ABSTRACT
OBJECTIVE:To establish a method for the content determination of chlorogenic acid,rutin,phillyrin,quercetin and glycyrrhizic acid in Sangju ganmao granules. METHODS:HPLC method was adopted. The determination was performed on WondasilTM-C18 column with mobile phase consisted of acetonitrile-0.4% phosphoric acid solution(gradient elution)at the flow rate of 0.8 mL/min. The column temperature was set at 30 ℃,and the detection wavelength was set at 254 nm. The sample size was 5 μL. RESULTS:The linear range of chlorogenic acid,rutin,phillyrin,quercetin and glycyrrhizic acid were 0.014-0.560 μg (r＝0.999 2),0.022-0.880 μg(r＝0.999 6),0.010-0.400 μg(r＝0.999 9),0.016-0.640 μg(r＝0.999 9),0.011-0.440 μg(r＝0.999 1), respectively. The limits of quantitation were 0.752,0.647,0.483,0.372,0.242 mg/L;the limits of detection were 0.253,0.185, 0.157,0.162,0.098 mg/L. RSDs of precision,stability and reproducibility tests were all lower than 2.0%. The average recoveries were 97.4%-100.9%(RSD＝1.4%,n＝6),95.7%-99.0%(RSD＝1.1%,n＝6),95.1%-98.1%(RSD＝1.3%,n＝6),96.4%-99.8%(RSD＝1.4%,n＝6),97.8%-100.4%(RSD＝1.0%,n＝6),respectively. CONCLUSIONS:The method is simple,precise,stable and reproducible,and can be used for simultaneous determination of chlorogenic acid,rutin,phillyrin,quercetin and glycyrrhizic acid in Sangju ganmao granules.
ABSTRACT
OBJECTIVE:To develop a method for simultaneous determination of chlorogenic acid,geniposide,gentiopicro-side,ferulic acid,baicalin and ammonium glycyrrhizinate in Yindan pinggan capsule. METHODS:HPLC method was adopted. The separation was performed on Wonda SilTM-C18 column with mobile phase consisting of acetonitrile-0.4% phosphoric acid solu-tion(gradient elution)at the flow rate of 0.8 mL/min. The detection wavelength were set at 325 nm(chlorogenic acid,ferulic ac-id),250 nm (geniposide,ammonium glycyrrhizinate) and 275 nm (gentiopicroside,baicalin). The column temperature was 30 ℃. RESULTS:The linear ranges were 0.087-3.480 μg for chlorogenic acid(r=0.9998),0.201-8.040 μg for geniposide(r=0.9997),0.200-8.000 μg for gentiopicroside(r=0.9995),0.016-0.640 μg for ferulic acid(r=0.9999),0.105-4.200 μg for ba-icalin (r=0.9999) and 0.028-1.120 μg for ammonium glycyrrhizinate (r=0.9995),respectively. The limits of quantitation were 1.31,0.75,1.14,1.25,0.94,0.98 ng,and the limits of detection were 0.87,0.67,0.96,0.93,0.60,0.88 ng,respectively. RSDs of precision,stability and reproducibility tests were lower than 2.0%;recoveries were 99.9%-101.9%(RSD=0.7%,n=6), 98.7%-100.9%(RSD=0.9%,n=6),98.1%-101.5%(RSD=1.4%,n=6),98.5%-101.3%(RSD=1.3%,n=6),98.5%-101.7%(RSD=1.2%,n=6),98.2%-101.4%(RSD=1.2%,n=6),respectively. CONCLUSIONS:The method is simple and accurate , can be used for simultaneous determination of chlorogenic acid,geniposide,gentiopicroside,ferulic acid,baicalin and ammonium glycyrrhizinate in Yindan pinggan capsule.
ABSTRACT
OBJECTIVE:To study the preparation technology of Fanhuncao sustained-release dropping pills. METHODS:The preparation technology of Fanhuncao sustained-release dropping pills was optimized by orthogonal design and single factor test with PEG4000,PEG6000 and glycerol monostearate(GM)as carrier materials,using sphericity,pill weight difference and appearance quality as index,GM-PEG weight ratio,liquid temperature,nozzle temperature,dipping speed,dropping distance,diameter of emitter as factors and the verification test was conducted. RESULTS:The optimal technology was that the ratio of GM-PEG was 3∶7;the temperature of drug mixture was 85 ℃;the dropping speed was 40 drop/min;dropping distance was 4 cm;and the conden-sate temperature was 15 ℃;diameter of emitter was 4 mm. RSD of each index of 3 batches of dripping pills were all ≤0.58%(n=3)in verification test;the average content of chlorogenic acid was 0.14 mg/g;the average pill weight difference was 3.21%;the average sphericity was 9.43;and the average appearance quality was 4.33. Q1 h were 23.4%,24.4% and 23.3% in average(n=6),and Q12 h were 89.6%,91.2% and 91.5%(n=6). CONCLUSIONS:The optimal preparation technology is stable and simple, and can be used for industrial production of Fanhuncao sustained-release dropping pills.
ABSTRACT
OBJECTIVE:To optimize the isolation and purification technology of active components of Senecio cannabifolius with macroporous adsorption resin. METHODS:The type of macroporous adsorption resin was selected with static adsorption using adsorption capacity and resolution rate of chlorogenic acid and hyperoside as index. The isolation and purification condition was op-timized with dynamic adsorption using the elution volume of chlorogenic acid and hyperoside as index,such as maximal sample size,rinse water quantity,volume fraction and collective volume of eluant ethanol. RESULTS:Among 7 kinds of resin,HPD100 had the best purification property;the optimal purification technology was as follows as mass concentration of sample 6 mg/ml,the speed of sample loading 2 ml/min,maximal sample size 3 times of column volume(BV), rinse water quantity of 2.5 BV,60%ethanol as eluting reagent. The contents of chlorogenic acid and hyperoside were increased from 0.90,0.18 mg/g to 7.26,1.04 mg/g after purification. RSD of each index were all ≤3.0%(n=3) in validation test. CONCLUSIONS:The isolation and purification technology of active components of S. cannabifolius with HPD100 macroporous adsorption resin is stable and effective.