1.Simultaneous determination of 25 components in Bawei xiaobopi capsules by HPLC-QqQ-MS
Huan YI ; Fang PENG ; Yuchen XIE ; Xiaoling GOU ; Yin DING ; Gang FAN
China Pharmacy 2022;33(14):1682-1687
OBJECTIVE To esta blish the method for simultaneous determination of 25 components (such as berberine , magnoflorine and hydroxysafflor yellow A )in Bawei xiaobopi capsules. METHODS High-performance liquid chromatography- tandem triple quadrupole mass spectrometry (HPLC-QqQ-MS)method was adopted. The determination was performed on WondaSil C18-WR column with mobile phase consisted of 0.1% formic acid solution-methanol (gradient elution )at the flow rate of 0.5 mL/min. The column temperature was 25 ℃,and sample size was 5 μL. Electrospray ionization source was scanned in positive and negative ion mode at the same time ,with multiple reaction monitoring. The capillary voltage was 4 000 V(+)and 2 500 V(-). The drying gas flow rate was 11 L/min with the temperature of 300 ℃. The pressure was 15 psi. RESULTS Totally 25 components of Bawei xiaobopi capsules had good linear relationship within a certain range ,such as magnolflorine ,jatrorrhizine,berberine, palmatine,bufotenine,bufotenidine,piperine,glycyrrhizic acid ,ferulic acid ,ferulic acid 4-O-β-D-glucopyranoside,hydroxysafflor yellow A ,chlorogenic acid ,gallic acid ,chebulagic acid ,corilagin,ellagic acid ,liquiritigenin,liquiritin,rutin,quercetin, glycocholic acid ,cholic acid ,glycochenodeoxycholic acid ,glycodeoxycholic acid ,ursodeoxycholic acid (r≥0.999 0). The limits of quantitation were 0.62-554.50 ng/mL;the limits of detection were 0.18-166.30 ng/mL.RSDs of precision ,repeatability and stability(24 h)tests were all lower than 3.00%. The recovery rates were 80%-115%(all RSDs lower than 3.00%,n=6). The contents of above 25 components were 16.94-20.82,3.78-5.17,9.11-11.43,0.24-0.30,0.20-0.39,0.74-1.16,0.79-0.89,3.26-3.35, 0.48-0.66,11.96-13.35,2.30-3.12,0.19-0.21,6.07-8.83,10.42-10.48,1.43-1.64,4.17-4.76,0.14-0.15,0.46-0.52,0.04,0.01, 0.59-0.63,0.20-0.23,0.02,0.15-0.16,0.01 mg/g,respectively. CONCLUSIONS Established method is simple ,sensitive and stable,and can be used for content determination of 25 components in Bawei xiaobopi capsules simultaneously.