[Objectives]This study aimed to establish a method for determination of adulteration dye auramine O in Gegen Qinlian tablets by HPLC-MS/MS.[Methods]The instrument conditions were as follows:column,Agilent Eclipse plus...[Objectives]This study aimed to establish a method for determination of adulteration dye auramine O in Gegen Qinlian tablets by HPLC-MS/MS.[Methods]The instrument conditions were as follows:column,Agilent Eclipse plus C18(2.1 mm×100 mm,1.8μm);mobile phase,acetonitrile-0.01 mol/L ammonium acetate;gradient elution;flow rate,0.3 mL/min;column temperature,35℃;injection volume,2μL;ion source,electrospray ionization source(ESI);and scanning mode,multiple reaction monitoring(MRM).[Results]Methodological validation shows that auramine O had a good linear relationship in the range of 0.0934-1.869 pg(r=0.9999),and the average recovery rate was 94.38%(RSD=3.60%,n=9).[Conclusions]The method established is accurate,convenient,precise,reproducible,and stable,with good linear relationship,and it can be used determine the content of adulteration dye auramine O in Gegen Qinlian tablets.展开更多
[Objectives]To establish a HPLC method for the simultaneous determination of 14 characteristic components in Gegen Qinlian tablets and the content of Gegen Qinlian tablets in 11 manufacturers.[Methods]A Inertsil ODS-3...[Objectives]To establish a HPLC method for the simultaneous determination of 14 characteristic components in Gegen Qinlian tablets and the content of Gegen Qinlian tablets in 11 manufacturers.[Methods]A Inertsil ODS-3(250 mm×4.6 mm,5μm)reversed-phase high performance liquid chromatography column was used with acetonitrile-0.02 mol/L ammonium acetate+0.03%triethylamine solution(adjusted with glacial acetic acid to pH of 4.3)as the mobile phase for gradient elution at a flow rate of 1.0 mL/min.The determination wavelength of 8 components(puerarin,daidzin,liquiritin,baicalin,wogonoside,daidzein,ammonium glycyrrhizinate,baicalein)was 250 nm;the determination wavelength of wogonoside was 280 nm;the determination wavelength of 5 components(epierberine,jatrorrhizine hydrochloride,coptisine,palmatine hydrochloride and berberine hydrochloride)was 346 nm.[Results]There was a good linear relationship between the injection volume of puerarin,daidzin,liquiritin,baicalin,wogonoside,epierberine,jatrorrhizine hydrochloride,coptisine,daidzein,palmatine hydrochloride,ammonium glycyrrhizinate,berberine hydrochloride,baicalein and wogonin and peak area(r>0.9990)in the range of 146.26-5850.24,24.13-965.04,18.45-738.00,79.18-3167.32,9.57-382.80,4.76-190.40,2.57-102.80,13.41-536.40,10.60-424.00,11.33-453.22,12.08-483.20,46.73-1869.25,20.28-811.20,12.11-484.50 ng,respectively;the average recovery rates(n=6)were 2.18%,1.79%,1.81%,1.68%,2.27%,2.13%,1.96%,1.07%,0.93%,0.61%,2.92%,0.77%,2.79%and 0.62%,respectively;the precision,repeatability and stability were good,and the RSD was less than 3%.This method was used to determine 16 batches of Gegen Qinlian tablets produced by 11 enterprises.Wogonoside was not detected in a lot of samples,but 14 components were detected for other enterprises,but the content was different.[Conclusions]The method was accurate and feasible and could be used for the overall quality control of this variety.展开更多
文摘[Objectives]This study aimed to establish a method for determination of adulteration dye auramine O in Gegen Qinlian tablets by HPLC-MS/MS.[Methods]The instrument conditions were as follows:column,Agilent Eclipse plus C18(2.1 mm×100 mm,1.8μm);mobile phase,acetonitrile-0.01 mol/L ammonium acetate;gradient elution;flow rate,0.3 mL/min;column temperature,35℃;injection volume,2μL;ion source,electrospray ionization source(ESI);and scanning mode,multiple reaction monitoring(MRM).[Results]Methodological validation shows that auramine O had a good linear relationship in the range of 0.0934-1.869 pg(r=0.9999),and the average recovery rate was 94.38%(RSD=3.60%,n=9).[Conclusions]The method established is accurate,convenient,precise,reproducible,and stable,with good linear relationship,and it can be used determine the content of adulteration dye auramine O in Gegen Qinlian tablets.
文摘[Objectives]To establish a HPLC method for the simultaneous determination of 14 characteristic components in Gegen Qinlian tablets and the content of Gegen Qinlian tablets in 11 manufacturers.[Methods]A Inertsil ODS-3(250 mm×4.6 mm,5μm)reversed-phase high performance liquid chromatography column was used with acetonitrile-0.02 mol/L ammonium acetate+0.03%triethylamine solution(adjusted with glacial acetic acid to pH of 4.3)as the mobile phase for gradient elution at a flow rate of 1.0 mL/min.The determination wavelength of 8 components(puerarin,daidzin,liquiritin,baicalin,wogonoside,daidzein,ammonium glycyrrhizinate,baicalein)was 250 nm;the determination wavelength of wogonoside was 280 nm;the determination wavelength of 5 components(epierberine,jatrorrhizine hydrochloride,coptisine,palmatine hydrochloride and berberine hydrochloride)was 346 nm.[Results]There was a good linear relationship between the injection volume of puerarin,daidzin,liquiritin,baicalin,wogonoside,epierberine,jatrorrhizine hydrochloride,coptisine,daidzein,palmatine hydrochloride,ammonium glycyrrhizinate,berberine hydrochloride,baicalein and wogonin and peak area(r>0.9990)in the range of 146.26-5850.24,24.13-965.04,18.45-738.00,79.18-3167.32,9.57-382.80,4.76-190.40,2.57-102.80,13.41-536.40,10.60-424.00,11.33-453.22,12.08-483.20,46.73-1869.25,20.28-811.20,12.11-484.50 ng,respectively;the average recovery rates(n=6)were 2.18%,1.79%,1.81%,1.68%,2.27%,2.13%,1.96%,1.07%,0.93%,0.61%,2.92%,0.77%,2.79%and 0.62%,respectively;the precision,repeatability and stability were good,and the RSD was less than 3%.This method was used to determine 16 batches of Gegen Qinlian tablets produced by 11 enterprises.Wogonoside was not detected in a lot of samples,but 14 components were detected for other enterprises,but the content was different.[Conclusions]The method was accurate and feasible and could be used for the overall quality control of this variety.
