Simultaneous determination of 10 constituents in Huoxiang zhengqi soft capsules by UPLC-MS/MS / 中国药房

ABSTRACT

OBJECTIVE To establish the ultra-high performance liquid chromatography-mass spectrometry/mass spectrometry method for simultaneous determination of liquiritin ， naringin， hesperidin， neohesperidin， nobiletin， atractylenolide Ⅲ ， imperatorin，honokiol，isoimperatorin and magnolol in Huoxiang zhengqi soft capsules. METHODS Twelve batches of Huoxiang zhengqi soft capsules were extracted by ultrasonic extraction with ethanol. The determination was performed on Ultimate XB-C 18 column with mobile phase consisted of acetonitrile - 0.1％ formic acid solution for gradient elution at the flow rate of 0.4 mL/min. The column temperature was 30 ℃. The electrospray ionization source was applied to carry out the positive and negative ion scanning with multiple react ion monitoring mode. RESULTS The linear range of liquiritin ，naringin，hesperidin，neohesperidin， nobiletin，atractylenolide Ⅲ ，imperatorin，honokiol，isoimperatorin and magnolol were 1.64-52.40，1.73-55.20，1.54-49.20， 1.71-54.80，1.74-55.60，4.19-134.00，1.51-48.40，1.61-51.60，1.80-57.60，1.74-55.60 ng/mL（r≥0.999 5），respectively. The limits of quantitation were 0.41，0.43，0.19，0.43，0.11，1.05，0.19，0.40，0.45，0.11 ng/mL，respectively. RSDs of precision ，stability （24 h）and repeatability tests were all lower than 6％. Average recoveries were 102.42％，98.65％，98.34％，101.48％，96.74％， 100.40％，104.92％，98.53％，99.50％，105.40％（RSD＝1.34％-5.44％，n＝9）. The contents of the above 10 constituents in 12 batches of Huoxiang zhengqi soft capsules were 201.21-287.89，5.03-20.37，1 465.56-1 988.35，5.35-9.01，217.09-306.44，1.91- 16.17，1 081.59-1 377.12，2 388.34-2 915.13，341.26-397.45 and 7 633.47-8 976.99 μg/g，respectively. CONCLUSIONS The established method for content determination is convenient ，sensitive and accurate ，which can be used for the quality control and evaluation of Huoxiang zhengqi related preparations.