CN105699549A - Pretreatment method for determining geniposide content in antipyretic toxin-vanquishing powder - Google Patents
Pretreatment method for determining geniposide content in antipyretic toxin-vanquishing powder Download PDFInfo
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- CN105699549A CN105699549A CN201610080374.8A CN201610080374A CN105699549A CN 105699549 A CN105699549 A CN 105699549A CN 201610080374 A CN201610080374 A CN 201610080374A CN 105699549 A CN105699549 A CN 105699549A
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- antipyretic
- toxin
- methanol solution
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- antitoxic powder
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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
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
Abstract
The invention discloses a pretreatment method for determining geniposide content in antipyretic toxin-vanquishing powder, aiming to solve the problem of poor effect in determining the content of geniposide used by the antipyretic toxin-vanquishing powder in the prior art.The pretreatment method includes the steps of precisely weighing 1.0 g of antipyretic toxin-vanquishing powder, adding a more than 50% methanol solution into the antipyretic toxin-vanquishing powder according to an addition quantity of 20-50 ml/g, weighing, performing supersonic extraction with the power being 100 W and the frequency being 40 KHz or performing heating reflux extraction for 30 minutes, cooling to the room temperature and complementing the reduced weight by the methanol solution and filtering so as to obtain filtrate.By the pretreatment method, stability and repeatability are improved greatly, and RSD (relative standard deviation) values of average adding sample recovery rate and adding sample recovery rate are increased remarkably.
Description
Technical field
The present invention relates to a kind of preprocess method, be specifically related to Determination of Gardenoside mensuration preprocess method in a kind of antipyretic and antitoxic powder。
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 the Detection results of the Determination of Gardenoside assay method disclosed in prior art is poor, it is impossible to meet demand。
Summary of the invention
The technical problem to be solved is: in prior art, the Detection results of the assay of antipyretic and antitoxic powder jasminoidin is poor, it is therefore intended that provide Determination of Gardenoside mensuration preprocess method in assay effect stability and repeated high a kind of antipyretic and antitoxic powder。
The present invention is achieved through the following technical solutions:
Determination of Gardenoside mensuration preprocess method in a kind of antipyretic and antitoxic powder, including:
Precision measures antipyretic and antitoxic powder 1.0g, adds in antipyretic and antitoxic powder according to the addition of 20～50ml/g by the methanol solution that concentration is more than 50%, and weighed weight is extracted, is cooled to room temperature, supplies less loss weight with methanol solution, obtains filtrate after filtration。
In prior art before carrying out the assay of jasminoidin, first raw material is carried out pretreatment, then it is added on chromatographic column again and carries out assay, the difference of usual form of feed pretreatment can cause that the result of detection exists huge difference, and the repeatability of testing result, degree of stability etc. are all caused greatly to be affected。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, thus the preprocessing means of different pharmaceutical component is also not quite similar。
In prior art, not a kind of can the preprocess method of Determination of Gardenoside mensuration suitable in antipyretic and antitoxic powder very well, the present invention is according to the composition in antipyretic and antitoxic powder and ratio, design a kind of preprocess method, the impact that in antipyretic and antitoxic powder, Determination of Gardenoside is measured by other materials can be prevented effectively from, and make the stability of testing result, repeatability all be greatly improved after which processes, and the RSD value of mean sample recovery rate and average recovery is remarkably improved, effect is very notable。
Further, described extracting method is the supersound extraction of power 100W, frequency 40KHz, or extraction time is the heating and refluxing extraction of 30min。
Preferably, when described extracting method is supersound extraction, the time of supersound extraction is more than 30min。
As optimally a kind of set-up mode, the concentration of described methanol solution is 75%, and the addition of methanol solution is 25ml/g。
The present invention compared with prior art, has such advantages as and beneficial effect:
Being designed by the optimization of the present invention, make the stability of testing result, repeatability all be greatly improved, and the RSD value of mean sample recovery rate and average recovery is remarkably improved, effect is very notable。
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
Determination of Gardenoside mensuration preprocess method in a kind of antipyretic and antitoxic powder, concrete preparation process is as follows:
Precision measures antipyretic and antitoxic powder 1.0g, adds in antipyretic and antitoxic powder according to the addition of 25ml/g by the methanol solution that concentration is 75%, weighed weight, power 100W, frequency 40KHz supersound extraction, being cooled to room temperature, supply less loss weight with methanol solution, the filtrate of filtration is need testing solution。
Utilizing need testing solution to carry out liquid chromatographic detection, concrete detection process is as follows:
The mobile phase of liquid chromatographic detection is chosen as acetonitrile and the water of 13: 87。In described liquid chromatographic detection, chromatographic column adopts C18Chromatographic column, chromatographic column is of a size of ID4.6mm, length 250mm, particle diameter 5um, detects wavelength 238nm。
Testing result:
(1) need testing solution six parts taking 10ul carries out liquid chromatographic detection respectively, and the calculated by peak area according to detecting the jasminoidin obtained show that RSD value is 1.098%；
(2) by need testing solution 10ul 0,2,4,6,8,10h time respectively sample introduction carry out liquid chromatographic detection, the calculated by peak area of the jasminoidin obtained according to detection show that RSD value is 0.335%；
(3) configuring the jasminoidin reference substance of 0.2732mg/mL, need testing solution 10ul and jasminoidin reference substance 10ul is carried out liquid chromatographic detection, is 99.60% according to calculated by peak area mean sample recovery rate, the RSD value of average recovery is 0.76%。
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:
Precision measures antipyretic and antitoxic powder 1.0g, adds in antipyretic and antitoxic powder according to the addition of 20ml/g by the methanol solution that concentration is 80%, weighed weight, power 100W, frequency 40KHz supersound extraction, being cooled to room temperature, supply less loss weight with methanol solution, the filtrate of filtration is need testing solution。
The testing result of the present embodiment:
(1) need testing solution six parts taking 10ul carries out liquid chromatographic detection respectively, and the calculated by peak area according to detecting the jasminoidin obtained show that RSD value is 1.206%；
(2) by need testing solution 10ul 0,2,4,6,8,10h time respectively sample introduction carry out liquid chromatographic detection, the calculated by peak area of the jasminoidin obtained according to detection show that RSD value is 0.724%；
(3) configuring the jasminoidin reference substance of 0.2732mg/mL, need testing solution 10ul and jasminoidin reference substance 10ul is carried out liquid chromatographic detection, is 93.84% according to calculated by peak area mean sample recovery rate, the RSD value of average recovery is 2.13%。
Embodiment 3
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:
Precision measures antipyretic and antitoxic powder 1.0g, adds in antipyretic and antitoxic powder according to the addition of 30ml/g by the methanol solution that concentration is 70%, weighed weight, power 100W, frequency 40KHz supersound extraction, being cooled to room temperature, supply less loss weight with methanol solution, the filtrate of filtration is need testing solution。
The testing result of the present embodiment:
(1) need testing solution six parts taking 10ul carries out liquid chromatographic detection respectively, and the calculated by peak area according to detecting the jasminoidin obtained show that RSD value is 1.104%；
(2) by need testing solution 10ul 0,2,4,6,8,10h time respectively sample introduction carry out liquid chromatographic detection, the calculated by peak area of the jasminoidin obtained according to detection show that RSD value is 1.156%；
(3) configuring the jasminoidin reference substance of 0.2732mg/mL, need testing solution 10ul and jasminoidin reference substance 10ul is carried out liquid chromatographic detection, is 95.61% according to calculated by peak area mean sample recovery rate, the RSD value of average recovery is 3.12%。
Embodiment 4
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:
Precision measures antipyretic and antitoxic powder 1.0g, adds in antipyretic and antitoxic powder according to the addition of 50ml/g by the methanol solution that concentration is 50%, weighed weight, power 100W, frequency 40KHz supersound extraction, being cooled to room temperature, supply less loss weight with methanol solution, the filtrate of filtration is need testing solution。
The testing result of the present embodiment:
(1) need testing solution six parts taking 10ul carries out liquid chromatographic detection respectively, and the calculated by peak area according to detecting the jasminoidin obtained show that RSD value is 1.131%；
(2) by need testing solution 10ul 0,2,4,6,8,10h time respectively sample introduction carry out liquid chromatographic detection, the calculated by peak area of the jasminoidin obtained according to detection show that RSD value is 0.576%；
(3) configuring the jasminoidin reference substance of 0.2732mg/mL, need testing solution 10ul and jasminoidin reference substance 10ul is carried out liquid chromatographic detection, is 96.2% according to calculated by peak area mean sample recovery rate, the RSD value of average recovery is 3.28%。
Being contrasted it can be seen that the stability of preferred version of the present invention, repeatability are all greatly improved by embodiment 1-4 testing result, and the RSD value of mean sample recovery rate and average recovery is remarkably improved, effect is very notable。
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. Determination of Gardenoside mensuration preprocess method in an antipyretic and antitoxic powder, it is characterised in that including:
Precision measures antipyretic and antitoxic powder 1.0g, adds in antipyretic and antitoxic powder according to the addition of 20～50ml/g by the methanol solution that concentration is more than 50%, and weighed weight is extracted, is cooled to room temperature, supplies less loss weight with methanol solution, obtains filtrate after filtration。
2. Determination of Gardenoside mensuration preprocess method in a kind of antipyretic and antitoxic powder according to claim 1, it is characterised in that described extracting method is the supersound extraction of power 100W, frequency 40KHz, or extraction time is the heating and refluxing extraction of 30min。
3. Determination of Gardenoside mensuration preprocess method in a kind of antipyretic and antitoxic powder according to claim 2, it is characterised in that when described extracting method is supersound extraction, the time of supersound extraction is more than 30min。
4. Determination of Gardenoside mensuration preprocess method in a kind of antipyretic and antitoxic powder according to claim 1 or 2 or 3, it is characterised in that the concentration of described methanol solution is 75%, and the addition of methanol solution is 25ml/g。
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| CN105169012A (en) * | 2015-08-28 | 2015-12-23 | 徐州天意动物药业有限公司 | Antivirus traditional Chinese medicine composition for livestock and poultry, fermented traditional Chinese medicine and preparation method and application |
| CN105273014A (en) * | 2015-11-12 | 2016-01-27 | 云南麦瑞科生物科技有限公司 | Preparation method of high-content geniposide crystals |
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Patent Citations (8)
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| JPS57151657A (en) * | 1981-03-13 | 1982-09-18 | Riken Vitamin Co Ltd | Preparation of yellow pigment resistant to green discoloration |
| KR20010096213A (en) * | 2000-04-18 | 2001-11-07 | 한태룡 | Process for Preparing Blue Pigment from Gardenia jasminoides |
| CN101537088A (en) * | 2009-04-14 | 2009-09-23 | 文永盛 | Method for controlling quality of Longdanxiegan Capsule |
| US20130202703A1 (en) * | 2010-09-27 | 2013-08-08 | Shin Sadano | Method for producing gardenia blue pigment |
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Application publication date: 20160622 |