ABSTRACT
OBJECTIVE:To develop a method for simultaneous determination of harpagide,harpagoside,chlorogenic acid, caffeic acid and phillyrin in Xiaoer qingyan granules. METHODS:HPLC method was adopted. The determination was performed on Zorbax SB-C18 column with mobile phase consisted of acetonitrile-0.1% phosphoric acid solution (gradient elution) at a flow rate of 1.0 mL/min. The detection wavelength was set at 210 nm (0-13 min,harpagide),327 nm (13-25 min,chlorogenic acid and caffeic acid),277 nm(25-29 min,phillyrin),210 nm(29-40 min,harpagosid);the column temperature was 30℃,and sam-ple size was 10 μL. RESULTS:The linear ranges of harpagide,harpagosid,chlorogenic acid,caffeic acid and phillyrin were 8.400-168.0 ng(r=0.9996),11.30-226.0 ng(r=0.9998),128.8-257.6 ng(r=0.9993),8.110-162.2 ng(r=0.9996),29.69-593.8 ng(r=0.9994),respectively. LOQs of the 5 components were 33.39,451.2,515.2,324.5,1188 ng/mL;LODs were 8.348, 112.8,128.8,81.12,297.0 ng/mL,respectively;RSDs of precision,stability and reproducibility tests were all lower than 2.0%. The recoveries were 96.39%-98.64%(RSD=0.83%,n=6),96.60%-98.89%(RSD=0.89%,n=6),96.28%-99.22%(RSD=1.25%,n=6),96.49%-99.54%(RSD=1.16%,n=6),96.26%-99.70%(RSD=1.30%,n=6),respectively. CONCLUSIONS:The method is simple,accurate and suitable for simultaneous determination of 5 components in Xiaoer qingyan granules
ABSTRACT
Objective: Taking thewater extraction of Compound Banlangen Liyan Granules (IsatidisRadix, ScrophulariaeRadix, PlatycodiRadix, GlycyrrhizaeRadix, etc.)as the research object to explore the dynamic migration regular of the active ingredient population of compoundChinesemateriamedica in different apertures in ceramic membrane separation process and compare its membrane filtration flux and solid inclusion removal rate. Methods: The water extraction of Compound Banlangen Liyan Granules was separated with 200 nm and 50 nm aperture of ceramic membrane, respectively. Continuously sampling for many times was done in the ceramic membrane separation process. The optimized HPLC methods were as follows: chromatographic column was Agilent Zorbox Eclipse XDB-C18, mobile phase was acetonitrile-0.05% phosphoric acid in gradient elution at flow rate of 1 mL/min, detection wavelength was wavelength switching, injection volum was 10 μL, the column temperature was 30 ℃. The contents of sixactive ingredients[adenosine, (R,S)-goitrin, liquiritin, harpagosid, platycodinD, and monoammonium glycyrrhizinate]were determined in thecompound at the same time, and the dynamic migration rates were investigated. Results:The simultaneous determination of the sixactive ingredient in thecompound was done with HPLC method. For the water extraction in Compound Banlangen Liyan Granules, in the 200 nm ceramic membrane separation process, the dynamic migration rates of the sixactive ingredientsranged between 71%-104%, the average migration rate was 85%, the membrane filter flux attenuation was smaller, the stable flux was in 426-340 L/(m2∙h), solid inclusion removal rate was 21.0%. But in 50 nm ceramic membrane, the dynamic migration rates of the sixactiveingredients ranged between 83%-107%, the average migration rate was83%, the membrane filter flux attenuation was larger, the stable flux was in 258-228 L/(m2∙h), and solid inclusion removal rate was23.9%. Conclusion :The experiment preliminarily reflects the dynamic migration regular of the active ingredient population of compoundChinesemateriamedica in two different aperture ceramic membrane separation process. It lays a migration theoretical foundation of effective materials for popularization and application of modern ceramic membrane technology in Chinese materiamedica refining.