Simultaneous Determination of 8 Components Contents in Shenqi Jianwei Granules by UPLC-Q-Exactive Qua- drupole Electrostatic Field Orbital Hydrazine High Resolution Mass Spectrometry / 中国药房

ABSTRACT

OBJECTIVE：To develo p a method for simultaneous determination of chlorogenic acid ，paeoniflorin，hesperidin， ammonium glycyrrhizate ，limonin，nobiletin，tangeretin and lobetyolin in Shenqi jianwei granules. METHODS ：UPLC-Q-Exactive quadrupole electrostatic field orbital hydrazine high resolution mass spectrometry method was adopted. The determination was performed on Hypersil Gold C 18 column with a mobile phase consisted of acetonile- 0.1％ formic acid （gradient elution ）at the flow rate of 0.4 mL/min. The column temperature was set at 35 ℃，the sample size was 1 μL. High resolution full scan experiments was performed over the range of m/z 100-1 000 in heating electro-spray lonization and positive mode to extract the accurate mass of analytes. The contents of 8 components were determined in 3 batches of samples from 2 manufacturers. RESULTS ：The linear range of chlorogenic acid ，paeoniflorin，hesperidin，ammonium glycyrrhizate ，limonin，nobiletin，tangeretin and lobetyolin were 0.12-1.46，3.51-42.15，2.71-32.55，1.76-21.10，0.04-0.46，0.04-0.24，0.02-0.21 and 0.01-0.25 μg/mL，respectively（all r≥0.999 0）. The limits of quantitation were 6.06，0.04，0.03，0.02，7.60，0.05，0.02，6.25 ng/mL，respectively. The limits of detection were 3.03，0.01，0.01，0.01，3.80，0.01，0.01，2.50 ng/mL，respectively. RSDs of precision ，reproducibility and stability （24 h）tests were all lower than 5％（n＝6）. Average recoveries were 93.16％-97.78％（RSD≤5％，n＝6）. The contents of 8 components in 3 batches of samples were 12.62-13.20，265.01-472.26，234.20-278.90，173.10-255.74，2.32-2.83，2.37-3.58，0.79-1.22，0.91-1.78 μg/g，respectively. CONCLUSIONS ：The established method is simple ，convenient，rapid，accurate，highly reproducible and sensitive，which can be used for quality control of Shenqi jianwei granules.