ABSTRACT
Objective To establish an HPLC-DAD method for the simultaneous determination of amygdalin, oleanolic acid, ursolic acid, agrimol B, liquiritin, calycosin-7-glucoside, ruscogenin, gallic acid, psoralen, and shionone in Yifei Qinghua Granules (YQG). Methods The chromatographic separation was achieved on an Waters Symmetry-C18 (250 mm × 4.6 mm, 5.0 μm) column with mobile phase consisted of (1.0 g potassium phosphate monobasic in 1 000 mL water, the pH value was adjusted to 3.5 with phosphate)- (acetonitrile-methanol 1:1) for gradient elution, at the flow rate of 0.8 mL/min; The column temperature was 40 ℃. Results The linear ranges of amygdalin, oleanolic acid, ursolic acid, agrimol B, liquiritin, calycosin-7-glucoside, ruscogenin, gallic acid, psoralen, and shionone were 0.2-2.0 μg/mL (r = 0.999 4), 0.4-4.0 μg/mL (r = 0.999 4), 0.3-3.0 μg/mL (r = 0.999 6), 0.1-1.0 μg/mL (r = 0.999 3), 0.5-5.0 μg/mL (r = 0.999 1), 0.15-1.50 μg/mL (r = 0.999 2), 0.25-2.50 μg/mL (r = 0.999 5), 0.6-6.0 μg/mL (r = 0.999 1), 0.45-4.50 μg/mL (r = 0.999 3), and 0.12-1.20 μg/mL (r = 0.999 4), respectively. These ten components were well resolved. Their average recoveries (n = 6) respectively were 98.7% (RSD = 0.7%), 98.0% (RSD = 1.3%), 99.6% (RSD = 1.4%), 98.0% (RSD = 1.4%), 99.1% (RSD = 1.1%), 99.4% (RSD = 0.8%), 98.8% (RSD = 0.9%), 101.1% (RSD = 0.5%), 100.6% (RSD = 0.5%), and 101.7% (RSD = 0.8%). The content of ten batches of the amygdalin, oleanolic acid, ursolic acid, agrimol B, liquiritin, calycosin-7-glucoside, ruscogenin, gallic acid, psoralen, and shionone was 0.104-0.123, 0.600-0.621, 0.501-0.523, 0.100-0.121, 0.103-0.122, 0.231-0.260, 0.043-0.065, 0.055-0.069, 0.061-0.079, 0.031-0.043 mg/g, respectively. Conclusion The method is accurate, sensitive, credible, and repeatable, which can be applied to the quality control of YQG.
ABSTRACT
Objective: To develop an UPLC-Q-TOF-MS method for the determination of seven components (naringin, hesperidin, strychnine, brucine, agrimol B, wogonin, and protocatechuic acid) in Pingxiao Tablets. Methods: The analysis was performed on a Waters Acquity BEH C18 column (100 mm×2.1 mm, 1.7 μm) with the mixture of acetonitrile-water-formic acid as mobile phase, and the flow rate was 0.45 mL/min; MS scanning mode: negativion; Sample volume: 2.0 μL. Results: The linear relationship between the concentration and peak areas of the seven compounds were all linear (r>0.9996). The average recoveries (n=6) were between 99%-101%. Conclusion: This method is simple, accurate, and reliable to determine the seven contents in Pingxiao Tablets for the quality control.