| Filifolium sibiricum(L.)Kitam.(FSK)is from compositae Filifolium Kitamura perennial herbs.Taste bitter,cold in nature,into the liver meridian.Have heat-clearing and detoxifying,antibacterial anti-inflammatory,sedative calm,regulated the menstrual function hemostatic effect and so on.In order to improve the study of the FSK,control the authenticity of a FSK medicinal materials quality,standardize the production and use of FSK,developing new drugs for FSK,it is necessary to carry out FSK quality criteria,specific content is as follows:1.study on quality standard of FSKWith reference to the 2015 edition of China pharmacopoeia relevant methods of the general principles of the fourth,the FSK water content,total ash,acid insoluble components and content of water-soluble extract were determined;By thin layer chromatography,with rutin as reference substance,qualitative identification for FSK;The NaNO2-Al(NO3)3-NaOH colorimetric method,with rutin as index,by researching methodology,established a method for the determination of content of the total flavones;By HPLC method,Venusil XBP C18(L)(4.6 mm*250 mm,5 microns)chromatographic column,with acetonitrile:PBS system(0.1 mol/L sodium dihydrogen phosphate and 2%glacial acetic acid in 1:1 mixed)as mobile phase,elution program of 0 min to 60 min,acetonitrile percentage from 12%to 18%,the flow rate of 0.8 mL/min,column temperature of 35,C,sample volume for 10?L,detection wavelength of 360 nm,in different harvesting time of FSK isoorientin,scopoletin,rutin,isoquercitrin,luteoloside,isorhamnetin-3-O-?-D-glucoside for quantitative analysis.And FSK of different harvesting time isoorientin,scopoletin and rutin content were determined.From the experimental results show that the thin layer identification method has good specificity is strong,the spots were clear,good separating degree;The average moisture content was 6.010%,the average total ash content was 8.161%,the average acid insoluble component content is 3.824%,the average content of water-soluble extract was 15.06%,the average content of the total flavones is 14.62%;After content analysis,determine the FSK optimal harvest time for July and August,in the best harvest time,minimum content of isoorientin content is 0.1942 mg/g,minimum content of rutin is 10.06 mg/g,minimum content of isoquercitrin is 2.219 mg/g,minimum content of luteoloside is 10.61 mg/g,minimum content of isorhamnetin-3-O-?-D-glucoside is 1.681 mg/g.According to the experimental results to set limit to of FSK,moisture content shall not exceed 8%,the total ash content must not exceed 10%.acid insoluble ash content must not exceed 5%,water soluble extract shall not be less than 10%,in terms of dry goods,the total flavones content shall not be less than 10%,the content of isoorientin should be not less than 0.014%,the content of rutin should be not less than 0.70%,the content of isoquercitrin should not less than 0.15%,the content of luteoloside should be not under 0.75%,the content of isorhamnetin-3-O-?-D-glucoside should be not less than 0.12%.2.Preparation the total flavones of FSKThrough the study of preparation technology,optimize the preparation technology of the total flavones of FSK.First of all,through the orthogonal experiment for ethanol concentration,solid-liquid ratio,extraction time and extraction times four factors were studied,in order to extract the flavonoids content as an index to evaluate;Second,different concentration of alcohol and ethanol volume in addition to the ability of chlorophyll,except the chlorophyll to optimize the process;Finally,the AB-8,D101,DM130,HPD600 four different macroporous adsorption resin on the research of the the total flavones of FSK purification ability,choose suitable for FSK and purification of macroporous adsorption resin.The study found that the best preparation technology of 20 times the quality of crude drug,50%ethanol,heating reflux extraction 3 times,1.5 hours every time,after recovered solvents,with 30 times the quality of crude drug volume of 50%ethanol alcohol sink in addition to the chlorophyll,with AB-8 macroporous adsorption resin for purification the total flavones of FSK.3.Study on quality standard of the total flavones of FSK capsulesReference to the 2015 edition of Chinese pharmacopoeia of the general principles of the fourth in the relevant methods,determination the water content of the total flavones of FSK capsules,the difference of filling quantity and disintegration time,the experimental results show that the water content,the difference of filling quantity and disintegration time of the total flavones of FSK capsules are conform to the 2015 edition of Chinese pharmacopoeia relevant provision.On the total flavones of FSK capsules content analysis showed that total flavones of FSK capsules containing total flavones of FSK 50mg,the total flavones of FSK capsules(specifications 50 mg/grain)containing total flavones 28.37 mg/grains,total flavones content in each capsules should be not less than 20 mg,isoorientin,rutin,isoquercitrin,luteoloside,isorhamnetin-3-O-?-D-glucoside five compounds content is 0.06050mg/grain,2.659mg/grain,0.4126mg/grain,0.4088mg/grain and 0.7090mg/grain,according to the experimental results to set limit to of FSK capsules,the contents of the total flavones of FSK capsules limited,the content of isoorientin should be not less than 0.04mg,the content of rutin should be not less than 1.8mg5 the content of isoquercitrin should not less than 0.28mg,the content of luteoloside should be not under 0.28mg,the content of isorhamnetin-3-O-?-D-glucoside should be not less than 0.50mg.In experiment using HPLC to establish fingerprint of the total flavones of FSK capsules,through the methodology,the method has good precision,repeatability and stability,and the study of 10 batches of the total flavones of FSK capsules fingerprint hair found that fingerprint of isoorientin,scopoletin,rutin,isoquercitrin,luteoloside,isorhamnetin-3-O-?-D-glucoside six characteristic peak peak shape and separation degree are good,have a certain characteristic,the method is simple,accurate and reproducible,and can provide a certain basis for identification and quality evaluation of the total flavones of FSK capsules. |
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