae Sinensis reference medicine chromatography, same color fluorescence principal spot (Fig. 4) is shown;It sets and is inspected under ultraviolet lamp 254nm,
In sample chromatogram, on position corresponding with ramulus cinnamomi reference medicine chromatography, show same color principal spot (Fig. 5);
D. jujube control medicinal material 0.2g is taken, methanol 2ml is added, is ultrasonically treated 20 minutes, centrifugation, supernatant is as control medicinal material
Solution;Extracting liquorice control medicinal material 0.1g again adds methanol 3ml to be ultrasonically treated 20 minutes, and centrifugation, supernatant is as Radix Glycyrrhizae control medicinal material
Solution;2~3 μ l of Radix Glycyrrhizae control medicinal material solution, 4~5 μ l of jujube control medicinal material, 5~6 μ l of test solution under A are drawn, is divided
Other point is with chloroform-ethyl hexanoate-methanol-strong ammonia solution of volume ratio 1: 2: 4: 0.5 on same silica gel g thin-layer plate
Solvent is unfolded, and takes out, hot blast drying, and with 10% sulfuric acid solution, it is clear to be heated to spot development at 105 DEG C for spray, sets ultraviolet light
It is inspected under lamp 365nm, in sample chromatogram, on position corresponding with Radix Glycyrrhizae reference medicine chromatography, shows identical green fluorescence
Principal spot (Fig. 6);It is inspected under daylight, on position corresponding with jujube reference medicine chromatography, shows same color principal spot (figure
7)。
The principle of the present invention is as follows:
Chemical structure and property according to each effective component of Chinese medicine, it then follows the extraction principle of similar compatibility, using suitable
Extraction solvent, simplicity quickly prepare test sample and control medicinal material solution.Again with different component, different ratio, opposed polarity
Solvent is unfolded, and various chemical components will be with different solvents, and foundation Adsorption and desorption is attached, adsorbs, solves again again
The ability of absorption is different, and is able to good separation on respective lamellae.Again by the approximate effective component of various polarity,
On same lamellae, it is different inspect under the conditions of, although overlapping, by different colour developing means, makes it in different layers
It on secondary, does not interfere with each other, shows respectively different spot colors, obtain the thin-layer chromatogram of multi information.Realize it is easy, quick,
Inexpensive, efficient thin layer hope.
It innovative point of the invention and has the beneficial effect that:
Test sample and control medicinal material solution are obtained with simple, fast pre-treating method, using same test solution,
On 4 blocks of lamellaes, 4 kinds different inspect under the conditions of, authenticated 6 taste medicinal materials, inspected more than 10 traditional Chinese medicine ingredients spots;Each spot
Clearly, they intersect, but the ingredient of different levels, and do not interfere with each other.Accomplish that water extracts thin layer in compound preparation and identifies
Revising and enlarging rate is 100%.All identifying only needs sample 0.5g, Extraction solvent and solvent 67ml, time 3 hours.Method is easy, fast
Prompt, efficient, same test solution, the thin layer for completing full flavour of a drug identifies, and yet there are no identical report.
2. rhizoma zingiberis is unfolded, innovates it using chlorofonn-ethylacetate-strong ammonia solution of volume ratio 5: 3.5: 0.5 as solvent
Place be that this solvent be it is alkaline, can with ferulic acid, glycyrrhizic acid in Radix Angelicae Sinensis and Radix Glycyrrhizae in compound preparation etc. it is acid at
It is divided into salt, slows down the attached ability of its Adsorption and desorption, be purified ingredient to be identified, the compound system of a Six-element Chinese medicinal composition
Agent is not required to any processing step, the directly filtrate with methanol ultrasound, and two of ginger are presented only on the lamellae of its expansion
Principal spot, clear spot, no background interference.Using the component of solvent, ratio, soda acid characteristic, the technology of exclusive PCR has
Innovation and practicality.
3. Radix Angelicae Sinensis and ramulus cinnamomi, expansion is unfolded using cyclohexane-ethyl acetate-formic acid of volume ratio 8: 4: 0.1 as solvent
Afterwards, Radix Angelicae Sinensis, which is directly set, inspects bright blue fluorescence principal spot under ultraviolet lamp 365nm;Ramulus cinnamomi is set and inspects palm fibre under ultraviolet lamp 254nm
Brown principal spot;Merely with the self property of ingredient to be detected in Radix Angelicae Sinensis and ramulus cinnamomi, accurate detection judgement can be made, is not required to
Any chromogenic reaction is carried out, it is environmentally protective, to report for the first time.
4. Radix Glycyrrhizae is unfolded using chloroform-ethyl hexanoate-methanol-strong ammonia solution of volume ratio 1: 2: 4: 0.5 as solvent
And jujube, expansion is all water-soluble ingredient, and after these ingredients and 10% sulfuric acid solution react, Radix Glycyrrhizae is in ultraviolet lamp
It is inspected under 365nm, shows green fluorescence principal spot, and jujube unstressed configuration spot;Jujube is inspected in the sunlight is presented a palm fibre
Brown principal spot, and the basic immaculate of Radix Glycyrrhizae;It is different inspect under the conditions of inspect the characteristic spots of each medicinal material, clear spot,
Easily judgement.And the water soluble ingredient spot content of jujube is high, and control medicinal material sampling amount is few, only needs 0.2g, is pharmacopeia sampling amount
One of 1/10, interference component consequently also drops to 1/10, and the principal spot inspected on the lamellae being finally unfolded is made there was only Radix Glycyrrhizae
And jujube, creative and practicability, to report for the first time.
5. not only having accomplished that taste taste medicinal material has mirror in preparation compared with the traditional thin layer enumerated under background technique item identifies
Not, and the identification is completed, and only needs sample 0.5g, Extraction solvent and solvent 67ml, time 3 hours.Method is easy, quick, low
Cost, high one after another, organic solvent-free evaporation, concentration, bring environmental pollution.Have novelty, innovation and practicality, produces
The significant beneficial effect that section money, synergy, comprehensive work under supervision feed intake.
Detailed description of the invention
Fig. 1 is the life inspected in darkroom by light after the colour developing of Danggui Jianzhong Tang freeze-dried powder vanillin-sulfuric acid ethanol solution
Ginger TLC figure.
Fig. 2 is after Danggui Jianzhong Tang freeze-dried powder vanillin-sulfuric acid ethanol solution develops the color, and the Radix Paeoniae Alba TLC inspected under daylight schemes.
After Fig. 3 is the colour developing of Danggui Jianzhong Tang freeze-dried powder vanillin-sulfuric acid ethanol solution, inspected in darkroom by light white
Chinese herbaceous peony TLC figure.
Fig. 4 is the Radix Angelicae Sinensis TLC figure inspected under Danggui Jianzhong Tang freeze-dried powder ultraviolet lamp 365nm.
Fig. 5 is the ramulus cinnamomi TLC figure inspected under Danggui Jianzhong Tang freeze-dried powder ultraviolet lamp 254nm.
Fig. 6 is the Radix Glycyrrhizae TLC that inspects under ultraviolet lamp 254nm after the colour developing of Danggui Jianzhong Tang freeze-dried powder ethanol solution of sulfuric acid
Figure.
Fig. 7 is after Danggui Jianzhong Tang freeze-dried powder ethanol solution of sulfuric acid develops the color, and the jujube TLC inspected under daylight schemes.
In Fig. 1,4. rhizoma zingiberis control medicinal material 5.6- gingerol of 1.2.3 sample.
Fig. 2,3 be same lamellae, difference inspect under the conditions of thin-layer chromatogram, wherein 4. blank sample of 1.2.3 sample
5. Radix Paeoniae Alba control medicinal material of product, 6. Paeoniflorin reference substance
Fig. 4,5 be same lamellae, difference inspect under the conditions of thin-layer chromatogram, wherein 1. ramulus cinnamomi blank, 2. ramulus cinnamomi
6. Radix Angelicae Sinensis control medicinal material of control medicinal material 3.4.5 sample, 7. Radix Angelicae Sinensis blank.
Fig. 6,7 be same lamellae, difference inspect under the conditions of thin-layer chromatogram, wherein 1. jujube blank, 2. jujube
6. Radix Glycyrrhizae control medicinal material of control medicinal material 3.4.5 sample, 7. Radix Glycyrrhizae blank.
The specific embodiment of the invention is as follows:
A. Danggui Jianzhong Tang freeze-dried powder 0.5g is taken, methanol 2ml is added, is ultrasonically treated 10 minutes, centrifugation, supernatant is used as examination
Product solution;Rhizoma zingiberis control medicinal material 0.1g separately is taken, adds water 30ml, small fire decocts 20 minutes, and filtration, filtrate is concentrated to dryness, and residue adds
Methanol 1ml makes to dissolve, as control medicinal material solution;It takes 6-gingerol reference substance appropriate again, adds methanol to be configured to every 1ml and contain
The solution of 0.5mg, as reference substance solution;Draw 5~6 μ l of control medicinal material solution, 2~3 μ l of reference substance solution, test solution
8~10 μ l are put respectively in same silica G F254On lamellae, with the dense ammonia examination of the chlorofonn-ethylacetate-of volume ratio 5: 3.5: 0.5
Liquid is solvent, is unfolded, and is taken out, hot blast drying, is sprayed molten with 5% vanillin-sulfuric acid solution-ethyl alcohol mixing of volume ratio 1: 8
Liquid, 105 DEG C are heated to rhizoma zingiberis clear spot, set in darkroom and inspect through light, in sample chromatogram, with reference substance and compare
On the corresponding position of medicinal material chromatography, same color principal spot is shown respectively;
B. Radix Paeoniae Alba control medicinal material 0.2g is taken, methanol 2ml is added, is ultrasonically treated 20 minutes, supernatant is as control medicinal material solution;
It separately takes Paeoniflorin reference substance appropriate, adds methanol that every 1ml solution containing 1mg is made, as reference substance solution;Draw 5 μ of reference substance solution
L, 5~8 μ l of control medicinal material solution, 8~10 μ l of test solution under A, put respectively in same silica G F254On lamellae, with
Ethyl acetate-butanone-formic acid-water of volume ratio 12.5: 2.2: 1: 0.3 is solvent, is unfolded, and is taken out, hot blast drying, is sprayed with body
Product compares 1: 8 5% vanillin-sulfuric acid solution-ethyl alcohol mixed solution, and 105 DEG C to be heated to spot development clear, under daylight or
It is inspected in darkroom through light, in sample chromatogram, on position corresponding with reference substance and reference medicine chromatography, shows phase respectively
Same color principal spot;
C. Radix Angelicae Sinensis control medicinal material 0.1g is taken, adds methanol 4ml to be ultrasonically treated 20 minutes, takes supernatant molten as control medicinal material
Liquid;Ramulus cinnamomi 0.3g separately is taken, adds water 30ml, small fire decocts 20 minutes, and filtration, filtrate is concentrated to dryness, and residue adds methanol 0.5ml, makes
Dissolution, as ramulus cinnamomi control medicinal material solution;Draw 2~3 μ l of Radix Angelicae Sinensis control medicinal material solution, 15 μ l of ramulus cinnamomi control medicinal material, under A
10~12 μ l of test solution, puts respectively in same silica G F254On lamellae, with hexamethylene-acetic acid of volume ratio 8: 4: 0.1
Ethyl ester-formic acid be solvent, be unfolded, take out, hot blast drying is set and is inspected under ultraviolet lamp 365nm, in sample chromatogram, with
On the corresponding position of Radix Angelicae Sinensis reference medicine chromatography, same color fluorescence principal spot is shown;It sets and is inspected under ultraviolet lamp 254nm, for examination
In product chromatography, on position corresponding with ramulus cinnamomi reference medicine chromatography, same color principal spot is shown;
D. jujube control medicinal material 0.2g is taken, methanol 2ml is added, is ultrasonically treated 20 minutes, centrifugation, supernatant is as control medicinal material
Solution;Extracting liquorice control medicinal material 0.1g again adds methanol 3ml to be ultrasonically treated 20 minutes, and centrifugation, supernatant is as Radix Glycyrrhizae control medicinal material
Solution;2~3 μ l of Radix Glycyrrhizae control medicinal material solution, 4~5 μ l of jujube control medicinal material, 5~6 μ l of test solution under A are drawn, is divided
Other point is with chloroform-ethyl hexanoate-methanol-strong ammonia solution of volume ratio 1: 2: 4: 0.5 on same silica gel g thin-layer plate
Solvent is unfolded, and takes out, hot blast drying, and with 10% sulfuric acid solution, it is clear to be heated to spot development at 105 DEG C for spray, sets ultraviolet light
It is inspected under lamp 365nm, in sample chromatogram, on position corresponding with Radix Glycyrrhizae reference medicine chromatography, shows identical green fluorescence
Principal spot;It is inspected under daylight, on position corresponding with jujube reference medicine chromatography, shows same color principal spot.
Claims (2)
1. a kind of quick thin-layer identification method of the full taste medicinal material of Danggui Jianzhong Tang freeze-dried powder, it is characterised in that:
A. Danggui Jianzhong Tang freeze-dried powder 0.5g is taken, methanol 2ml is added, is ultrasonically treated 10 minutes, is centrifuged, supernatant is molten as test sample
Liquid;Rhizoma zingiberis control medicinal material 0.1g separately is taken, adds water 30ml, small fire decocts 20 minutes, and filtration, filtrate is concentrated to dryness, and residue adds methanol
1ml makes to dissolve, as control medicinal material solution;It takes 6-gingerol reference substance appropriate again, methanol is added to be configured to every 1ml containing 0.5mg's
Solution, as reference substance solution;Draw 5~6 μ l of control medicinal material solution, 2~3 μ l of reference substance solution, 8~10 μ of test solution
L is put respectively in same silica G F254It is exhibition with chlorofonn-ethylacetate-strong ammonia solution of volume ratio 5: 3.5: 0.5 on lamellae
Agent to be opened, is unfolded, is taken out, hot blast drying, spray is with 5% vanillin-sulfuric acid solution-ethyl alcohol mixed solution of volume ratio 1: 8, and 105
DEG C be heated to rhizoma zingiberis clear spot, set in darkroom and inspected through light, in sample chromatogram, with reference substance and comparison medicine wood color
It composes on corresponding position, shows same color principal spot respectively;
B. Radix Paeoniae Alba control medicinal material 0.2g is taken, methanol 2ml is added, is ultrasonically treated 20 minutes, supernatant is as control medicinal material solution;Separately take
Paeoniflorin reference substance is appropriate, adds methanol that every 1ml solution containing 1mg is made, as reference substance solution;Draw 5 μ l of reference substance solution, right
According to 8~10 μ l of test solution under 5~8 μ l of medicinal material solution, A, put respectively in same silica G F254On lamellae, with volume
Ethyl acetate-butanone-formic acid-water than 12.5: 2.2: 1: 0.3 is solvent, is unfolded, and is taken out, hot blast drying, is sprayed with volume ratio
1: 8 5% vanillin-sulfuric acid solution-ethyl alcohol mixed solution, 105 DEG C of clear, under daylight or darkrooms that are heated to spot development
It is interior to be inspected through light, in sample chromatogram, on position corresponding with reference substance and reference medicine chromatography, identical face is shown respectively
Color principal spot;
C. Radix Angelicae Sinensis control medicinal material 0.1g is taken, adds methanol 4ml to be ultrasonically treated 20 minutes, takes supernatant as control medicinal material solution;Separately
Ramulus cinnamomi 0.3g is taken, water 30ml is added, small fire decocts 20 minutes, and filtration, filtrate is concentrated to dryness, and residue adds methanol 0.5ml, make to dissolve,
As ramulus cinnamomi control medicinal material solution;Draw 2~3 μ l of Radix Angelicae Sinensis control medicinal material solution, 15 μ l of ramulus cinnamomi control medicinal material, under A for trying
10~12 μ l of product solution, puts respectively in same silica G F254On lamellae, with the cyclohexane-ethyl acetate-of volume ratio 8: 4: 0.1
Formic acid is solvent, be unfolded, take out, hot blast drying is set and is inspected under ultraviolet lamp 365nm, in sample chromatogram, with Radix Angelicae Sinensis pair
According on the corresponding position of medicinal material chromatography, same color fluorescence principal spot is shown;It sets and is inspected under ultraviolet lamp 254nm, sample chromatogram
In, on position corresponding with ramulus cinnamomi reference medicine chromatography, show same color principal spot;
D. jujube control medicinal material 0.2g is taken, methanol 2ml is added, is ultrasonically treated 20 minutes, is centrifuged, supernatant is molten as control medicinal material
Liquid;Extracting liquorice control medicinal material 0.1g again adds methanol 3ml to be ultrasonically treated 20 minutes, centrifugation, and supernatant is molten as Radix Glycyrrhizae control medicinal material
Liquid;2~3 μ l of Radix Glycyrrhizae control medicinal material solution, 4~5 μ l of jujube control medicinal material, 5~6 μ l of test solution under A are drawn, is distinguished
Point is exhibition with chloroform-ethyl hexanoate-methanol-strong ammonia solution of volume ratio 1: 2: 4: 0.5 on same silica gel g thin-layer plate
Agent is opened, is unfolded, is taken out, hot blast drying, with 10% sulfuric acid solution, it is clear to be heated to spot development at 105 DEG C for spray, sets ultraviolet lamp
It is inspected under 365nm, in sample chromatogram, on position corresponding with Radix Glycyrrhizae reference medicine chromatography, shows identical green fluorescence master
Spot;It is inspected under daylight, on position corresponding with jujube reference medicine chromatography, shows same color principal spot.
2. a kind of quick thin-layer identification method of the full taste medicinal material of Danggui Jianzhong Tang freeze-dried powder according to claim 1, special
Sign is the suitable 3.5~4.2g of primary crude drug of the every 1g of freeze-dried powder.
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CN114894952A (en) * | 2022-06-08 | 2022-08-12 | 国药集团广东环球制药有限公司 | Thin-layer identification method for six traditional Chinese medicine ingredients of angelica Jianzhong decoction |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1167374A1 (en) * | 2000-06-29 | 2002-01-02 | Kibun Food ChemiFA Co., Ltd. | Glycosphingolipid |
CN1668320A (en) * | 2002-07-12 | 2005-09-14 | 株式会社津村 | Tablet composition containing chinese orthodox medicine extract and process for producing the same |
CN1943680A (en) * | 2005-10-09 | 2007-04-11 | 成都华神集团股份有限公司 | A Chinese traditional medicinal composition for treatment of endometriosis and its preparation method |
CN101007072A (en) * | 2007-01-18 | 2007-08-01 | 天津红日药业股份有限公司 | Quality-control method of a traditional Chinese medicine 'Xuebijing' injection |
CN101049389A (en) * | 2007-03-12 | 2007-10-10 | 张文武 | Method for controlling quality of granule preparation for treating chilly sensation type gastritis |
CN106153812A (en) * | 2016-08-04 | 2016-11-23 | 贵阳中医学院 | A kind of detection method of the Chinese medicine preparation treating endometriosis |
CN106841500A (en) * | 2017-03-03 | 2017-06-13 | 四川德成动物保健品有限公司 | The thin-layered chromatography detection method of baked ginger in a kind of female biochemistry mixture of benefit |
-
2018
- 2018-07-27 CN CN201810838360.7A patent/CN108956842B/en active Active
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1167374A1 (en) * | 2000-06-29 | 2002-01-02 | Kibun Food ChemiFA Co., Ltd. | Glycosphingolipid |
CN1668320A (en) * | 2002-07-12 | 2005-09-14 | 株式会社津村 | Tablet composition containing chinese orthodox medicine extract and process for producing the same |
CN1943680A (en) * | 2005-10-09 | 2007-04-11 | 成都华神集团股份有限公司 | A Chinese traditional medicinal composition for treatment of endometriosis and its preparation method |
CN101007072A (en) * | 2007-01-18 | 2007-08-01 | 天津红日药业股份有限公司 | Quality-control method of a traditional Chinese medicine 'Xuebijing' injection |
CN101049389A (en) * | 2007-03-12 | 2007-10-10 | 张文武 | Method for controlling quality of granule preparation for treating chilly sensation type gastritis |
CN106153812A (en) * | 2016-08-04 | 2016-11-23 | 贵阳中医学院 | A kind of detection method of the Chinese medicine preparation treating endometriosis |
CN106841500A (en) * | 2017-03-03 | 2017-06-13 | 四川德成动物保健品有限公司 | The thin-layered chromatography detection method of baked ginger in a kind of female biochemistry mixture of benefit |
Non-Patent Citations (8)
Title |
---|
刘勇 等: "提高归脾丸( 浓缩丸) 质量控制方法的研究", 《中国药品标准》 * |
刘勇 等: "甘草的梯度式多息薄层鉴别研究及其在制剂中应用", 《河北中医》 * |
曾昀等: "紫雪颗粒中甘草、玄参的薄层鉴别", 《今日药学》 * |
毛和平等: "舒气安神丸定性定量方法研究", 《中南药学》 * |
牛伟霞: "加味当归建中颗粒制剂工艺及质量标准研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
董占军 等: "多种中药材的同时鉴别研究", 《中成药》 * |
郭新华 等: "小儿生血颗粒质量标准研究", 《中国中医药信息杂志》 * |
韩桂茹 等: "中药全息薄层色谱鉴别研究", 《中成药》 * |
Cited By (10)
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CN110806459A (en) * | 2019-11-11 | 2020-02-18 | 东阿阿胶股份有限公司 | Multi-medicine-flavor rapid thin-layer identification method and containing device for Erdi decoction reference substance |
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 |
CN112051353A (en) * | 2020-09-23 | 2020-12-08 | 浙江金大康动物保健品有限公司 | Gradient full-information thin-layer identification method for radix peucedani medicinal material |
CN112051353B (en) * | 2020-09-23 | 2022-10-11 | 浙江金大康动物保健品有限公司 | Gradient full-information thin-layer identification method for radix peucedani medicinal material |
CN114689783A (en) * | 2020-12-31 | 2022-07-01 | 四川新绿色药业科技发展有限公司 | Rapid thin-layer identification method for poria cocos, cassia twig, rhizoma atractylodis and licorice root decoction freeze-dried powder |
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CN113156001A (en) * | 2021-03-31 | 2021-07-23 | 湖南易能生物医药有限公司 | Fingerprint construction method and application of Chinese herbal compound containing angelica sinensis |
CN114047282A (en) * | 2021-10-29 | 2022-02-15 | 绍兴双石药业有限公司 | Method for identifying traditional Chinese medicine cassia bark core |
CN114814069A (en) * | 2022-06-08 | 2022-07-29 | 国药集团广东环球制药有限公司 | Thin-layer identification method for 8 medicinal flavors in 9 medicinal flavors of cassia twig, Chinese herbaceous peony and rhizoma anemarrhenae decoction |
CN114894952A (en) * | 2022-06-08 | 2022-08-12 | 国药集团广东环球制药有限公司 | Thin-layer identification method for six traditional Chinese medicine ingredients of angelica Jianzhong decoction |
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