CN102085220A - Thin-layer identification method with fluorescence intensifier detection for traditional Chinese medicines - Google Patents
Thin-layer identification method with fluorescence intensifier detection for traditional Chinese medicines Download PDFInfo
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Abstract
The invention discloses a thin-layer identification method with fluorescence intensifier detection for traditional Chinese medicines. In the method, on the basis of common thin-layer identification, a fluorescence intensifier is additionally provided for identifying various traditional Chinese medicines without detection information, and ideal results are acquired, thus the detection way of thin-layer identification is greatly widened, and the revised and enlarged rate of thin-layer identification in traditional Chinese medicine preparations can be effectively improved.
Description
Technical field
The present invention relates to a kind of thin layer discrimination method of Chinese crude drug, particularly, what relate to a kind of Chinese crude drug increases fluoroscopic examination thin layer discrimination method.
Background technology
In all kinds of Chinese medicine preparation quality standards of country, the thin layer of its medical material differentiates that the rate of revising and enlarging is low at present, on average is about 30% of prescription Chinese crude drug total amount, can't the conduct monitoring at all levels quality of the pharmaceutical preparations.Especially extract preparation, the not attached existence of the microscopic features of medical material, microscopical identification is felt simply helpless to it, and thin layer is differentiated to seek less than characteristic again and is detected information, with regard to the uncontrollable quality of the pharmaceutical preparations.Cause some illegal operators to use inferior materials and turn out substandard goods in the production process of medicine, take place with bad Dai You, the situation of passing a fake product off as a genuine one, the lighter affects patient's the state of an illness adversely, and weight person directly endangers patient's health.
Summary of the invention
Differentiate the detection approach for widening thin layer, the thin layer that improves in the Chinese traditional patent formulation preparation is differentiated the rate of revising and enlarging, and the inventor has carried out increasing FLUORESCENCE STUDY to the Chinese crude drug that multiple nothing detects information, and obtains ideal results.
What the invention provides a kind of Chinese crude drug increases fluoroscopic examination thin layer discrimination method, and this method comprises following steps:
A, respectively get test sample medical material and control medicinal material powder 0.01-0.5 the gram, add methanol 3-10 milliliter, supersound process 10-15 minute, get supernatant as need testing solution and reference substance solution;
B, absorption need testing solution and each 2-4 microlitre of reference substance solution are put in same GF respectively
254On the lamellae, launch, take out, dry with developing solvent;
Spray is with fluorescence-enhancing agent on c, the lamellae, and 105 ℃ to be heated to speckle colour developing clear;
D, put under the 365nm uviol lamp and inspect, the test sample chromatograph with the corresponding position of reference substance chromatograph on show the fluorescence speckle of same color.
As preferred version, the Chinese crude drug of thin layer discrimination method kind of the present invention is preferably a kind of in Venenum Bufonis, the Rhizoma Atractylodis Macrocephalae, Fructus Forsythiae, artificial Calculus Bovis, the Radix Linderae, Herba Artemisiae Scopariae, Cortex Moutan or the Rhizoma Cyperi, increases fluorescent agent and is preferably 10% ethanol solution of sulfuric acid or 1% aluminum chloride alcoholic solution.
In theory, originally do not have the Chinese crude drug of any detection information, can carry out thin layer by the method that increases fluorescence of the present invention and differentiate, the inventor is preferred especially several medical materials increase fluoroscopic examination thin layer discrimination method, as follows respectively:
1, the fluoroscopic examination thin layer discrimination method that increases of Venenum Bufonis is preferably:
A, get Venenum Bufonis medical material and Venenum Bufonis control medicinal material powder 0.05 gram respectively, add 3 milliliters of methanol, supersound process 15 minutes is got supernatant as need testing solution and reference substance solution;
B, absorption need testing solution and each 2 microlitre of reference substance solution are put in same GF respectively
254On the lamellae, the cyclohexane extraction-ethyl acetate-formic acid that with the volume ratio is 4:6:0.2 is that developing solvent launches, and takes out, and dries;
As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 10% ethanol solution of sulfuric acid in spray on c, the lamellae;
D, put under the 365nm uviol lamp and inspect, Venenum Bufonis test sample chromatograph with the corresponding position of Venenum Bufonis reference substance chromatograph on show the fluorescence speckle of same color.
2, the fluoroscopic examination thin layer discrimination method that increases of the Rhizoma Atractylodis Macrocephalae is preferably:
A, get Rhizoma Atractylodis Macrocephalae medical material and Rhizoma Atractylodis Macrocephalae control medicinal material powder 0.5 gram respectively, add 5 milliliters of methanol, supersound process 10 minutes is got supernatant as need testing solution and reference substance solution;
B, absorption need testing solution and each 4 microlitre of reference substance solution are put in same GF respectively
254On the lamellae, the cyclohexane extraction-ethyl acetate-formic acid that with the volume ratio is 8:2:0.2 is that developing solvent launches, and takes out, and dries;
As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 10% ethanol solution of sulfuric acid in spray on c, the lamellae;
D, put under the 365nm uviol lamp and inspect, Rhizoma Atractylodis Macrocephalae test sample chromatograph with the corresponding position of Rhizoma Atractylodis Macrocephalae reference substance chromatograph on show the fluorescence speckle of same color.
3, the fluoroscopic examination thin layer discrimination method that increases of Fructus Forsythiae is preferably:
A, get Fructus Forsythiae medical material and Fructus Forsythiae control medicinal material powder 0.4 gram respectively, add 5 milliliters of methanol, supersound process 10 minutes is got supernatant as need testing solution and reference substance solution;
B, absorption need testing solution and each 4 microlitre of reference substance solution are put in same GF respectively
254On the lamellae, the cyclohexane extraction-ethyl acetate-formic acid that with the volume ratio is 10:2:0.2 is that developing solvent launches, and takes out, and dries;
As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 10% ethanol solution of sulfuric acid in spray on c, the lamellae;
D, put under the 365nm uviol lamp and inspect, Fructus Forsythiae test sample chromatograph with the corresponding position of Fructus Forsythiae reference substance chromatograph on show the fluorescence speckle of same color.
4, artificial Calculus Bovis's the fluoroscopic examination thin layer discrimination method that increases is preferably:
A, get artificial Calculus Bovis's medical material and artificial Calculus Bovis's control medicinal material powder 0.15 gram respectively, add 6 milliliters of methanol, supersound process 10 minutes is got supernatant as need testing solution and reference substance solution;
B, absorption need testing solution and each 2 microlitre of reference substance solution are put in same GF respectively
254On the lamellae, the cyclohexane extraction-ethyl acetate-acetic acid-methanol that with the volume ratio is 10:25:2:3 is that developing solvent launches, and takes out, and dries;
As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 10% ethanol solution of sulfuric acid in spray on c, the lamellae;
D, put under the 365nm uviol lamp and inspect, artificial Calculus Bovis's test sample chromatograph with the corresponding position of artificial Calculus Bovis's reference substance chromatograph on show the fluorescence speckle of same color.
5, the fluoroscopic examination thin layer discrimination method that increases of the Radix Linderae is preferably:
A, get Radix Linderae medical material and Radix Linderae control medicinal material powder 0.3 gram respectively, add 4 milliliters of methanol, supersound process 10 minutes is got supernatant as need testing solution and reference substance solution;
B, absorption need testing solution and each 4 microlitre of reference substance solution are put in same GF respectively
254On the lamellae, the cyclohexane extraction-ethyl acetate-formic acid that with the volume ratio is 8:2:0.2 is that developing solvent launches, and takes out, and dries;
As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 10% ethanol solution of sulfuric acid in spray on c, the lamellae;
D, put under the 365nm uviol lamp and inspect, Radix Linderae test sample chromatograph with the corresponding position of Radix Linderae reference substance chromatograph on show the fluorescence speckle of same color.
6, the fluoroscopic examination thin layer discrimination method that increases of Herba Artemisiae Scopariae is preferably:
A, get Herba Artemisiae Scopariae medical material and Herba Artemisiae Scopariae control medicinal material powder 0.4 gram respectively, add 8 milliliters of methanol, supersound process 10 minutes is got supernatant as need testing solution and reference substance solution;
B, absorption need testing solution and each 4 microlitre of reference substance solution are put in same GF respectively
254On the lamellae, the cyclohexane extraction-ethyl acetate that with the volume ratio is 7:3 is that developing solvent launches, and takes out, and dries;
As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 10% ethanol solution of sulfuric acid in spray on c, the lamellae;
D, put under the 365nm uviol lamp and inspect, Herba Artemisiae Scopariae test sample chromatograph with the corresponding position of Herba Artemisiae Scopariae reference substance chromatograph on show the fluorescence speckle of same color.
7, the fluoroscopic examination thin layer discrimination method that increases of Cortex Moutan is preferably:
A, get Cortex Moutan medical material and Cortex Moutan control medicinal material powder 0.01 gram respectively, add 10 milliliters of methanol, supersound process 10 minutes is got supernatant as need testing solution and reference substance solution;
B, absorption need testing solution and each 3 microlitre of reference substance solution are put in same GF respectively
254On the lamellae, the cyclohexane extraction-ethyl acetate-acetone-formic acid that with the volume ratio is 8:2:1:0.2 is that developing solvent launches, and takes out, and dries;
As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 1% aluminum chloride alcoholic solution in spray on c, the lamellae;
D, put under the 365nm uviol lamp and inspect, Cortex Moutan test sample chromatograph with the corresponding position of Cortex Moutan reference substance chromatograph on show the fluorescence speckle of same color.
8, the fluoroscopic examination thin layer discrimination method that increases of Rhizoma Cyperi is preferably:
A, get Rhizoma Cyperi medical material and Rhizoma Cyperi control medicinal material powder 0.5 gram respectively, add 4 milliliters of methanol, supersound process 10 minutes is got supernatant as need testing solution and reference substance solution;
B, absorption need testing solution and each 4 microlitre of reference substance solution are put in same GF respectively
254On the lamellae, the cyclohexane extraction-ethyl acetate-formic acid that with the volume ratio is 10:2:0.2 is that developing solvent launches, and takes out, and dries;
As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 10% ethanol solution of sulfuric acid in spray on c, the lamellae;
D, put under the 365nm uviol lamp and inspect, Rhizoma Cyperi test sample chromatograph with the corresponding position of Rhizoma Cyperi reference substance chromatograph on show the fluorescence speckle of same color.
Increase the thin-layer chromatogram relative analysis of fluorescence front and back from 8 kinds of medical materials, increase before the fluorescence, no matter under 254nm or the 365nm, all not having detection information clearly presents, can't make judgement to the result, but increase after the fluorescence, the amplitude of containing much information increases, sensitivity improves, and presents 8～9 indigo plants, green fluorescence speckle as the Radix Linderae; The Rhizoma Atractylodis Macrocephalae presents 5～6 indigo plants, green fluorescence speckle; Fructus Forsythiae presents 3 Huangs and sapphirine fluorescence speckle etc., clear spot, and intensity is very high, can be used for qualitative even quantitative study, sees each thin-layer chromatogram of embodiment testing result for details.
In a word, the present invention increases fluoroscopic examination thin layer discrimination method and has sensitivity, quick, characteristics of high efficiency, solved not only do not have uv absorption, but also the discriminating problem of non-blooming medical material, make the discriminating of these medical materials can high sensitivity, carry out exactly, the thin layer that improves Chinese crude drug and Chinese traditional patent formulation preparation is differentiated the rate of revising and enlarging, and one has the use value invention very much beyond doubt.
Description of drawings
Fig. 1 Venenum Bufonis thin layer is differentiated collection of illustrative plates, A inspects photo for increasing before the fluorescence under the 254nm uviol lamp, and B inspects photo for increasing under the preceding 365nm uviol lamp of fluorescence, and C inspects photo for increasing behind the fluorescence under the 365nm uviol lamp, from left to right first three is a sample to speckle, and back three is control medicinal material.
Fig. 2 Rhizoma Atractylodis Macrocephalae thin layer is differentiated collection of illustrative plates, A inspects photo for increasing before the fluorescence under the 254nm uviol lamp, and B inspects photo for increasing under the preceding 365nm uviol lamp of fluorescence, and C inspects photo for increasing behind the fluorescence under the 365nm uviol lamp, from left to right first three is a sample to speckle, and back three is control medicinal material.
Fig. 3 Fructus Forsythiae thin layer is differentiated collection of illustrative plates, A inspects photo for increasing before the fluorescence under the 254nm uviol lamp, and B inspects photo for increasing under the preceding 365nm uviol lamp of fluorescence, and C inspects photo for increasing behind the fluorescence under the 365nm uviol lamp, from left to right first three is a sample to speckle, and back three is control medicinal material.
Fig. 4 artificial Calculus Bovis thin layer is differentiated collection of illustrative plates; A inspects photo for increasing before the fluorescence under the 254nm uviol lamp, and B inspects photo for increasing under the preceding 365nm uviol lamp of fluorescence, and C inspects photo for increasing behind the fluorescence under the 365nm uviol lamp; from left to right first three is a sample to speckle, and latter two is a control medicinal material.
Fig. 5 Radix Linderae thin layer is differentiated collection of illustrative plates, A inspects photo for increasing before the fluorescence under the 254nm uviol lamp, and B inspects photo for increasing under the preceding 365nm uviol lamp of fluorescence, and C inspects photo for increasing behind the fluorescence under the 365nm uviol lamp, from left to right first three is a sample to speckle, and latter two is a control medicinal material.
Fig. 6 Herba Artemisiae Scopariae thin layer is differentiated collection of illustrative plates, A inspects photo for increasing before the fluorescence under the 254nm uviol lamp, and B inspects photo for increasing under the preceding 365nm uviol lamp of fluorescence, and C inspects photo for increasing behind the fluorescence under the 365nm uviol lamp, from left to right first three is a sample to speckle, and latter two is a control medicinal material.
Fig. 7 Cortex Moutan thin layer is differentiated collection of illustrative plates, A inspects photo for increasing before the fluorescence under the 254nm uviol lamp, and B inspects photo for increasing under the preceding 365nm uviol lamp of fluorescence, and C inspects photo for increasing behind the fluorescence under the 365nm uviol lamp, from left to right first three is a sample to speckle, and latter two is a control medicinal material.
Fig. 8 Rhizoma Cyperi thin layer is differentiated collection of illustrative plates, A inspects photo for increasing before the fluorescence under the 254nm uviol lamp, and B inspects photo for increasing under the preceding 365nm uviol lamp of fluorescence, and C inspects photo for increasing behind the fluorescence under the 365nm uviol lamp, from left to right first three is a sample to speckle, and latter two is a control medicinal material.
The specific embodiment
Following embodiment is used to illustrate the specific embodiment of the inventive method, but it can not constitute any restriction to scope of the present invention, for confirming the technique effect of the inventive method, each embodiment is all after launching to dry with developing solvent, spray increases before the fluorescence, under 254nm and 365nm uviol lamp, inspect and take pictures, compare with chromatogram after doing to increase fluorescence.
Embodiment 1
The fluoroscopic examination thin layer that increases of Venenum Bufonis is differentiated:
A, get Venenum Bufonis medical material and Venenum Bufonis control medicinal material powder 0.05 gram respectively, add 3 milliliters of methanol, supersound process 15 minutes is got supernatant as need testing solution and reference substance solution;
B, absorption need testing solution and each 2 microlitre of reference substance solution are put in same GF respectively
254On the lamellae, the cyclohexane extraction-ethyl acetate-formic acid that with the volume ratio is 4:6:0.2 is that developing solvent launches, and takes out, and dries, and inspects under 254nm and 365nm uviol lamp respectively and takes pictures;
As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 10% ethanol solution of sulfuric acid in spray on c, the lamellae;
D, put to inspect under the 365nm uviol lamp and take pictures;
The results are shown in Figure 1, as seen increase after the fluorescence Venenum Bufonis test sample chromatograph with the corresponding position of Venenum Bufonis reference substance chromatograph on show the fluorescence speckle of 4 same colors, and do not increase in the thin layer chromatography of fluorescence, under 254nm and 365nm uviol lamp, all do not show obvious speckle.
Embodiment 2
The fluoroscopic examination thin layer that increases of the Rhizoma Atractylodis Macrocephalae is differentiated:
A, get Rhizoma Atractylodis Macrocephalae medical material and Rhizoma Atractylodis Macrocephalae control medicinal material powder 0.5 gram respectively, add 5 milliliters of methanol, supersound process 10 minutes is got supernatant as need testing solution and reference substance solution;
B, absorption need testing solution and each 4 microlitre of reference substance solution are put in same GF respectively
254On the lamellae, the cyclohexane extraction-ethyl acetate-formic acid that with the volume ratio is 8:2:0.2 is that developing solvent launches, and takes out, and dries, and inspects under 254nm and 365nm uviol lamp respectively and takes pictures;
As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 10% ethanol solution of sulfuric acid in spray on c, the lamellae;
D, put to inspect under the 365nm uviol lamp and take pictures;
The results are shown in Figure 2, as seen increase after the fluorescence Rhizoma Atractylodis Macrocephalae test sample chromatograph with the corresponding position of Venenum Bufonis reference substance chromatograph on show the fluorescence speckle of a plurality of same colors, and do not increase in the thin layer chromatography of fluorescence, under 254nm and 365nm uviol lamp, all do not show obvious speckle.
Embodiment 3
The fluoroscopic examination thin layer that increases of Fructus Forsythiae is differentiated:
A, get Fructus Forsythiae medical material and Fructus Forsythiae contrast medicine inborn ability end 0.4 gram respectively, add 5 milliliters of methanol, supersound process 10 minutes is got supernatant as need testing solution and reference substance solution;
B, absorption need testing solution and each 4 microlitre of reference substance solution are put in same GF respectively
254On the lamellae, the cyclohexane extraction-ethyl acetate-formic acid that with the volume ratio is 10:2:0.2 is that developing solvent launches, and takes out, and dries, and inspects under 254nm and 365nm uviol lamp respectively and takes pictures;
As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 10% ethanol solution of sulfuric acid in spray on c, the lamellae;
D, put to inspect under the 365nm uviol lamp and take pictures;
The results are shown in Figure 3, as seen increase after the fluorescence Fructus Forsythiae test sample chromatograph with the corresponding position of Fructus Forsythiae reference substance chromatograph on show the fluorescence speckle of 3 same colors, and do not increase in the thin layer chromatography of fluorescence, under 254nm and 365nm uviol lamp, all do not show obvious speckle.
Embodiment 4
Artificial Calculus Bovis's the fluoroscopic examination thin layer that increases is differentiated:
A, get artificial Calculus Bovis's medical material and artificial Calculus Bovis's control medicinal material powder 0.15 gram respectively, add 6 milliliters of methanol, supersound process 10 minutes is got supernatant as need testing solution and reference substance solution;
B, absorption need testing solution and each 2 microlitre of reference substance solution are put in same GF respectively
254On the lamellae, the cyclohexane extraction-ethyl acetate-acetic acid-methanol that with the volume ratio is 10:25:2:3 is that developing solvent launches, and takes out, and dries, and inspects under 254nm and 365nm uviol lamp respectively and takes pictures;
As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 10% ethanol solution of sulfuric acid in spray on c, the lamellae;
D, put to inspect under the 365nm uviol lamp and take pictures;
The results are shown in Figure 4; as seen increase artificial Calculus Bovis's test sample chromatograph after the fluorescence with the corresponding position of artificial Calculus Bovis's reference substance chromatograph on show the fluorescence speckle of 4 same colors; and do not increase in the thin layer chromatography of fluorescence, under 254nm and 365nm uviol lamp, all do not show obvious speckle.
Embodiment 5
The fluoroscopic examination thin layer that increases of the Radix Linderae is differentiated:
A, get Radix Linderae medical material and Radix Linderae control medicinal material powder 0.3 gram respectively, add 4 milliliters of methanol, supersound process 10 minutes is got supernatant as need testing solution and reference substance solution;
B, absorption need testing solution and each 4 microlitre of reference substance solution are put in same GF respectively
254On the lamellae, the cyclohexane extraction-ethyl acetate-formic acid that with the volume ratio is 8:2:0.2 is that developing solvent launches, and takes out, and dries, and inspects under 254nm and 365nm uviol lamp respectively and takes pictures;
As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 10% ethanol solution of sulfuric acid in spray on c, the lamellae;
D, put to inspect under the 365nm uviol lamp and take pictures;
The results are shown in Figure 5, as seen increase after the fluorescence Radix Linderae test sample chromatograph with the corresponding position of Radix Linderae reference substance chromatograph on show the fluorescence speckle of a plurality of same colors, and do not increase in the thin layer chromatography of fluorescence, under 254nm and 365nm uviol lamp, all do not show obvious speckle.
Embodiment 6
The fluoroscopic examination thin layer that increases of Herba Artemisiae Scopariae is differentiated:
A, get Herba Artemisiae Scopariae medical material and Herba Artemisiae Scopariae control medicinal material powder 0.4 gram respectively, add 8 milliliters of methanol, supersound process 10 minutes is got supernatant as need testing solution and reference substance solution;
B, absorption need testing solution and each 4 microlitre of reference substance solution are put in same GF respectively
254On the lamellae, the cyclohexane extraction-ethyl acetate that with the volume ratio is 7:3 is that developing solvent launches, and takes out, and dries, and inspects under 254nm and 365nm uviol lamp respectively and takes pictures;
As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 10% ethanol solution of sulfuric acid in spray on c, the lamellae;
D, put to inspect under the 365nm uviol lamp and take pictures;
The results are shown in Figure 5, as seen increase after the fluorescence Herba Artemisiae Scopariae test sample chromatograph with the corresponding position of Herba Artemisiae Scopariae reference substance chromatograph on show the fluorescence speckle of a plurality of same colors, and do not increase in the thin layer chromatography of fluorescence, under 254nm and 365nm uviol lamp, all do not show obvious speckle.
Embodiment 7
The fluoroscopic examination thin layer that increases of Cortex Moutan is differentiated:
A, get Cortex Moutan medical material and Cortex Moutan control medicinal material powder 0.01 gram respectively, add 10 milliliters of methanol, supersound process 10 minutes is got supernatant as need testing solution and reference substance solution;
B, absorption need testing solution and each 3 microlitre of reference substance solution are put in same GF respectively
254On the lamellae, the cyclohexane extraction-ethyl acetate-acetone-formic acid that with the volume ratio is 8:2:1:0.2 is that developing solvent launches, and takes out, and dries, and inspects under 254nm and 365nm uviol lamp respectively and takes pictures;
As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 1% aluminum chloride alcoholic solution in spray on c, the lamellae;
D, put to inspect under the 365nm uviol lamp and take pictures;
The results are shown in Figure 5, as seen increase after the fluorescence Cortex Moutan test sample chromatograph with the corresponding position of Cortex Moutan reference substance chromatograph on show the fluorescence speckle of 1 same color, and do not increase in the thin layer chromatography of fluorescence, under 254nm and 365nm uviol lamp, all do not show obvious speckle.
Embodiment 8
The fluoroscopic examination thin layer that increases of Rhizoma Cyperi is differentiated:
A, get Rhizoma Cyperi medical material and Rhizoma Cyperi control medicinal material powder 0.5 gram respectively, add 4 milliliters of methanol, supersound process 10 minutes is got supernatant as need testing solution and reference substance solution;
B, absorption need testing solution and each 4 microlitre of reference substance solution are put in same GF respectively
254On the lamellae, the cyclohexane extraction-ethyl acetate-formic acid that with the volume ratio is 10:2:0.2 is that developing solvent launches, and takes out, and dries, and inspects under 254nm and 365nm uviol lamp respectively and takes pictures;
As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 10% ethanol solution of sulfuric acid in spray on c, the lamellae;
D, put to inspect under the 365nm uviol lamp and take pictures;
The results are shown in Figure 5, as seen increase after the fluorescence Rhizoma Cyperi test sample chromatograph with the corresponding position of Rhizoma Cyperi reference substance chromatograph on show the fluorescence speckle of a plurality of same colors, and do not increase in the thin layer chromatography of fluorescence, under 254nm and 365nm uviol lamp, all do not show obvious speckle.
Claims (10)
- A Chinese crude drug increase the fluorescence thin layer discrimination method, it is characterized in that this method comprises following steps:A, respectively get test sample medical material and control medicinal material powder 0.01-0.5 the gram, add methanol 3-10 milliliter, supersound process 10-15 minute, get supernatant as need testing solution and reference substance solution;B, absorption need testing solution and each 2-4 microlitre of reference substance solution are put in same GF respectively 254On the lamellae, launch, take out, dry with developing solvent;Spray is with fluorescence-enhancing agent on c, the lamellae, and 105 ℃ to be heated to speckle colour developing clear;D, put under the 365nm uviol lamp and inspect, the test sample chromatograph with the corresponding position of reference substance chromatograph on show the fluorescence speckle of same color.
- 2. according to the described fluorescence thin layer discrimination method that increases of claim 1; it is characterized in that described Chinese crude drug is a kind of in Venenum Bufonis, the Rhizoma Atractylodis Macrocephalae, Fructus Forsythiae, artificial Calculus Bovis, the Radix Linderae, Herba Artemisiae Scopariae, Cortex Moutan or the Rhizoma Cyperi, the described fluorescent agent that increases is 10% ethanol solution of sulfuric acid or 1% aluminum chloride alcoholic solution.
- 3. according to the described fluorescence thin layer discrimination method that increases of claim 1-2, it is characterized in that this method comprises following steps:A, get Venenum Bufonis medical material and Venenum Bufonis control medicinal material powder 0.05 gram respectively, add 3 milliliters of methanol, supersound process 15 minutes is got supernatant as need testing solution and reference substance solution;B, absorption need testing solution and each 2 microlitre of reference substance solution are put in same GF respectively 254On the lamellae, the cyclohexane extraction-ethyl acetate-formic acid that with the volume ratio is 4:6:0.2 is that developing solvent launches, and takes out, and dries;As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 10% ethanol solution of sulfuric acid in spray on c, the lamellae;D, put under the 365nm uviol lamp and inspect, Venenum Bufonis test sample chromatograph with the corresponding position of Venenum Bufonis reference substance chromatograph on show the fluorescence speckle of same color.
- 4. according to the described fluorescence thin layer discrimination method that increases of claim 1-2, it is characterized in that this method comprises following steps:A, get Rhizoma Atractylodis Macrocephalae medical material and Rhizoma Atractylodis Macrocephalae control medicinal material powder 0.5 gram respectively, add 5 milliliters of methanol, supersound process 10 minutes is got supernatant as need testing solution and reference substance solution;B, absorption need testing solution and each 4 microlitre of reference substance solution are put in same GF respectively 254On the lamellae, the cyclohexane extraction-ethyl acetate-formic acid that with the volume ratio is 8:2:0.2 is that developing solvent launches, and takes out, and dries;As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 10% ethanol solution of sulfuric acid in spray on c, the lamellae;D, put under the 365nm uviol lamp and inspect, Rhizoma Atractylodis Macrocephalae test sample chromatograph with the corresponding position of Rhizoma Atractylodis Macrocephalae reference substance chromatograph on show the fluorescence speckle of same color.
- 5. according to the described fluorescence thin layer discrimination method that increases of claim 1-2, it is characterized in that this method comprises following steps:A, get Fructus Forsythiae medical material and Fructus Forsythiae control medicinal material powder 0.4 gram respectively, add 5 milliliters of methanol, supersound process 10 minutes is got supernatant as need testing solution and reference substance solution;B, absorption need testing solution and each 4 microlitre of reference substance solution are put in same GF respectively 254On the lamellae, the cyclohexane extraction-ethyl acetate-formic acid that with the volume ratio is 10:2:0.2 is that developing solvent launches, and takes out, and dries;As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 10% ethanol solution of sulfuric acid in spray on c, the lamellae;D, put under the 365nm uviol lamp and inspect, Fructus Forsythiae test sample chromatograph with the corresponding position of Fructus Forsythiae reference substance chromatograph on show the fluorescence speckle of same color.
- 6. according to the described fluorescence thin layer discrimination method that increases of claim 1-2, it is characterized in that this method comprises following steps:A, get artificial Calculus Bovis's medical material and artificial Calculus Bovis's control medicinal material powder 0.15 gram respectively, add 6 milliliters of methanol, supersound process 10 minutes is got supernatant as need testing solution and reference substance solution;B, absorption need testing solution and each 2 microlitre of reference substance solution are put in same GF respectively 254On the lamellae, the cyclohexane extraction-ethyl acetate-acetic acid-methanol that with the volume ratio is 10:25:2:3 is that developing solvent launches, and takes out, and dries;As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 10% ethanol solution of sulfuric acid in spray on c, the lamellae;D, put under the 365nm uviol lamp and inspect, artificial Calculus Bovis's test sample chromatograph with the corresponding position of artificial Calculus Bovis's reference substance chromatograph on show the fluorescence speckle of same color.
- 7. according to the described fluorescence thin layer discrimination method that increases of claim 1-2, it is characterized in that this method comprises following steps:A, get Radix Linderae medical material and Radix Linderae control medicinal material powder 0.3 gram respectively, add 4 milliliters of methanol, supersound process 10 minutes is got supernatant as need testing solution and reference substance solution;B, absorption need testing solution and each 4 microlitre of reference substance solution are put in same GF respectively 254On the lamellae, the cyclohexane extraction-ethyl acetate-formic acid that with the volume ratio is 8:2:0.2 is that developing solvent launches, and takes out, and dries;As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 10% ethanol solution of sulfuric acid in spray on c, the lamellae;D, put under the 365nm uviol lamp and inspect, Radix Linderae test sample chromatograph with the corresponding position of Radix Linderae reference substance chromatograph on show the fluorescence speckle of same color.
- 8. according to the described fluorescence thin layer discrimination method that increases of claim 1-2, it is characterized in that this method comprises following steps:A, get Herba Artemisiae Scopariae medical material and Herba Artemisiae Scopariae control medicinal material powder 0.4 gram respectively, add 8 milliliters of methanol, supersound process 10 minutes is got supernatant as need testing solution and reference substance solution;B, absorption need testing solution and each 4 microlitre of reference substance solution are put in same GF respectively 254On the lamellae, the cyclohexane extraction-ethyl acetate that with the volume ratio is 7:3 is that developing solvent launches, and takes out, and dries;As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 10% ethanol solution of sulfuric acid in spray on c, the lamellae;D, put under the 365nm uviol lamp and inspect, Herba Artemisiae Scopariae test sample chromatograph with the corresponding position of Herba Artemisiae Scopariae reference substance chromatograph on show the fluorescence speckle of same color.
- 9. according to the described fluorescence thin layer discrimination method that increases of claim 1-2, it is characterized in that this method comprises following steps:A, get Cortex Moutan medical material and Cortex Moutan control medicinal material powder 0.01 gram respectively, add 10 milliliters of methanol, supersound process 10 minutes is got supernatant as need testing solution and reference substance solution;B, absorption need testing solution and each 3 microlitre of reference substance solution are put in same GF respectively 254On the lamellae, the cyclohexane extraction-ethyl acetate-acetone-formic acid that with the volume ratio is 8:2:1:0.2 is that developing solvent launches, and takes out, and dries;As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 1% aluminum chloride alcoholic solution in spray on c, the lamellae;D, put under the 365nm uviol lamp and inspect, Cortex Moutan test sample chromatograph with the corresponding position of Cortex Moutan reference substance chromatograph on show the fluorescence speckle of same color.
- 10. according to the described fluorescence thin layer discrimination method that increases of claim 1-2, it is characterized in that this method comprises following steps:A, get Rhizoma Cyperi medical material and Rhizoma Cyperi control medicinal material powder 0.5 gram respectively, add 4 milliliters of methanol, supersound process 10 minutes is got supernatant as need testing solution and reference substance solution;B, absorption need testing solution and each 4 microlitre of reference substance solution are put in same GF respectively 254On the lamellae, the cyclohexane extraction-ethyl acetate-formic acid that with the volume ratio is 10:2:0.2 is that developing solvent launches, and takes out, and dries;As fluorescence-enhancing agent, 105 ℃ to be heated to speckle colour developing clear with 10% ethanol solution of sulfuric acid in spray on c, the lamellae;D, put under the 365nm uviol lamp and inspect, Rhizoma Cyperi test sample chromatograph with the corresponding position of Rhizoma Cyperi reference substance chromatograph on show the fluorescence speckle of same color.
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| CN 201110246271 Division CN102288722B (en) | 2010-11-02 | 2010-11-02 | Method for discriminating enhanced fluorescence thin layer of combined spicebush root |
| CN201110246240A Division CN102305841A (en) | 2010-11-02 | 2010-11-02 | Method for identifying enhanced fluorescent thin layer of calculus bovis factitius |
| CN201110246241A Division CN102323373A (en) | 2010-11-02 | 2010-11-02 | Fluorescence increasing thin-layer identification method for fructus forsythiae |
| CN 201110246243 Division CN102247422B (en) | 2010-11-02 | 2010-11-02 | Fluorescence thin layer identification method for bighead atractylodes rhizome |
| CN201110246268.XA Division CN102426212B (en) | 2010-11-02 | 2010-11-02 | Enhanced fluorescence thin layer identification method for Cyperus Rotundus L |
| CN2011102462444A Division CN102401821A (en) | 2010-11-02 | 2010-11-02 | Fluorescence reinforcing thin layer identification method of tree peony root-bark |
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