RESUMO
OBJECTIVE:To establish a method for simultaneous determination of berberine hydrochloride,icariin,acteoside,isoflavone glucoside,paeoniflorin,mangiferin,salvianolic acid B and puerarin in Pingzang tiaoshen granule.METHODS:HPLC method was adopted.The determination was performed on InertSustain C18 column with mobile phase consisted of acetonitrile-0.05mol/L potassium dihydrogen phosphate solution (pH to 3,gradient elution) with the flow rate of 1.0 mL/min.The detection wavelength was set at 250 nm (0-23 min,puerarin,mangiferin),230 nm (＞23-30 min,paeoniflorin),220 nm (＞30-50 min,isoflavone glucoside,acteoside),286 nm (＞50-60 min,salvianolic acid B),265 nm (＞60-75 min,berberine hydrochloride),220 nm (＞75-90 min,icariin).The column temperature was set at 30 ℃,and sample size was 10 μL.RESLUTS:The linear range of berberine hydrochloride,icariin,acteoside,isoflavone glucoside,paeoniflorin,mangiferin,salvianolic acid B and puerarin were 4.000-400.0,4.843-484.3,0.498-49.8,2.366-236.6,23.26-2 326.0,3.067-306.7,3.629-362.9 μg/mL,48.23-4 823.2 μg/mL(r≥0.999 4),respectively.The limits of detection were 0.02,0.02,0.02,0.02,0.01,0.02,0.01,0.01 μg/mL;the limits of quantitation were 0.07,0.05,0.06,0.05,0.03,0.07,0.02,0.03 μg/mL,respectively.RSDs of precision,stability (24 h)and repetition tests were a11＜2.0％ (n=6).The average recoveries were 95.77％-103.50％ (RSD=0.77％-2.22％,n=6).CONCLUSIONS:Established method can be used for simultaneous determination of 8 components such as berberine hydrochloride in Pingzang tiaoshen granule.
RESUMO
OBJECTIVE:To optimize the water extraction technology of Yinju jiedu oral liquid,and provide reference for the industrial production of the preparation. METHODS:According to the investigation of extraction time-extraction rate curves of chlo-rohenic acid of Yinju jiedu formula and extraction rate of chlorohenic acid in Lonicera japonica and other combined medicinal mate-rials in the formula,decoction methods and time of L. japonica were determined. Using the comprehensive scores of linarin,harpa-goside,(R,S)-epigoitrin,psoralen+angelicin contents and dry extraction yield as indexes,L9(34)orthogonal test was designed to detect the effects of adding water amount,decoction time times and optimize the extraction technology of the residues and other me-dicinal materials. Verification test was conducted. RESULTS:The optimal technology was L. japonica decocted first for 30 min with 8-fold water;the residues and other medicinal materials were decocted with 8-fold water for 3 times,1 h each time;combin-ing all the syrups. In verification test,the average contents of chlorohenic acid,linarin,harpagoside,(R,S)-epigoitrin,psoralen+angelicin were respectively 34.51,10.31,1.97,0.21,9.79 mg/g(RSD=1.24％,1.19％,1.40％,1.71％,1.28％,n=3);aver-age dry extraction yield was 25.4％(RSD=1.64％,n=3);average extraction rate of chlorohenic acid was 78.95％(RSD=1.24％,n=3). CONCLUSIONS:In the optimized water extraction technology,both the extraction rate of chlorohenic acid and contents of other ingredients are relatively high. The technology is stable and feasible.
RESUMO
OBJECTIVE:To establish a method for the simultaneous determination of 7 active constituents in Tangshen qing-du granule. METHODS:HPLC was performed on the column of SHIMADZU Inert Sustain C18 with mobile phase of acetonitrile-0.1%phosphoric acid at a flow rate of 1.0 mL/min,detection wavelength was 327 nm for chlorogenic acid and caffeic acid,280 nm for baicalin,228 nm for arctiin and 276 nm for wogonoside,baicalein and wogonin,column temperature was 35℃,and injection volume was 10 μL. RESULTS:The linear range was 4.830-154.6 μg/mL for chlorogenic acid and(r=0.9998),0.750-24.1 μg/mL for caffeic acid(r=0.9997),22.859-731.5 μg/mL for baicalin(r=0.9997),8.491-271.7 μg/mL for arctiin(r=0.9993),2.471-79.0μg/mL for wogonoside(r=0.9996),6.656-213.0 μg/mL for baicalein(r=0.9994) and 2.756-88.2 μg/mL for wogonin (r=0.9998);RSDs of precision,stability and reproducibility tests were lower than 2.0%,recoveries were 96.86%-100.82%(RSD=1.46%,n=6),98.79%-101.09%(RSD=0.93%,n=6),97.57%-101.51%(RSD=1.37%,n=6),97.76%-99.63%(RSD=0.77%,n=6),97.99%-100.12%(RSD=0.76%,n=6),96.54%-101.07%(RSD=1.87%,n=6) and 96.60%-99.59%(RSD=1.14%,n=6). CONCLUSIONS:The method is simple with good precision,stability and reproducibilty,and can be used for the simultaneous determination of 7 active constituents in Tangshen qingdu granule.