CN105675791A - Antipyretic-and-antitoxic-powder pretreatment method for detecting rehmannia in thin-layer chromatography mode - Google Patents
Antipyretic-and-antitoxic-powder pretreatment method for detecting rehmannia in thin-layer chromatography mode Download PDFInfo
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- CN105675791A CN105675791A CN201610080408.3A CN201610080408A CN105675791A CN 105675791 A CN105675791 A CN 105675791A CN 201610080408 A CN201610080408 A CN 201610080408A CN 105675791 A CN105675791 A CN 105675791A
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- 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
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Abstract
The invention discloses an antipyretic-and-antitoxic-powder pretreatment method for detecting rehmannia in a thin-layer chromatography mode. The problem that the thin-layer chromatographym measurement effect on rehmannia for antipyretic-and-antitoxic powder in the prior art is not ideal is solved. The antipyretic-and-antitoxic-powder pretreatment method includes the steps that the antipyretic-and-antitoxic powder is taken, methyl alcohol is added into the antipyretic-and-antitoxic powder according to the adding amount of 10-20 ml/g, the mixture is subjected to supersonic extraction and filtered, filter liquid is evaporated to be dry, and residues are dissolved with water; then shaking extraction is carried out through ethyl acetate two times or above, ethyl acetate liquid is merged and evaporated to be dry, and 2 ml of methyl alcohol is added into the residues to dissolve the residues. By means of the antipyretic-and-antitoxic-powder pretreatment method, the influence of other substances in the antipyretic-and-antitoxic powder on measurement of the content of the rehmannia can be effectively avoided, and the detecting effect treated with the method is more obvious and convenient to observe.
Description
Technical field
The present invention relates to a kind of preprocess method, be specifically related to thin layer chromatography detection Radix Rehmanniae antipyretic and antitoxic powder preprocess method.
Background technology
Antipyretic and antitoxic powder is the recipe that teacher is stupid formulated more than the Qing Dynasty famous epidemic febrile disease scholar, is loaded in its " A View of Epidemic Febrile Diseases with Rashes " book shown, is now embodied in " People's Republic of China's veterinary drug allusion quotation " version two in 2010. This medicine is made up of 14 taste medical materials such as Gypsum Fibrosum, Radix Rehmanniae, Cornu Bubali, Rhizoma Coptidis, is " Baihu Tang ", " Rhizoma Coptidis toxic materials clearing away decoction " and " xijiao Dihuang Tang " tripartite's addition or subtraction of changes and obtains. The prescription of antipyretic and antitoxic powder includes: Gypsum Fibrosum 120g, Radix Rehmanniae 30g, Cornu Bubali 60g, Rhizoma Coptidis 20g, Fructus Gardeniae 30g, Cortex Moutan 20g, Radix Scutellariae 25g, Radix Paeoniae Rubra 25g, Radix Scrophulariae 25g, Rhizoma Anemarrhenae 30g, Fructus Forsythiae 30g, Radix Platycodonis 25g, Radix Glycyrrhizae 15g, Herba Lophatheri 25g; There is eliminating fire and detoxication, effect of removing heat from blood, it is mainly used in treatment pyretic toxicity clinically at veterinary drug and sends out speckle, unconsciousness due to high fever.
The quality standard of version " People's Republic of China's veterinary drug allusion quotation " two middle antipyretic and antitoxic powder in 2010 only has the thin layer of microscopical identification and Rhizoma Coptidis and differentiates, is difficult to control its quality, it is ensured that the safety of product, effectiveness and quality controllability. But in prior art, antipyretic and antitoxic powder is undesirable by the effect of the Tlc Determination of Radix Rehmanniae, it is impossible to meet demand.
Summary of the invention
The technical problem to be solved is: in prior art, antipyretic and antitoxic powder is undesirable by the effect of the Tlc Determination of Radix Rehmanniae, it is therefore intended that provide the thin layer chromatography detection Radix Rehmanniae antipyretic and antitoxic powder preprocess method solving the problems referred to above.
The present invention is achieved through the following technical solutions:
Thin layer chromatography detection Radix Rehmanniae antipyretic and antitoxic powder preprocess method, including:
Take antipyretic and antitoxic powder, according to the addition of 10～20ml/g, methanol is joined in antipyretic and antitoxic powder, supersound extraction, filters, filtrate is evaporated, and residue is dissolved in water, then make again employing ethyl acetate jolting extract twice and more than, combined ethyl acetate liquid, is evaporated, and residue adds methanol 2mL and dissolves.
In prior art before the thin layer chromatography carrying out Radix Rehmanniae detects, first raw material is carried out pretreatment, then it is added on thin layer chromatography again and carries out Determination of composition, and due to the interference effect that composition to be measured is made by other compositions in medicine, thus the preprocessing means being applicable to one of which medicine is not necessarily suitable another kind of medicine, the difference of usual form of feed pretreatment can cause testing result is caused extreme influence, thus the preprocessing means of different pharmaceutical component is also not quite similar.
In prior art, not a kind of can the thin layer chromatography of Radix Rehmanniae detects suitable in antipyretic and antitoxic powder very well preprocessing method of raw materials, the present invention character according to composition each in antipyretic and antitoxic powder, design a kind of preprocess method, can be prevented effectively from antipyretic and antitoxic powder the impact on Radix Rehmanniae assay of other materials, and make Detection results become apparent from after which processes.
Further, the power of institute's supersound extraction is 100W, frequency is 40KHz, and extraction time is 30min.
Preferably, the addition of described methanol is 12.5ml/g.
As optimally a kind of set-up mode, the amount of taking of described antipyretic and antitoxic powder is 2g, and water addition is 10mL, and ethyl acetate jolting extraction time is twice, and the addition of each ethyl acetate is 10mL.
The present invention compared with prior art, has such advantages as and beneficial effect:
Designed by the optimization of the present invention, it is possible to be prevented effectively from antipyretic and antitoxic powder the impact on Radix Rehmanniae assay of other materials, and make Detection results become apparent from after which processes, it is simple to observe.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearly understand, below in conjunction with embodiment, the present invention is described in further detail, and exemplary embodiment and the explanation thereof of the present invention are only used for explaining the present invention, not as a limitation of the invention.
Embodiment 1
Thin layer chromatography detection Radix Rehmanniae antipyretic and antitoxic powder preprocess method, concrete preparation process is as follows:
Take antipyretic and antitoxic powder 2g, add methanol 25ml, at the ultrasonic lower process 30min of power to be 100W, frequency be 40KHz, filter, filtrate is evaporated, the residue 10ml that adds water makes it dissolve, and then adopts ethyl acetate jolting to extract 2 times, each 10mL, combined ethyl acetate liquid, being evaporated, residue adds methanol 2mL and dissolves, and makes need testing solution.
Utilize Radix Rehmanniae and do not include antipyretic and antitoxic powder formula preparation control medicinal material solution and the negative sample solution of Radix Rehmanniae; Concrete preparation process is as follows:
Take control medicinal material Radix Rehmanniae 1g, add methanol 25ml, ultrasonic 30min, filter, filtrate is evaporated, and the residue 10ml that adds water makes it dissolve, and then adopts ethyl acetate jolting to extract 2 times, each 10mL, combined ethyl acetate liquid, is evaporated, and residue adds methanol 2mL and dissolves, and namely makes control medicinal material solution;
First configure the antipyretic and antitoxic powder prescription not including Radix Rehmanniae, take the 1/500 of recipe quantity, add methanol 25ml, ultrasonic 30min, filtering, filtrate is evaporated, and the residue 10ml that adds water makes it dissolve, then ethyl acetate jolting is adopted to extract 2 times, each 10mL, combined ethyl acetate liquid, it is evaporated, residue adds methanol 2mL and dissolves, and namely makes negative sample solution.
Draw need testing solution, control medicinal material solution and negative sample solution point on silica gel g thin-layer plate, with ratio be 14: 1: 0.1 chloroform, methanol and ammonia for developing solvent, launch, take out, dry; Spray, with 5% vanillin-sulfuric acid solution, is then heated to clear spot under 105 DEG C of temperature below.
Testing result:
The chromatographic results control medicinal material solution manifested after drying and the Chromatogram display clear spot of need testing solution, position corresponding with control medicinal material solution chromatograph on need testing solution, the speckle of the Chromatogram display same color of need testing solution, and the corresponding position in the chromatograph of negative sample solution does not have the speckle of same color, represent that this negative sample solution is noiseless.
Embodiment 2
The present embodiment is the comparative examples of embodiment 1, and in the present embodiment, the preprocess method of need testing solution is different, and concrete preparation process is as follows:
Taking antipyretic and antitoxic powder 2g, add methanol 25ml, at the ultrasonic lower process 30min of power to be 100W, frequency be 40KHz, filter, filtrate is evaporated, and residue adds methanol 2mL and dissolves, and makes need testing solution.
Utilize Radix Rehmanniae and do not include antipyretic and antitoxic powder formula preparation control medicinal material solution and the negative sample solution of Radix Rehmanniae;Concrete preparation process is as follows:
Taking control medicinal material Radix Rehmanniae 1g, add methanol 25ml, ultrasonic 30min, filter, filtrate is evaporated, and residue adds methanol 2mL and dissolves, and namely makes control medicinal material solution;
First configuring the antipyretic and antitoxic powder prescription not including Radix Rehmanniae, take the 1/500 of recipe quantity, add methanol 25ml, ultrasonic 30min, filter, filtrate is evaporated, and residue adds methanol 2mL and dissolves, and namely makes negative sample solution.
Draw need testing solution, control medicinal material solution and negative sample solution point on silica gel g thin-layer plate, with ratio be 14: 1: 0.1 chloroform, methanol and ammonia for developing solvent, launch, take out, dry; Spray, with 5% vanillin-sulfuric acid solution, is then heated to clear spot under 105 DEG C of temperature below.
Testing result:
The chromatographic results control medicinal material solution manifested after drying and the Chromatogram display clear spot of need testing solution, position corresponding with control medicinal material solution chromatograph on need testing solution, speckle overlaps, and is not easy to distinguish, and the corresponding position in the chromatograph of negative sample solution there is also interference.
Above-described detailed description of the invention; the purpose of the present invention, technical scheme and beneficial effect have been further described; it is it should be understood that; the foregoing is only the specific embodiment of the present invention; the protection domain being not intended to limit the present invention; all within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.
Claims (4)
1. thin layer chromatography detection Radix Rehmanniae antipyretic and antitoxic powder preprocess method, it is characterised in that including:
Take antipyretic and antitoxic powder, according to the addition of 10～20ml/g, methanol is joined in antipyretic and antitoxic powder, supersound extraction, filters, filtrate is evaporated, and residue is dissolved in water, then make again employing ethyl acetate jolting extract twice and more than, combined ethyl acetate liquid, is evaporated, and residue adds methanol 2mL and dissolves.
2. thin layer chromatography according to claim 1 detection Radix Rehmanniae antipyretic and antitoxic powder preprocess method, it is characterised in that the power of institute's supersound extraction is 100W, frequency is 40KHz, and extraction time is 30min.
3. thin layer chromatography according to claim 2 detection Radix Rehmanniae antipyretic and antitoxic powder preprocess method, it is characterised in that the addition of described methanol is 12.5ml/g.
4. the thin layer chromatography detection Radix Rehmanniae antipyretic and antitoxic powder preprocess method according to claim 1 or 2 or 3, it is characterized in that, the amount of taking of described antipyretic and antitoxic powder is 2g, and water addition is 10mL, ethyl acetate jolting extraction time is twice, and the addition of each ethyl acetate is 10mL.
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Citations (5)
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| JPS6281322A (en) * | 1985-10-04 | 1987-04-14 | Tsumura Juntendo Inc | Aldose reductase inhibitor |
| CN101672834A (en) * | 2008-12-01 | 2010-03-17 | 浙江万马药业有限公司 | Method for detecting quality of Chinese medicinal preparation for treating diabetic retinopathy |
| CN102091175A (en) * | 2011-03-18 | 2011-06-15 | 王志敏 | Method for identifying traditional Chinese medicinal preparation for treatment or adjuvant treatment of tumor diseases |
| KR20110104196A (en) * | 2010-03-16 | 2011-09-22 | (주)아모레퍼시픽 | Composition for prevention of losing hair or promotion of growing hair |
| US8168238B2 (en) * | 2009-12-29 | 2012-05-01 | Taipei Medical University | Extracts of Aquilaria hulls and use thereof in the treatment of cancer |
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2016
- 2016-02-05 CN CN201610080408.3A patent/CN105675791A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6281322A (en) * | 1985-10-04 | 1987-04-14 | Tsumura Juntendo Inc | Aldose reductase inhibitor |
| CN101672834A (en) * | 2008-12-01 | 2010-03-17 | 浙江万马药业有限公司 | Method for detecting quality of Chinese medicinal preparation for treating diabetic retinopathy |
| US8168238B2 (en) * | 2009-12-29 | 2012-05-01 | Taipei Medical University | Extracts of Aquilaria hulls and use thereof in the treatment of cancer |
| KR20110104196A (en) * | 2010-03-16 | 2011-09-22 | (주)아모레퍼시픽 | Composition for prevention of losing hair or promotion of growing hair |
| CN102091175A (en) * | 2011-03-18 | 2011-06-15 | 王志敏 | Method for identifying traditional Chinese medicinal preparation for treatment or adjuvant treatment of tumor diseases |
Non-Patent Citations (3)
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| 刘玉成 等: "仙灵骨葆片的薄层色谱鉴别", 《中医药学报》 * |
| 张涛等: "清热解毒软胶囊地黄、麦冬薄层色谱鉴别", 《亚太传统医药》 * |
| 聚乙二醇6000: "生地黄的薄层鉴别", 《丁香园论坛网HTTP://WWW.DXY.CN/BBS/TOPIC/5981363》 * |
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