CN111024880B - Rapid multi-information thin-layer identification method for wintersweet flower medicinal materials, particles and target decoction dry powder - Google Patents
Rapid multi-information thin-layer identification method for wintersweet flower medicinal materials, particles and target decoction dry powder Download PDFInfo
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Abstract
The invention relates to a rapid multi-information thin-layer identification method for wintersweet flower medicinal materials, particles and standard decoction dry powder. The method is characterized in that: a test sample and a medicinal material solution are obtained by a simple and quick pretreatment method, and are respectively spotted on the same thin-layer plate, and after the thin-layer plate is unfolded, 7 information spots of wintersweet flower medicinal materials, particles and standard decoction dry powder are inspected under 3 different inspection conditions. The fluorescent spot not only shows fluorescence, but also has no fluorescence, and the fluorescence of the spot is excited and enhanced when the fluorescent spot meets 10% sulfuric acid ethanol solution, and the fluorescent spot are mutually staggered but do not interfere with each other, so that the information spot complementation under different inspection conditions is exerted. Compared with the conventional thin-layer identification, the quality controllability of the identified object is greatly improved, the quality supervision is facilitated, and the method is simple, convenient and quick, has high efficiency and low cost and does not pollute the environment.
Description
Technical Field
The invention relates to a rapid multi-information thin-layer identification method for wintersweet flower medicinal materials, particles and standard decoction dry powder. Belongs to the field of thin-layer identification of traditional Chinese medicines. Namely, thin-layer chromatography is adopted for identification, and 7 information spots of wintersweet flower medicinal materials, particles and standard decoction dry powder are detected on the same thin-layer plate under 3 different detection conditions.
Background
The so-called rapid multi-information thin-layer identification method is simple, convenient, rapid and efficient as the name implies, the sample solution and the reference medicinal material solution do not need repeated purification treatment, no operation procedures such as evaporation, concentration and the like polluting the environment, after ultrasonic treatment by using a proper solvent, filtration is not needed, the sample application, the development and the inspection of the supernatant are carried out, and the thin-layer result can be obtained quickly. The multi-information refers to a thin layer plate which is unfolded for 1 time, and various information spots under different inspection conditions can be obtained. Compared with the conventional thin-layer identification, the quality controllability of the detected object is greatly improved, the market quality supervision is facilitated, and the safety and the effectiveness of the drug use of people are ensured.
Wintersweet flower is a kind of wintersweet plant. The dry flower bud of wintersweet, also known as snowflake, usually blooms in the middle of 11 months until about 3 months of the next year, with a very long flowering phase. Chimonanthus praecox has warm property and sweet and slightly bitter taste. Ben Cao gang mu Yun can relieve summer-heat and promote the production of body fluid. The main functional indications are as follows: relieving summer-heat and promoting the production of body fluid. It is indicated for feverish sensation with thirst, chest distress, cough, and fire injury due to decoction. Compendium (compendium): relieve summer-heat and promote the production of body fluid. Zhejiang Chinese medicine handbook: it is indicated for summer-heat, chest stuffiness, polydipsia, infantile measles and pertussis. Jiangsu Zhizhizizhi: it is indicated for restlessness, thirst, qi stagnation and stomach stuffiness. Modern researches show that the wintersweet contains various volatile oils, prunetin, wintersweet glycoside and beta-carotene. However, the Chinese pharmacopoeia has not been brought in, so that no report is made on the legal quality standard of the Chinese pharmacopoeia. Only consult one【1】The identification of plum blossom and wintersweet flower includes the microscopic identification and the thin-layer identification of two medicinal materials. Because the thin-layer map is a plurality of spots drawn manually, the interference condition of the thin-layer background cannot be confirmed, and the color and the definition of each spot cannot be known. The thin-layer identification of wintersweet flower medicinal materials, water-decocted particles and standard decoction dry powder can be carried out quickly and simultaneously by multiple information is not reported.
The method provides scientific basis for the rapid multi-information control of the quality of wintersweet flower medicinal materials, particles and target decoction dry powder and the preparation process thereof, and carries out special thin-layer identification research on the wintersweet flower medicinal materials, the particles and the target decoction dry powder based on the purposes of simplicity, rapidness, low cost, high efficiency and multi-information. A set of convenient, fast and environment-friendly rapid multi-information thin-layer identification method for wintersweet flower medicinal materials, particles and standard decoction dry powder is obtained. The preparation process of wintersweet flower medicinal materials, particles and standard decoction dry powder is described as follows:
the wintersweet flower medicinal material is prepared by removing impurities from collected wintersweet flowers, quickly cleaning and drying.
The wintersweet flower granule is prepared by decocting wintersweet flower medicinal materials with water for 2 times, wherein each time lasts for 1-2 hours, filtering, combining filtrates, concentrating under reduced pressure to an appropriate relative density, spray drying, adding an appropriate amount of dextrin into dry powder, mixing uniformly, and granulating.
The dried powder of Chimonanthus praecox decoction is prepared by decocting Chimonanthus praecox with water for 2 times (each time for 1 hr), filtering, mixing filtrates, concentrating at room temperature to appropriate relative density, oven drying at 60 deg.C, and pulverizing.
Disclosure of Invention
The rapid multi-information thin-layer identification method for wintersweet flower medicinal materials, particles and standard decoction dry powder is created for the first time. Namely, a test sample and a medicinal material solution are obtained by a simple and rapid pretreatment method, and are respectively spotted on the same thin-layer plate, and after the thin-layer plate is unfolded, 7 information spots of wintersweet flower medicinal materials, particles and standard decoction dry powder are inspected under 3 different inspection conditions. The fluorescence is present and not present, the fluorescence is excited and enhanced when the fluorescence meets 10 percent sulfuric acid ethanol solution, and the fluorescence is staggered but not interfered with each other, so that the information spot complementation under different inspection conditions is exerted. Compared with the conventional thin-layer identification, the quality controllability of the identified object is greatly improved, the quality supervision is facilitated, and the method is simple, convenient and quick, has high efficiency and low cost and does not pollute the environment.
The technical scheme adopted by the invention for solving the technical problems is as follows:
taking wintersweet flower particles and wintersweet flower standard decoction dry powder 0.5g respectively, adding 3ml of methanol, performing ultrasonic treatment for 10 minutes, centrifuging, and taking supernate as a test solution; taking 0.2g of wintersweet flower medicinal material powder, adding 2ml of methanol, carrying out ultrasonic treatment for 15 minutes, centrifuging, and taking supernate as a medicinal material solution; sucking 4 μ l of the test solution, 4 μ l of the dry powder of the standard decoction, and 5 μ l of the medicinal solution, and respectively dropping on the same silica gel GF254On the thin layer plate, cyclohexane-ethyl acetate-methanol-formic acid-water with the volume ratio of 6: 4: 2: 0.1Developing the sample as developing agent, taking out, drying with hot air, and inspecting under 365nm ultraviolet lamp to obtain main fluorescence spots with the same color in the chromatogram of the sample at the position corresponding to the chromatogram of Chimonanthus praecox; inspecting under 254nm ultraviolet lamp to obtain main spots of the same color in the chromatogram of the sample at the position corresponding to the chromatogram of Chimonanthus praecox; spraying 10% ethanol sulfate solution, heating at 105 deg.C until yellow spots appear, and inspecting under 365nm ultraviolet lamp to obtain at least 4 identical blue and green fluorescence main spots in the chromatogram of the sample at the position corresponding to the chromatogram of Chimonanthus praecox.
The principle of the invention is as follows:
according to the chemical structure and properties of each effective component of the traditional Chinese medicine, a test sample and a reference medicinal solution are simply, conveniently and quickly prepared by adopting a proper extraction solvent according to a similar compatible extraction principle. And then proper developing agent is adopted for developing, and various chemical components can be well separated on the thin-layer plate along with the selected developing agent according to different adsorption, desorption, re-adsorption and re-desorption capabilities. And then, by means of effective components with similar polarities, the effective components are overlapped on the same thin-layer plate under different inspection conditions, but are not interfered with each other on different layers, so that different color spots are displayed, and the thin-layer chromatogram with multiple information is obtained.
The invention has the following innovation points and beneficial effects:
1. the rapid multi-information thin-layer identification method for wintersweet flower medicinal materials, particles and standard decoction dry powder is created for the first time. Namely, a test sample and a medicinal material solution are obtained by a simple and rapid pretreatment method, and are respectively spotted on the same thin-layer plate, and after the thin-layer plate is unfolded, 7 information spots of wintersweet flower medicinal materials, particles and standard decoction dry powder are inspected under 3 different inspection conditions. The fluorescence is present and not present, the fluorescence is excited and enhanced when the fluorescence is encountered in a 10% sulfuric acid ethanol solution, the fluorescence is overlapped or staggered, but the fluorescence does not interfere with each other under respective inspection conditions, and the information spot complementation under different inspection conditions is exerted. Compared with the conventional thin-layer identification, the quality controllability of the identified object is greatly improved, the quality supervision is facilitated, and the method is simple, convenient and quick, has high efficiency and low cost and does not pollute the environment.
2. Developing wintersweet flower medicinal materials, particles and standard decoction dry powder by using cyclohexane-ethyl acetate-methanol-formic acid-water as a developing agent in a volume ratio of 6: 4: 2: 0.1, and then placing the dried wintersweet flower medicinal materials, particles and standard decoction dry powder under an ultraviolet lamp of 365nm for inspection, wherein 5 fluorescent spots (shown in figure 1) with different colors are inspected on the medicinal materials and the test sample; inspecting under 254nm ultraviolet lamp to obtain 2 clear brown spots (FIG. 2); comparing the shape and size of the spots in FIGS. 1 and 2, the fluorescent spot and the tan spot are not the same compound. After 10% sulfuric acid ethanol solution is sprayed for color development, the solution is placed under an ultraviolet lamp 365nm for inspection, 4 same main fluorescent spots (figure 3) are presented on the medicinal material and the test sample, wherein 1 yellow-green fluorescent spot is different from the corresponding brown spot or fluorescent spot in figures 1 and 2 in content and spot shape analysis, which shows that the new component spot is excited after the sulfuric acid ethanol solution is sprayed for color development, so that 7 information spots are detected under 3 different inspection conditions, wherein 3 spots are overlapped or staggered, but do not interfere with each other under the respective inspection conditions, and the information spot complementation effect is exerted.
3. The identification method can obtain a sample and a medicinal material solution only by 0.2g of wintersweet flower medicinal material, 0.5g of particles and standard decoction dry powder respectively and 8ml of methanol in 20 minutes, and can perform multi-index evaluation on the sample quality by adding 12ml of developing agent, wherein the developing time is 30 minutes and the total time is 1 hour.
Drawings
FIG. 1 is a thin-layer TLC chart of Chimonanthus praecox medicinal materials, particles and target decoction dry powder under an ultraviolet lamp 365 nm.
FIG. 2 is a thin-layer TLC chart of Chimonanthus praecox medicinal materials, particles and target decoction dry powder under an ultraviolet lamp 254 nm.
FIG. 3 is a thin-layer TLC chart under 365nm of ultraviolet light after the color development of Chimonanthus praecox medicinal materials, particles and target decoction dry powder by 10% sulfuric acid ethanol solution.
FIGS. 1, 2 and 3 are thin layer chromatograms of the same thin layer plate under different inspection conditions, wherein 1.2.3 is wintersweet; 4. dried powder of wintersweet flower bud decoction; 5.6. is wintersweet flower granules;
the specific implementation mode of the invention is as follows:
taking wintersweet flower particles and wintersweet flower standard decoction dry powder 0.5g respectively, adding 3ml of methanol, performing ultrasonic treatment for 10 minutes, centrifuging, and taking supernate as a test solution; taking 0.2g of wintersweet flower medicinal material powder, adding 2ml of methanol, carrying out ultrasonic treatment for 15 minutes, centrifuging, and taking supernate as a medicinal material solution; sucking 4 μ l of the test solution, 4 μ l of the dry powder of the standard decoction, and 5 μ l of the medicinal solution, and respectively dropping on the same silica gel GF254Taking cyclohexane-ethyl acetate-methanol-formic acid-water as a developing agent with the volume ratio of 6: 4: 2: 0.1 on a thin layer plate, developing, taking out, drying by hot air, placing under an ultraviolet lamp at 365nm for inspection, and displaying main fluorescent spots with the same color on the chromatogram of the test sample at the positions corresponding to the chromatogram of the wintersweet flower medicinal material; inspecting under 254nm ultraviolet lamp to obtain main spots of the same color in the chromatogram of the sample at the position corresponding to the chromatogram of Chimonanthus praecox; spraying 10% ethanol sulfate solution, heating at 105 deg.C until yellow spots appear, and inspecting under 365nm ultraviolet lamp to obtain at least 4 identical blue and green fluorescence main spots in the chromatogram of the sample at the position corresponding to the chromatogram of Chimonanthus praecox.
Reference to the literature
【1】 Zhang Xukui sunflower, Duxiufen, Xuyanhong, etc. identification of plum blossom and Chimonanthus praecox, Shizhen national and medical science and medicine, 2003,14(8): page 480.
Claims (3)
1. A rapid multi-information thin-layer identification method for wintersweet flower granules and standard decoction dry powder is characterized in that:
taking wintersweet flower particles and wintersweet flower standard decoction dry powder 0.5g respectively, adding 3ml of methanol, performing ultrasonic treatment for 10 minutes, centrifuging, and taking supernate as a test solution; taking 0.2g of wintersweet flower medicinal material powder, adding 2ml of methanol, carrying out ultrasonic treatment for 15 minutes, centrifuging, and taking supernate as a medicinal material solution; sucking 4 μ l of the test solution, 4 μ l of the dry powder of the standard decoction, and 5 μ l of the medicinal solution, and respectively dropping on the same silica gel GF254On the thin layer plate, cyclohexane-ethyl acetate-methyl with the volume ratio of 6: 4: 2: 0.1Developing with alcohol-formic acid-water as developing agent, taking out, drying with hot air, inspecting under ultraviolet lamp 365nm, and displaying main fluorescence spots with the same color in the chromatogram of the sample at the position corresponding to the chromatogram of Chimonanthus praecox; inspecting under 254nm ultraviolet lamp to obtain main spots of the same color in the chromatogram of the sample at the position corresponding to the chromatogram of Chimonanthus praecox; spraying 10% ethanol sulfate solution, heating at 105 deg.C until yellow spots appear, and inspecting under 365nm ultraviolet lamp to obtain at least 4 identical blue and green fluorescence main spots in the chromatogram of the sample at the position corresponding to the chromatogram of Chimonanthus praecox.
2. The method for rapidly identifying the thin-layer identification of the wintersweet flower granules and the standard decoction dry powder by multiple information according to claim 1, wherein each 1g of granules is equal to 3.5g of crude drugs; each 1g of standard decoction is equivalent to 3.5g of the original medicinal material.
3. The method of claim 1, wherein the same developing agent is used to inspect 7 information spots of the dried powder of the wintersweet flower herb, the particles and the standard decoction on the same thin layer plate under 3 different inspection conditions.
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