To establish an UPLC-MS/MS method to measure the content of 18 characteristic components in Fengshiantai tablets,and conduct chemometric analysis on the measurement results to provide a basis for quality control.
The components were separated on Waters BEH C18 (100 mm×2.1 mm,1.7 μm) column with methanol and 0.1% formic acid aqueous solution as the mobile phase by gradient elution at a flow rate of 0.2 mL·min-1. The column temperature was set at 40 ℃. The injection volume was 1 μL. The detection was carried out by electrospray ionization(ESI),and electron spray ionization source was adopted in positive ion detection with multiple reaction monitoring mode(MRM).
The established methods showed a good linear relationship in a certain range (r≥0.998 3),whose average recovery rates of samples were 90.2%-101.7% with the RSD of 1.1%-4.9%. The content of ephedrine(calculated as ephedrine hydrochloride),chlorogenic acid,syringin,strychnine,brucine,berberine(calculated as berberine hydrochloride),naringin,cinnamaldehyde,ginsenoside Re,ginsenoside Rg1,epimedin C,icariin,asperosaponin Ⅵ,glycyrrhizic acid(calculated as glycyrrhizic acid ammonium salt),ginsenoside Rb1,notopterol,isoimperatorin in 39 batches of samples were 20.23-141.75 μg per tablet,10.50-121.69 μg per tablet,215.24-697.34 μg per tablet,8.46-42.42 μg per tablet,135.24-363.32 μg per tablet,91.29-242.87 μg per tablet,19.65-80.31 μg per tablet,22.57-105.05 μg per tablet,4.69-86.88 μg per tablet,10.32-241.15 μg per tablet,3.36-65.07 μg per tablet,10.79-390.69 μg per tablet,6.51-86.29 μg per tablet,4.10-89.75 μg per tablet,195.55-566.37 μg per tablet,96.98-448.95 μg per tablet,0-132.41 μg per tablet,7.09-232.71 μg per tablet. The results of chemometrics showed that 39 batches of samples from 5 production enterprises were classify into three categories,and there were certain differeces in sample quality among different production enterprises,eight differential markers(naringin,glycyrrhizic acid,isoimperatorin,berberine,syringin,ephedrine,pseudoephedrine,strychnine) that caused quality differences were found.
The established method is simple and feasible,combined with chemometric methods,and can be used for quality evaluation of Fengshiantai tablets.
| 科 Family | 属数 Number of genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) | 属 Genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) |
|---|---|---|---|---|---|---|
| 鹅膏菌科Amanitaceae | 2 | 11 | 5.26 | 鹅膏菌属 Amanita | 10 | 4.78 |
| 小菇科 Mycenaceae | 2 | 12 | 5.74 | 丝盖伞属 Inocybe | 5 | 2.39 |
| 多孔菌科 Polyporaceae | 8 | 14 | 6.70 | 蜡蘑属 Laccaria | 5 | 2.39 |
| 红菇科 Russulaceae | 3 | 23 | 11.00 | 小皮伞属 Marasmius | 6 | 2.87 |
| 小菇属 Mycena | 11 | 5.26 | ||||
| 光柄菇属 Pluteus | 5 | 2.39 | ||||
| 红菇属 Russula | 17 | 8.13 | ||||
| 栓菌属 Trametes | 5 | 2.39 |