CN116087403B - Thin layer identification method for folium Apocyni Veneti and flos Chrysanthemi in compound herba Apocyni Veneti granule - Google Patents
Thin layer identification method for folium Apocyni Veneti and flos Chrysanthemi in compound herba Apocyni Veneti granule Download PDFInfo
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- 239000008187 granular material Substances 0.000 title claims abstract description 34
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- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 claims description 26
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- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- SOSLMHZOJATCCP-AEIZVZFYSA-N afzelin Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1OC1=C(C=2C=CC(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O SOSLMHZOJATCCP-AEIZVZFYSA-N 0.000 description 1
- 206010003549 asthenia Diseases 0.000 description 1
- 230000004531 blood pressure lowering effect Effects 0.000 description 1
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- LSYBEKRLBPCVES-UHFFFAOYSA-N ethyl acetate formic acid Chemical compound C(C)(=O)OCC.C(=O)O.C(=O)O LSYBEKRLBPCVES-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
- G01N30/94—Development
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
- G01N30/95—Detectors specially adapted therefor; Signal analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
- G01N30/94—Development
- G01N2030/945—Application of reagents to undeveloped plate
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention provides a thin-layer identification method of apocynum leaves and chrysanthemum in compound apocynum granules, and belongs to the technical field of traditional Chinese medicine detection. The thin layer identification method of the present invention includes the steps of: s1, preparing a sample solution, S2, preparing a reference medicinal material solution, S3, preparing a mixed reference solution and identifying by S4 thin layer chromatography. The invention is prepared by mixing cyclohexane, ethyl acetate and formic acid according to the volume ratio of (6-8): (4-6): (0.6-1) mixing and taking the mixture as a developing agent, spotting the developing agent on the same thin layer plate, taking an aluminum trichloride ethanol solution with the volume concentration of 1% as a color developing agent, and simultaneously identifying two medicinal flavors of dogbane leaves and chrysanthemum in the compound dogbane particles by one-time identification test, reflecting the quality information of the two medicinal flavors, having clear spots, strong specificity and good durability, being more comprehensive in identification, being more beneficial to controlling the quality of the compound dogbane particles, reducing the test times of thin layer identification, reducing the reagent consumption, saving time and improving the inspection efficiency.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine detection, in particular to a thin layer identification method of apocynum leaves and chrysanthemum in compound apocynum granules.
Background
The Chinese medicinal decoction pieces are the indispensible parts of the Chinese traditional medicine industry, are the traditional weapons necessary for the diagnosis and treatment of the Chinese traditional medicine in clinic, and the quality of the Chinese medicinal decoction pieces directly influences the curative effects of the Chinese traditional medicine in clinic on preventing and treating diseases. The compound apocynum granule is prepared by extracting three medicinal materials of apocynum leaves, hawthorns and chrysanthemums, has the effects of clearing heat, calming the liver and soothing the nerves, and is used for treating dizziness, palpitation, insomnia and the like caused by hypertension and neurasthenia. The compound apocynum granule is taken orally after being dissolved, and the product has the characteristics of accurate dosage, rapid dissolution, convenient absorption, quick effect, good taste, convenient carrying and storage, small dosage, stable property and the like. Wherein the folium Apocyni Veneti is leaf of Apocynaceae plant Apocynum Veneti, is collected in summer, is dried, and can be used for treating headache, dizziness and convulsion due to excessive liver fire, and has blood pressure lowering effect. At present, qualitative research literature on the apocynum venetum leaf formula particles is relatively lacking, and quality monitoring on the apocynum venetum leaf formula particles is difficult. The national formulary committee has shown in 2013-08-13 that "the quality standard of the variety is improved in relation to the improvement of the variety and the improvement of the drug standard of the edition of 2010 Chinese pharmacopoeia (one part)" annex 24 compound apocynum granule quality standard promulgating ", but the variety is not recorded in the edition of 2020 Chinese pharmacopoeia up to now. In the pharmacopoeia public standard of the breed 2013, the identification method of the apocynum She Baoceng comprises identification of apocynum leaf reference medicinal materials and identification of quercetin and kaempferide, the identification method of the chrysanthemum comprises identification of chrysanthemum reference medicinal materials and chlorogenic acid, and the identification method of 2 medicinal materials is 3, so that the components in the traditional Chinese medicine preparation are difficult to be identified simply and rapidly.
The Chinese patent document CN 101269158A discloses a medicinal composition for treating hypertension, a preparation method and a detection method, wherein the medicinal composition comprises the following raw material medicaments: apocynum venetum, prunellae Spica, ramulus Uncariae cum Uncis, alismatis rhizoma, concha Margaritifera, achyranthis radix, fructus crataegi and flos Chrysanthemi. The invention controls the quality of products by identifying selfheal and apocynum venetum, which is characterized in that 10 mu l of sample solution and 5 mu l of reference medicinal solution are sucked and respectively put on the same silica gel G thin layer plate, chloroform, methanol, water and formic acid are used as developing agents according to the volume ratio of 9:2.5:0.1:0.2, and the developing agents are developed, taken out, dried in the air, sprayed with 2% aluminum trichloride ethanol solution and heated at 100 ℃ for 10 minutes; spots of the same color appear on the chromatogram of the test sample at positions corresponding to those of the chromatogram of the control drug. The Chinese patent document CN 101669977A discloses a quality detection method of a dogbane leaf capsule, and the adopted thin-layer chromatography identification conditions are as follows: sucking 5ul of each of the test solution and the control medicinal solution, respectively spotting on the same silica gel thin layer plate, and using chloroform: methanol: water: formic acid=9: 2.5:0.1:0.2 The solution with the volume ratio is used as developing agent, developed, taken out, dried, sprayed with 1% aluminum trichloride ethanol solution, and inspected under 365nm ultraviolet lamp, wherein fluorescent spots with the same color appear on the positions corresponding to the control medicine chromatogram in the sample chromatogram. In the prior art, the thin-layer chromatography identification methods of the compound apocynum venetum particles all adopt single traditional Chinese medicine components for identification, and a plurality of traditional Chinese medicine components in the compound apocynum venetum particles are difficult to identify simultaneously by adopting the same method, so that a rapid and simple method for identifying a plurality of traditional Chinese medicine components in the compound apocynum venetum particles is established, and the method has important significance for comprehensively and scientifically identifying the quality of the compound apocynum venetum particles.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a thin layer identification method for folium apocyni veneti and chrysanthemum in compound herba apocyni veneti particles, which has clear spots, strong specificity and good durability; the quality information of the two medicinal apocynum venetum leaves and the chrysanthemum can be reflected by one identification test, the identification is more comprehensive, the quality of the compound apocynum venetum particles can be controlled more easily, the test times of thin-layer identification are reduced, the reagent consumption is reduced, the time is saved, and the inspection efficiency is improved.
In order to achieve the above purpose, the invention provides a thin layer identification method of apocynum venetum leaves and chrysanthemum in compound apocynum venetum particles, which comprises the following steps:
s1, preparing a sample solution: weighing compound herba Apocyni Veneti granule, grinding, adding dilute hydrochloric acid and ethyl acetate, ultrasonic treating, filtering, evaporating filtrate, and dissolving residue with methanol to obtain test solution;
s2, preparing a control medicinal material solution: weighing folium Apocyni Veneti control medicinal material and flos Chrysanthemi control medicinal material, heating respectively, filtering, evaporating filtrate, adding dilute hydrochloric acid and ethyl acetate respectively, performing ultrasonic treatment, filtering, evaporating filtrate, and dissolving residue with methanol to obtain folium Apocyni Veneti control medicinal material solution and flos Chrysanthemi control medicinal material solution;
s3, preparing a mixed reference substance solution: weighing quercetin reference substance and kaempferide reference substance, adding ethanol, and mixing to obtain quercetin and kaempferide mixed reference substance solution;
s4, identifying by thin layer chromatography: the sample solution, the reference medicinal material solution and the reference substance solution are sucked and respectively spotted on a thin layer plate, a developing agent is added, the thin layer plate is developed, taken out and dried, the developing agent is sprayed, and the thin layer plate is heated until spots develop clearly, and is inspected, wherein spots or fluorescent spots with the same color appear on the positions corresponding to the quercetin, the kaempferide reference substance chromatograph and the apocynum venetum leaf reference medicinal material chromatograph in the sample chromatograph, and fluorescent spots with the same color appear on the positions corresponding to the chrysanthemum reference medicinal material chromatograph.
Further, the compound apocynum granules are sucrose-free compound apocynum granules.
Further, in the step S1, 2.5g of compound apocynum venetum particles are weighed, ground, added with 1ml of dilute hydrochloric acid and 25ml of ethyl acetate, subjected to ultrasonic treatment for 30 minutes, filtered, evaporated to dryness, and added with 1ml of methanol to dissolve residues to serve as a test solution.
Further, in the step S2, 1g of each of the apocynum leaf reference medicinal material and the chrysanthemum reference medicinal material is weighed, 25ml of water is respectively added for ultrasonic treatment for 30 minutes, filtration is carried out, 1ml of diluted hydrochloric acid and 25ml of ethyl acetate are respectively added after the filtrate is evaporated to dryness, ultrasonic treatment is carried out for 30 minutes, filtration is carried out, the filtrate is evaporated to dryness, and 1ml of methanol is added into residues to dissolve the residues to be respectively used as an apocynum leaf reference medicinal material solution and a chrysanthemum reference medicinal material solution.
Further, the concentration of the mixed reference substance solution in the step S3 is 0.5mg of quercetin and kaempferide per 1 ml.
Further, the amount of the sample solution sucked in the step S4 is 5-10. Mu.l, the amount of the reference medicinal material solution is 5. Mu.l, and the amount of the reference medicinal material solution is 3. Mu.l.
Furthermore, the thin layer plates are the same silica gel G thin layer plate.
Further, the color developing agent is an aluminum trichloride ethanol solution with the volume concentration of 1%.
Further, the developing agent in the step S4 is prepared from cyclohexane, ethyl acetate and formic acid according to the volume ratio (6-8): (4-6): (0.6-1) and mixing.
Further, the developing agent is prepared from cyclohexane, ethyl acetate and formic acid according to a volume ratio of 7:5: 0.8.
Further, the inspection in the step S4 is performed under sunlight and 365nm ultraviolet light, respectively.
Compared with the prior art, the invention has the beneficial effects that: the thin-layer identification method of the apocynum venetum leaves and the chrysanthemum in the compound apocynum venetum particles provided by the invention has clear spots, strong specificity and good durability, is not influenced by thin-layer plate manufacturers, temperature, relative humidity and the like, can reflect the quality information of the two medicinal apocynum venetum leaves and the chrysanthemum through one-time identification test no matter under sunlight or 365nm ultraviolet light, is more comprehensive in identification, is more beneficial to controlling the quality of the compound apocynum venetum particles, reduces the test times of thin-layer identification, reduces the reagent consumption, saves time and improves the inspection efficiency.
Drawings
FIG. 1 is a thin layer chromatogram of example 1;
FIG. 2 is a thin layer chromatogram of example 2;
FIG. 3 is a thin layer chromatogram of example 3;
FIG. 4 is a thin layer chromatogram obtained by thin layer identification using Merk silica gel G plate as thin layer plate in different thin layer plate examinations;
FIG. 5 is a thin layer chromatogram obtained by thin layer identification using a tabacco silver dragon silica gel HSG plate as a thin layer plate in different thin layer plate surveys;
FIG. 6 is a thin layer chromatogram at a relative humidity of 23% for different relative humidity studies;
FIG. 7 is a thin layer chromatogram at a relative humidity of 60% for different relative humidity studies;
FIG. 8 is a thin layer chromatogram at 90% relative humidity for different relative humidity studies;
FIG. 9 is a thin layer chromatogram at a temperature of 3.8℃under different temperature studies;
FIG. 10 is a thin layer chromatogram at 20.2℃under different temperature studies;
FIG. 11 is a thin layer chromatogram at a temperature of 30℃under different temperature studies;
FIG. 12 is a thin layer chromatogram of comparative example 1;
fig. 13 is a thin layer chromatogram of comparative example 2.
Detailed Description
The experimental methods of the present invention, in which specific conditions are not specified in the following examples, are generally conducted under conventional conditions or under conditions recommended by the manufacturer. The various chemicals commonly used in the examples are commercially available. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The present invention will be further described in detail with reference to the following embodiments, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the description is only illustrative and is not intended to limit the scope of the invention. In addition, in the following description, descriptions of well-known structures and techniques are omitted so as not to unnecessarily obscure the present invention.
Example 1 identification of Apocynum venetum leaf and Chrysanthemum in thin layer of Compound Apocynum venetum particles of the invention
S1, preparing a sample solution: weighing 2.5g of compound apocynum granules (without sucrose), grinding, adding 1ml of dilute hydrochloric acid and 25ml of ethyl acetate, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, adding 1ml of methanol into residues to dissolve, and repeating the operation for 3 times to prepare 3 batches of compound apocynum granules as test solutions, wherein the numbers are respectively: KC220905, KC220906, KC221004;
s2, preparing a control medicinal material solution: weighing 1g of each of a dogbane leaf control medicinal material and a chrysanthemum control medicinal material, respectively heating 25ml of water, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, respectively adding 1ml of dilute hydrochloric acid and 25ml of ethyl acetate, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, and adding 1ml of methanol into residues to dissolve the residues to obtain a dogbane leaf control medicinal material solution and a chrysanthemum control medicinal material solution respectively;
s3, preparing a mixed reference substance solution: weighing quercetin reference substance and kaempferide reference substance, adding ethanol to obtain mixed solution containing 0.5mg of quercetin and kaempferide per 1ml, and taking the mixed solution as quercetin and kaempferide mixed reference substance solution;
s4, identifying by thin layer chromatography: sucking 5-10 mu l of 3 batches of compound apocynum venetum particle test solution, 5 mu l of control medicinal material solution and 3 mu l of control medicinal material solution, respectively spotting on the same silica gel G thin layer plate, and mixing with cyclohexane, ethyl acetate and formic acid according to a volume ratio of 7:5:0.8 is developing agent, developing, taking out, airing, spraying aluminum trichloride ethanol solution with volume concentration of 1%, heating at 105 ℃ until the color of spots is clear, respectively inspecting under sunlight and 365nm ultraviolet light, wherein the obtained thin-layer chromatogram is shown in figure 1, the left image of figure 1 is a thin-layer chromatogram inspected under ultraviolet light, the right image of figure 1 is a thin-layer chromatogram inspected under sunlight, and 3 batches of compound apocynum granules sample chromates display spots or fluorescent spots with the same color on the positions corresponding to quercetin, kaempferide reference sample chromates and apocynum leaf reference medicinal material chromates, and the apocynum She Yinxing granules and blank granules have no interference; the 3 batches of the test sample chromatogram of the compound apocynum venetum particles show fluorescence spots with the same color on the corresponding positions of the chrysanthemum control medicine chromatogram, and the chrysanthemum negative particles and the blank particles have no interference.
Example 2 method for identifying Apocynum venetum leaf and Chrysanthemum in Compound Apocynum venetum particles in the invention
S1, preparing a sample solution: weighing 2.5g of compound apocynum granules (without sucrose), grinding, adding 1ml of dilute hydrochloric acid and 25ml of ethyl acetate, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, adding 1ml of methanol into residues to dissolve, and repeating the operation for 6 times to prepare 6 batches of compound apocynum granules as test solutions, wherein the numbers are respectively: KC220907, KC220908, KC220909, KC220910, KC220911, KC220912;
s2, preparing a control medicinal material solution: weighing 1g of each of a dogbane leaf control medicinal material and a chrysanthemum control medicinal material, respectively heating 25ml of water, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, respectively adding 1ml of dilute hydrochloric acid and 25ml of ethyl acetate, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, and adding 1ml of methanol into residues to dissolve the residues to obtain a dogbane leaf control medicinal material solution and a chrysanthemum control medicinal material solution respectively;
s3, preparing a mixed reference substance solution: adding ethanol into quercetin reference substance and kaempferide reference substance to obtain mixed solution containing 0.5mg of quercetin and kaempferide per 1ml, and taking the mixed solution as quercetin and kaempferide mixed reference substance solution;
s4, identifying by thin layer chromatography: sucking 5-10 mu l of each of 6 batches of test solution, 5 mu l of each of control medicinal solution and 3 mu l of each of control solution, respectively spotting on the same silica gel G thin layer plate, and mixing cyclohexane and ethyl acetate formic acid according to a volume ratio of 7:5:0.8 is developing agent, developing, taking out, airing, spraying aluminum trichloride ethanol solution with volume concentration of 1%, heating at 105 ℃ until the color of spots is clear, respectively inspecting under sunlight and 365nm ultraviolet light, wherein the obtained thin-layer chromatogram is shown in figure 2, the left image of figure 2 is a thin-layer chromatogram inspected under ultraviolet light, the right image of figure 2 is a thin-layer chromatogram inspected under sunlight, and the color spectrum of 6 batches of compound apocynum granules to be tested is on the corresponding positions of quercetin, kaempferide reference color spectrum and apocynum leaf reference color spectrum, spots or fluorescent spots with the same color are displayed on the positions corresponding to the quercetin, kaempferide reference color spectrum and apocynum leaf reference color spectrum, and the apocynum She Yinxing granules and blank granules are free from interference; the color spectrum of the 6 batches of compound apocynum venetum particles to be tested shows fluorescent spots with the same color on the position corresponding to the color spectrum of the chrysanthemum control medicinal material, and the chrysanthemum negative particles and the blank particles have no interference.
Example 3 identification of Apocynum venetum leaf and Chrysanthemum in thin layer of Compound Apocynum venetum particles of the invention
S1, preparing a sample solution: weighing 2.5g of compound apocynum granules (without sucrose), grinding, adding 1ml of dilute hydrochloric acid and 25ml of ethyl acetate, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, adding 1ml of methanol into residues to dissolve, and repeating the operation for 6 times to prepare 6 batches of compound apocynum granules as test solutions, wherein the numbers are respectively: KC221001, KC221002, KC221003, KC221005, KC221006, KC221007;
s2, preparing a control medicinal material solution: weighing 1g of each of a dogbane leaf control medicinal material and a chrysanthemum control medicinal material, respectively heating 25ml of water, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, respectively adding 1ml of dilute hydrochloric acid and 25ml of ethyl acetate, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, and adding 1ml of methanol into residues to dissolve the residues to obtain a dogbane leaf control medicinal material solution and a chrysanthemum control medicinal material solution respectively;
s3, preparing a mixed reference substance solution: weighing quercetin reference substance and kaempferide reference substance, adding ethanol to obtain mixed solution containing 0.5mg of quercetin and kaempferide per 1ml, and taking the mixed solution as quercetin and kaempferide mixed reference substance solution;
s4, identifying by thin layer chromatography: sucking 5-10 mu l of each of 6 batches of test solution, 5 mu l of each of control medicinal solution and 3 mu l of each of control solution, respectively spotting on the same silica gel G thin layer plate, and mixing cyclohexane, ethyl acetate and formic acid according to a volume ratio of 7:5:0.8 is developing agent, developing, taking out, airing, spraying aluminum trichloride ethanol solution with volume concentration of 1%, heating at 105 ℃ until the color of spots is clear, respectively inspecting under sunlight and 365nm ultraviolet light, wherein the obtained thin-layer chromatogram is shown in figure 3, the left image of figure 3 is a thin-layer chromatogram inspected under ultraviolet light, the right image of figure 3 is a thin-layer chromatogram inspected under sunlight, and the color spectrum of 6 batches of compound apocynum granules to be tested is on the corresponding positions of quercetin, kaempferide reference color spectrum and apocynum leaf reference color spectrum, spots or fluorescent spots with the same color are displayed, and the apocynum She Yinxing granules and blank granules are free of interference; the color spectrum of the 6 batches of compound apocynum venetum particles to be tested shows fluorescent spots with the same color on the position corresponding to the color spectrum of the chrysanthemum control medicinal material, and the chrysanthemum negative particles and the blank particles have no interference.
Comparative example 1
S1, preparing a sample solution: weighing 5g of compound apocynum granules (without sucrose), grinding, adding 100ml of ethyl acetate, heating and refluxing for 1 hour, filtering, placing the filtrate in a separating funnel, washing with water for 2 times, each time 15ml, discarding washing liquid, adding 5g of anhydrous sodium sulfate into an ethyl acetate layer for dehydration, standing, filtering, evaporating the filtrate, adding 1ml of methanol into residues for dissolution, and repeating the operation for 3 times to obtain 3 batches of compound apocynum granule solutions with the numbers of KC220601, KC220701 and KC220702;
s2, preparing a control medicinal material solution: weighing folium Apocyni Veneti reference material 1g, adding ethyl acetate 20ml, refluxing under heating for 1 hr, filtering, evaporating filtrate to dryness, and dissolving residue in methanol 1ml to obtain reference material solution;
s3, preparing a control medicinal material solution by a water extraction method: taking 0.5g of apocynum leaf reference medicine, adding 25ml of water, heating and refluxing for 1 hour, cooling, filtering, shaking and extracting for 2 times with 20ml of ethyl acetate each time, combining ethyl acetate liquid, evaporating to dryness, and adding 1ml of methanol into residues to dissolve the residues to obtain apocynum leaf reference medicine (water extraction);
s4, detecting by thin layer chromatography: sucking 5-10ul of each of the 3 batches of test sample solutions, respectively dispensing 10ul of control medicinal material solutions on the same silica gel G thin layer plate, and mixing chloroform, methanol, water and formic acid according to a volume ratio of 9:2.5:0.1:0.2 is mixed as developing agent, developed, taken out, dried, sprayed with aluminum trichloride ethanol solution with volume concentration of 1%, heated for several minutes at 105 ℃, inspected under 365nm ultraviolet lamp, and the obtained thin layer chromatogram is shown in figure 12, wherein fluorescent spots with the same color appear on the corresponding position of the chromatogram of the reference medicinal material in the chromatogram of the sample to be tested, but the blank particles of the apocynum venetum leaves have negative interference, and the correspondence between the reference medicinal material and the sample is slightly poorer.
Comparative example 2
S1, preparing a sample solution: weighing 5g of compound apocynum granules (without sucrose), grinding, adding 2ml of dilute hydrochloric acid and 50ml of ethyl acetate, performing ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, and adding 2ml of methanol into residues to dissolve, wherein the residues are used as a sample solution, and the number is KC220703;
s2, preparing a control medicinal material solution: taking 1g of chrysanthemum control medicinal material, adding 1ml of dilute hydrochloric acid and 50ml of ethyl acetate, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, and adding 2ml of methanol into residues to dissolve the residues to obtain a control medicinal material solution;
s3, preparing a reference substance solution: adding methanol into chlorogenic acid reference substance to obtain solution containing 0.5mg per 1ml, and taking the solution as reference substance solution;
s4, carrying out thin layer chromatography test: sucking 0.5-1ul of the sample solution, the reference substance and the reference medicinal material solution respectively, and respectively dispensing the sample solution, the reference substance solution and the reference medicinal material solution on the same polyamide film, wherein toluene, ethyl acetate, formic acid, glacial acetic acid and water are used according to the volume ratio of 1:15:1:1:2, developing, taking out, airing, and inspecting under 365nm ultraviolet light, wherein the obtained thin layer chromatogram is shown in figure 13, and fluorescent spots with the same color appear on the positions corresponding to the control medicine chromatogram and the control medicine chromatogram in the test sample chromatogram, but the chrysanthemum control medicine and the compound apocynum venetum particles have poor correspondence, negative interference and chlorogenic acid control sample also have negative interference.
Test example: methodology investigation
1. Investigation of specificity
In the embodiment 1-3 of the invention, the thin-layer chromatogram of 15 batches of test samples of the compound apocynum venetum particles is identified by referring to the figure 1-3, the chromatogram of the test samples of the 15 batches of compound apocynum venetum particles shows spots or fluorescent spots with the same color at the positions corresponding to the chromatograms of quercetin, kaempferide reference substances and apocynum venetum leaf reference substances, and the She Yinxing particles of apocynum venetum and blank particles have no interference no matter whether the chromatogram is sunlight or 365nm ultraviolet light; the 15 batches of the test sample chromatogram of the compound apocynum venetum particles show fluorescent spots with the same color on the corresponding positions of the chromatogram of the chrysanthemum control medicinal material, and the chrysanthemum negative particles and the blank particles have no interference and clear spots, so that the thin-layer method has good specificity and can simultaneously identify the apocynum venetum leaves and the chrysanthemum in the compound apocynum venetum particles; while comparative examples 1-2 were subjected to thin-layer chromatography identification according to the standard disclosed in the "chinese pharmacopoeia" in 2013, the thin-layer chromatography is shown in fig. 12-13, and it is found that the identification of the reference apocynum venetum leaf as a reference medicine has negative interference, the specificity is poor, the identification of the chrysanthemum as a reference medicine as well as chlorogenic acid has negative interference, the specificity is poor, and the disclosed standard is difficult to accurately identify the components of the compound apocynum venetum particles (without sucrose).
2. Durability inspection
(1) Inspection of different lamina plates
Carrying out thin layer identification on 3 batches of compound apocynum venetum particle sample solutions KC220905, KC220906 and KC221004 obtained in the embodiment 1 by using silicon G thin layer plates of different manufacturers at the same temperature of 20.8 ℃ and the same relative humidity of 33%, wherein the obtained thin layer chromatograms refer to fig. 4-5, fig. 4 is a Merk silica gel G plate as the thin layer plate, fig. 5 is a smoke table silver dragon silica gel HSG plate as the thin layer plate, the left graph in fig. 4 and 5 is a thin layer chromatograms obtained under ultraviolet light, the right graph is a thin layer chromatograms obtained under sunlight, and the 3 batches of compound apocynum venetum particle sample chromates show spots or fluorescence spots with the same color at positions corresponding to quercetin, kaempferin reference sample chromates and apocynum venetum leaf reference medicinal material chromates under the sunlight or 365nm ultraviolet light, and apocynum venetum She Yinxing particles and blank particles have no interference; the 3 batches of the test sample chromatogram of the apocynum venetum particles show fluorescent spots with the same color on the corresponding positions of the chromatogram of the chrysanthemum control medicinal material, and the chrysanthemum negative particles and the blank particles have no interference, clear and bright spots and no obvious change, so that the thin layer identification method provided by the invention is suitable for the silica gel G thin layer plates of different manufacturers and has good durability.
(2) Investigation of different relative humidity
Carrying out thin-layer identification on 3 batches of compound apocynum venetum particle sample solutions KC220905, KC220906 and KC221004 obtained in the embodiment 1 at the same temperature of 5.6 ℃ and different relative humidity of 23%, 60% and 90%, wherein a thin-layer plate is a Merk silica gel G plate, the obtained thin-layer chromatograms refer to fig. 6-8, the relative humidity of 23% is shown in fig. 6, the relative humidity of 60% is shown in fig. 7, the relative humidity of 90% is shown in fig. 6, 7 and 8, the left graph is a thin-layer chromatograms obtained under ultraviolet light, and the right graph is a thin-layer chromatograms obtained under sunlight, and the 3 batches of compound apocynum venetum particle sample chromates show spots or fluorescence spots with the same color at positions corresponding to the chromatograms of quercetin, the kaempferide control sample and the apocynum venetum leaf control sample, and the apocynum She Yinxing particles and blank particles are free from interference; the color spectrum of the 3 batches of the test sample of the compound apocynum venetum particles shows fluorescent spots with the same color on the corresponding position of the color spectrum of the chrysanthemum control medicinal material, and the chrysanthemum negative particles and the blank particles have no interference, clear and bright spots and no obvious influence, so that the thin-layer identification method has good durability on different relative humidity.
(3) Investigation of different temperatures
The test solutions KC220905, KC220906 and KC221004 of 3 batches of compound apocynum venetum particles obtained in example 1 are subjected to thin-layer identification of leaves and chrysanthemum at the same relative humidity of 32%, different temperatures of 3.8 ℃, 20.2 ℃ and 30 ℃, the thin-layer plate is a Merk silica gel G plate, the obtained thin-layer chromatograms are shown in figures 9-11, the temperature of figure 9 is 3.8 ℃, the temperature of figure 10 is 20.2 ℃ and the temperature of figure 11 is 30 ℃, the left graph in fig. 9, 10 and 11 shows a thin-layer chromatogram obtained under ultraviolet light, the right graph shows a thin-layer chromatogram obtained under sunlight, and no matter under sunlight or 365nm ultraviolet light, the 3 batches of compound apocynum venetum particle sample chromatograms show spots or fluorescence spots with the same color at positions corresponding to quercetin, kaempferide control chromatograms and apocynum venetum leaf control chromatograms, and apocynum venetum She Yinxing particles and blank particles have no interference; the 3 batches of the test sample chromatogram of the apocynum venetum particles show fluorescent spots with the same color on the corresponding positions of the chromatogram of the chrysanthemum control medicinal material, and the chrysanthemum negative particles and the blank particles have no interference spots, are clear and bright and have no obvious influence, so that the thin-layer identification method disclosed by the invention has good durability on different temperatures.
The foregoing examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (7)
1. A thin layer identification method of apocynum leaves and chrysanthemum in compound apocynum granules is characterized by comprising the following steps:
s1, preparing a sample solution: weighing compound herba Apocyni Veneti granule, grinding, adding dilute hydrochloric acid and ethyl acetate, ultrasonic treating, filtering, evaporating filtrate, and dissolving residue with methanol to obtain test solution;
s2, preparing a control medicinal material solution: weighing folium Apocyni Veneti control medicinal material and flos Chrysanthemi control medicinal material, heating respectively, filtering, evaporating filtrate, adding dilute hydrochloric acid and ethyl acetate respectively, performing ultrasonic treatment, filtering, evaporating filtrate, and dissolving residue with methanol to obtain folium Apocyni Veneti control medicinal material solution and flos Chrysanthemi control medicinal material solution;
s3, preparing a mixed reference substance solution: weighing quercetin reference substance and kaempferide reference substance, adding ethanol, and mixing to obtain quercetin and kaempferide mixed reference substance solution;
s4, identifying by thin layer chromatography: drawing the sample solution, the reference medicinal material solution and the reference substance solution, respectively dotting on a thin layer plate, adding a developing agent, developing, taking out, airing, spraying a developing agent, heating until spots develop clearly, and inspecting, wherein spots or fluorescent spots with the same color appear on the positions corresponding to the quercetin, kaempferide reference substance chromatogram and apocynum venetum leaf reference medicinal material chromatogram in the sample chromatogram, and fluorescent spots with the same color appear on the positions corresponding to the chrysanthemum reference medicinal material chromatogram;
the thin layer plates are the same silica gel G thin layer plate;
the developing agent is prepared from cyclohexane, ethyl acetate and formic acid according to a volume ratio of 7:5: 0.8.
2. The method for identifying the leaves and the chrysanthemums of the compound apocynum granules by using the thin layer according to claim 1, wherein in the step S1, 2.5g of the compound apocynum granules are weighed, ground, added with 1ml of diluted hydrochloric acid and 25ml of ethyl acetate, subjected to ultrasonic treatment for 30 minutes, filtered, evaporated to dryness, and added with 1ml of methanol to dissolve residues to serve as a test solution.
3. The method for identifying herba Apocyni Veneti leaf and flos Chrysanthemi in compound herba Apocyni Veneti granule according to claim 1, wherein in step S2, 1g each of herba Apocyni Veneti leaf control medicinal material and flos Chrysanthemi control medicinal material is weighed, 25ml of water is respectively added for 30 minutes, the solution is filtered, 1ml of diluted hydrochloric acid and 25ml of ethyl acetate are respectively added after the filtrate is evaporated to dryness, the solution is treated for 30 minutes by ultrasound, the filtrate is filtered, and 1ml of methanol is added to residues to dissolve the solution respectively as herba Apocyni Veneti leaf control medicinal material solution and flos Chrysanthemi control medicinal material solution.
4. The thin-layer identification method of apocynum venetum leaves and chrysanthemum in compound apocynum venetum particles according to claim 1, wherein the concentration of the mixed reference substance solution in the step S3 is 0.5mg of quercetin and kaempferide per 1 ml.
5. The thin-layer identification method of apocynum venetum leaves and chrysanthemum in compound apocynum venetum particles according to claim 1, wherein the amount of the sample solution sucked in the step S4 is 5-10 μl, the amount of the reference medicinal material solution is 5 μl, and the amount of the reference solution is 3 μl.
6. The thin layer identification method of dogbane leaf and chrysanthemum in compound dogbane granule as claimed in claim 1, wherein the color developing agent is 1% volume concentration aluminium trichloride ethanol solution.
7. The method for identifying the thin layers of the apocynum venetum leaves and the chrysanthemum in the compound apocynum venetum particles according to claim 1, wherein the inspection in the step S4 is performed under sunlight and 365nm ultraviolet light respectively.
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