UPLC-QTRAP-MS/MS法同时测定苍耳类药材中酚酸、蒽醌及黄酮类成分

Simultaneous Determination of Phenolic Acids,Anthraquinones and Flavonoids in Xanthii Herba and Xanthii Fructus by UPLC-QTRAP-MS/MS

建立了超高效液相色谱-三重四极杆-线性离子阱质谱（UPLC-QTRAP-MS/MS）同时测定苍耳草、苍耳子药材中酚酸、蒽醌及黄酮类18种活性成分的方法。采用Agilent ZORBAX SB-C18色谱柱（250mm×4.6mm×5μm）,以甲醇-0.2%甲酸水溶液为流动相,梯度洗脱,柱温为35℃,选择电喷雾离子源（ESI）,负离子多反应监测（MRM）扫描方式检测。结果表明：在一定的浓度范围内,18种目标化合物的线性关系良好,线性相关系数均大于0.999 4,精密度、重复性和稳定性的RSD值均小于3%;加样回收率在96.81%-102.78%之间,RSD小于3%。该方法简便准确、灵敏度高、重复性好,适用于苍耳类药材中多元活性成分的同时测定,可为苍耳类药材内在质量的综合评价和全面控制提供方法参考。

A comprehensive analytical method based on UPLC-QTRAP-MS/MS was developed for the simultaneous determination of eighteen bioactive components including phenolic acids, anthraquinones and flavonoids in Xanthii Herba and Xanthii Fructus. Under the optimized chromatographic conditions, extracts of eighteen target components were obtained on an Agilent ZORBAX SB-C18 column （250 mm × 4. 6 m m ×5 μm） using methanol-0. 2% formic acid as mobile phases for gradient elution. The flow rate was 1. 0 mL/min and the column temperature was 35 ℃. The target compounds were analyzed in the negativeion multiple reaction monitoring （MRM） mode. The results show that eighteen components have good l inear i ty, the correlation coefficients of all the calibration curves are higher than 0. 999 4. Relative standard deviations （RSDs） of precision, repeatability and stability are lower than 3 % . The recoveries range from 96.81% to 102.78%, and the RSDs are less than 3 % . The established method is accurate, sensitive, and has good repeatability. It is suitable for simultaneous determination of eighteen components in Xanthii Herba and Xanthii Fructus, which can provide a reliable and effective technique for the quality control of Xanthii Herba and Xanthii Fructus.