CN101210915B - Cabrite medicinal materials discrimination method - Google Patents
Cabrite medicinal materials discrimination method Download PDFInfo
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- CN101210915B CN101210915B CN2007101856546A CN200710185654A CN101210915B CN 101210915 B CN101210915 B CN 101210915B CN 2007101856546 A CN2007101856546 A CN 2007101856546A CN 200710185654 A CN200710185654 A CN 200710185654A CN 101210915 B CN101210915 B CN 101210915B
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Abstract
The invention relates to a method for identifying a medicinal lizard material, which comprises the following steps of: selecting a reference lizard material as the reference, respectively preparing a test sample solution and a reference material solution, dispensing on the same silica gel G thin layer plate, developing by a developing solvent including toluene or benzene and ethyl acetate with a ratio of 1:(0.8-1.3), adding ethanol sulfate solution so that the test sample and the reference material render the identical color at corresponding positions, and visually inspecting using 365 nm UV light under UV lamp to observe fluorescent spots of the same color of the test sample and the reference material at corresponding positions. The inventive identification method has high specificity and good reproducibility, and is suitable for identification of lizard materials of all resources and for identification of the presence or not of lizard material in products prepared from lizard materials of all resources.
Description
Technical field
The invention belongs to medicinal material authentication technique field, relate to a kind of method for qualitative analysis of crude drug, particularly relate to a kind of discrimination method of Cabrite medicinal materials.
Background technology
Lizard has long medicinal history in China, and medicinal record is all arranged on Shennong's Herbal, the Compendium of Material Medica.Lizard belongs to the medicinal material of several titles, many cultivar origins, and " the Sanitation Ministry medicine standard Chinese traditional patent formulation preparation " (the 11) 217 pages of medicinal material names of recording are called " lizard ", derives from the dry body of the beautiful spot fiber crops of Lacertide lizard Eremiasargus Peters." Jilin Province's drug standards " (1977) 273 pages of medicinal material names of recording are called " numb lizard ", and another name " horse snake " derives from the dry all of the beautiful spot fiber crops of Lacertide animal lizard Eremias argus Peters; Flavor cool in nature is salty; Promoting blood circulation, the goitre that disappears dissipating bind, detoxifcation, calmness; Be used for the treatment of fracture, scrofula, tracheitis, epilepsy etc." Beijing's Chinese crude drug standard (in 1998 version) " 21～22 pages of medicinal material names of recording are called " horse snake ", derive from the dry all of beautiful spot fiber crops lizard Eremias argus Peters of Lacertide animal or North China fiber crops lizard Eremias brenchleyi Guenther; Flavor cold in nature is salty; Return lung, Liver Channel; The heat-clearing dissipating bind, inducing diuresis for removing edema; Be used for obstruction of the circulation of vital energy knot and stagnate epilepsy, scrofula, difficult urination." Beijing's prepared slices of Chinese crude drugs standard (2 years versions) " 339～340 pages of medicinal material names of recording are called " horse snake ", source, nature and flavor, return through, function and cure mainly with " Beijing's Chinese crude drug standard (in 1998 version) ".In addition, Cabrite medicinal materials also has other use title, as: numb snake, horse tongue, snake Shi Zi, beautiful line fiber crops lizard etc.Use the lizard in other sources to be used as medicine in addition in addition, and use other positions of lizard to be used as medicine, perhaps use the aquatic foods product of lizard to be used as medicine.
Although " Jilin Province's drug standards " (1977), " Beijing's Chinese crude drug standard (in 1998 version) " and " Beijing's prepared slices of Chinese crude drugs standard (2 years versions) " have all been recorded the medicinal material lizard, but just recorded the proterties of lizard, do not had chemical discrimination method about Cabrite medicinal materials." the Sanitation Ministry medicine standard Chinese traditional patent formulation preparation " (the 11) 217 pages of sources of also just having recorded lizard, the test tube experiment that in " reunion of bone sheet " [discriminating] (2) that 170 pages of this books record, provides a kind of lizard to differentiate, ninhydrin reaction for protein in the lizard, but the test findings of this method shows that feminine gender has interference, and specificity is poor.So far also do not have a kind of about the strong chemical discrimination method of the specificity of Cabrite medicinal materials.
Summary of the invention
The discrimination method that the purpose of this invention is to provide a kind of Cabrite medicinal materials, this method specificity is strong, and favorable reproducibility can accurately identify Cabrite medicinal materials and whether contain Cabrite medicinal materials.
Cabrite medicinal materials discrimination method of the present invention is to be reference substance with the lizard control medicinal material, adopts thin-layered chromatography to differentiate that concrete grammar is:
1, need testing solution preparation
Get lizard powder 0.5g, add ethanol 20mL, fully filter the dissolving back, and with the filtrate evaporate to dryness, residue adds methyl alcohol 1mL makes its dissolving, as need testing solution;
2, control medicinal material formulations prepared from solutions
Other gets lizard control medicinal material 0.5g, makes control medicinal material solution as stated above;
3, thin-layered chromatography is differentiated
Draw each 10 μ L of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene or benzene: ethyl acetate=1: 0.8～1.3 are developping agent, launch, and take out, dry, spray is with 10～15% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the spot colour developing, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color; Put under the ultraviolet lamp and inspect in 365nm, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
Described abundant dissolving is to take various possible methods, with ethanol the effective constituent in the lizard is dissolved out as much as possible, for example stirs, vibrates, heats or the like.Wherein the most simple and effective dissolving method is to place ultrasound wave to handle 20min solution.
The discrimination method of above-mentioned Cabrite medicinal materials provided by the invention is a typical method for qualitative analysis.Under different experimental situations and test condition, the experimental result that obtains may have difference slightly.In practical operation, allow the experiment condition in the above-mentioned discrimination method is carried out suitable adjustment, obtain best test findings with it, differentiate with convenient.
Generally be with toluene: ethyl acetate=1: 0.8～1.3 are developping agent, and toluene wherein can be replaced with benzene, and it is basic identical to launch effect.The developping agent ratio is 1: 1 preferably, can do suitable adjustment to the ratio of developping agent according to actual conditions.
The ethanol that uses in the experimentation and the concentration of methyl alcohol also can change, and ethanol and methyl alcohol can exchange, and to not influence of identification result, confirm in the experiment that just the effect of above-mentioned experiment condition is best.
The point sample amount of sample also can strengthen or reduce, if but the point sample amount is when being increased to 20 μ L, and need change into and put into streak, can not put is to justify spot, otherwise can produce conditions of streaking.
The developer that uses is 10～15% ethanol solution of sulfuric acid, can suitably adjust the concentration of developer as the case may be, simultaneously, also can use the methanol solution of sulfuric acid as developer.Wherein best with 10% ethanol solution of sulfuric acid color developing effect especially.
The thin layer plate that thin-layer developing is to use generally adopts the silica G plate, can also replace with silica gel H thin layer plate or other thin layer plates, and just the effect of silica gel g thin-layer plate is best.
If, perhaps be subjected to the influence of experimental situation because above-mentioned experiment condition changes, make that the colour developing of sample point is bad, can also suitably heat thin layer plate, be beneficial to colour developing.
Lizard discrimination method of the present invention is applicable to the discriminating based on the Cabrite medicinal materials in all sources that derive from beautiful spot fiber crops lizard Eremias argusPeters of Lacertide animal or North China fiber crops lizard Eremias brenchleyi Gunther, all medicinal parts that comprise lizard, and the dry product of lizard, bright product.
Lizard discrimination method of the present invention is equally applicable to contain the discriminating that whether contains Cabrite medicinal materials in the various manufactured goods (comprising folk prescription, compound manufactured goods) such as human drugs that the Cabrite medicinal materials (comprising all medicinal parts, dry product, bright product) in all sources prepares, food, health products, cosmetics, veterinary drug.
When above-mentioned discrimination method is whether the manufactured goods that are used for containing Cabrite medicinal materials are when containing the discriminating of Cabrite medicinal materials, the foundation of differentiating should be: in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the principal spot (or spot of apparent same color) of same color; Put under the ultraviolet lamp, inspect in 365nm, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence principal spot (or fluorescence spot of apparent same color) of same color.
The Chinese medicine standard modern is the modern important component part of traditional Chinese medicine, and the Chinese crude drug standard modern is the basis of Chinese medicine standard modern, and wherein, the discrimination method of Chinese crude drug is crucial.For being difficult to make clear fully specifically is the Chinese crude drug what chemical constitution has therapeutic action, and control medicinal material is that main tlc identification method is practicable, simple and rapid, economic, science, a modern discrimination method.Be based on the recognition, the present invention is in the present research data deficiency of relevant lizard, also imperfectly understands under the situation of concrete chemical constitution of lizard effective constituent, by groping repeatedly, proposed discrimination method of the present invention.
Lizard control medicinal material of the present invention be according to country about choosing the relevant regulations of control medicinal material, carry out cultivar identification with zoological method after, in conjunction with clinical efficacy, choose the complete all of high-quality Cabrite medicinal materials, pulverizing, mixing are made.Differentiate that with thin-layered chromatography lizard is to carry out according to the respective specified of Pharmacopoeia of People's Republic of China version in 2005.Discrimination method maturation of the present invention is carried out the thin layer Study on Identification to the lizard of the many batches of different places of production, separate sources, all can adopt discrimination method of the present invention to differentiate.Lizard discrimination method of the present invention is used for containing the discriminating of the manufactured goods of lizard such as reunion of bone sheet, reunion of bone capsule lizard, and negative noiseless, specificity is good, has good identification result equally.
Embodiment
Embodiment 1
Derive from the discriminating of all lizards (hereinafter to be referred as " beautiful spot fiber crops lizard ") of the beautiful spot fiber crops of Lacertide animal lizard Eremias argus Peters drying.
Get beautiful spot fiber crops lizard powder 0.5g, add ethanol 20mL, behind the sonicated 20min, filter, with the filtrate evaporate to dryness, residue adds methyl alcohol 1mL makes dissolving, as need testing solution.Get beautiful spot fiber crops lizard control medicinal material 0.5g, get control medicinal material solution with legal system.
Draw each 10 μ L of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene: ethyl acetate=1: 1 is a developping agent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the spot colour developing, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.Thin layer plate is placed under the ultraviolet lamp, inspects in 365nm, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.Medicinal material that decidable is differentiated is beautiful spot fiber crops lizard thus.
Embodiment 2
The discriminating of Cabrite medicinal materials composition in the reunion of bone capsule (capsule of making according to the Sanitation Ministry medicine standard WS3-B-2226-96 prescription).
Get reunion of bone capsule 's content 1g, add ethanol 20mL, behind the sonicated 20min, filter, with the filtrate evaporate to dryness, residue adds methyl alcohol 1mL makes dissolving, as need testing solution.Get lizard control medicinal material 0.5g, get control medicinal material solution with legal system.
Draw each 10 μ L of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene: ethyl acetate=1: 1 is a developping agent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the spot colour developing, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the principal spot of same color.Thin layer plate is placed under the ultraviolet lamp, under 365nm, inspects, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence principal spot of same color.Decidable is differentiated and is contained Cabrite medicinal materials in the medicine thus.
Embodiment 3
The discriminating of Cabrite medicinal materials composition in the reunion of bone sheet (sugar coated tablet of making according to the Sanitation Ministry medicine standard WS3-B-2226-96).
It is an amount of to get the reunion of bone sheet, removes dressing, pulverizes to be powder, takes by weighing above-mentioned powder 1g, adds ethanol 20mL, behind the sonicated 20min, filters, and filtrate evaporate to dryness, residue add methyl alcohol 1mL makes dissolving, as need testing solution.Get lizard control medicinal material 0.5g, get control medicinal material solution with legal system.
Draw each 1C μ L of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with benzene: ethyl acetate=1: 1 is a developping agent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the spot colour developing, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the principal spot of same color.Thin layer plate is placed under the ultraviolet lamp, under 365nm, inspects, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence principal spot of same color.Decidable is differentiated and is contained Cabrite medicinal materials in the medicine thus.
Claims (2)
1. the discrimination method of a Cabrite medicinal materials is to adopt thin-layered chromatography to differentiate, it is characterized in that:
Get lizard powder 0.5g, add ethanol 20mL, fully filter the dissolving back, and with the filtrate evaporate to dryness, residue adds methyl alcohol 1mL makes its dissolving, as need testing solution;
Other gets lizard control medicinal material 0.5g, makes control medicinal material solution as stated above;
Draw each 10 μ L of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene or benzene: ethyl acetate=1: 0.8～1.3 are developping agent, launch, take out, dry, spray is with 10～15% ethanol solution of sulfuric acid, it is clear that hot blast blows to spot colour developing, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on show the spot of same color; Put under the ultraviolet lamp and inspect in 365nm, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
2. Cabrite medicinal materials discrimination method according to claim 1 is characterized in that described abundant dissolving is with solution sonicated 20min.
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| CN2007101856546A CN101210915B (en) | 2007-12-24 | 2007-12-24 | Cabrite medicinal materials discrimination method |
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| CN2007101856546A CN101210915B (en) | 2007-12-24 | 2007-12-24 | Cabrite medicinal materials discrimination method |
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| CN101210915B true CN101210915B (en) | 2011-05-11 |
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| CN108426973A (en) * | 2017-02-15 | 2018-08-21 | 安徽科创药物研究所有限责任公司 | The method of quality control of Chinese medicine lizard and its application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1588082A (en) * | 2004-08-27 | 2005-03-02 | 广州中一药业有限公司 | Quality control method for Weinai-an capsule |
| CN1718220A (en) * | 2005-04-26 | 2006-01-11 | 江中药业股份有限公司 | method for discerning tablets of tonifying stomach and promoting digestion |
| CN101028474A (en) * | 2007-04-04 | 2007-09-05 | 西安碑林药业股份有限公司 | Method for inspecting the quality of Chinese preparation with Yang-and kidney tonifying functions |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1588082A (en) * | 2004-08-27 | 2005-03-02 | 广州中一药业有限公司 | Quality control method for Weinai-an capsule |
| CN1718220A (en) * | 2005-04-26 | 2006-01-11 | 江中药业股份有限公司 | method for discerning tablets of tonifying stomach and promoting digestion |
| CN101028474A (en) * | 2007-04-04 | 2007-09-05 | 西安碑林药业股份有限公司 | Method for inspecting the quality of Chinese preparation with Yang-and kidney tonifying functions |
Non-Patent Citations (1)
| Title |
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| 张明 等.几种常用中草药及制剂的薄层鉴别方法探讨.《中国医药导报》.2006,第3卷(第35期), * |
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Effective date of registration: 20210824 Address after: 036000 high tech Industrial Park, Huairen County, Shuozhou City, Shanxi Province Patentee after: SHANXI HUAYUAN MEDICINE BIOTECHNOLOGY Co.,Ltd. Address before: 202, room 5, unit eight, jade garden, Yongle court District, Shanxi, Taiyuan 030027, China Patentee before: Wang Zhimin |
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