基于UPLC-MS的牡丹皮药材质量评价研究

Study on quality evaluation of Cortex Moutan based on UPLC-MS

目的:建立超高效液相色谱-三重四极杆质谱串联法(UPLC-TQ-MS法)同时测定牡丹皮中18个化学成分,并比较其差异。方法:采用Acquity UPLC BEH C_(18)色谱柱(2.1 mm×100 mm,1.7μm),流动相为0.1%甲酸水溶液-乙腈,梯度洗脱,流速0.4 m L·min^(-1),柱温35℃,采用多反应监测(MRM)方法进行质谱扫描。结果:18个待测成分的浓度与峰面积线性关系良好(0.992 3<r^2<0.999 9)。利用正交偏最小二乘判别分析(OPLS-DA)绘制OPLS-DA得分图及VIP图,发现了芍药苷亚硫酸酯、槲皮素、儿茶素、氧化芍药苷、没食子酸、没食子酸甲酯为硫熏与未硫熏样品之间的差异性成分。结论:建立一种全面、准确的牡丹皮药材质量评价方法,同时为鉴别牡丹皮药材是否经硫熏以及质量控制提供参考。

Objective：To establish a method for simultaneous determination of 18 chemical constituents in Cortex Moutan by ultra performance liquid chromatography-triple quadrupole mass spectrometry（UPLC-TQ-MS） and to compare the differences between sulfur-smoked and sulfur-free samples.Methods：The determination was performed on a Waters UPLC BEH C18 column（2.1 mm×100 mm,1.7 μm）,with gradient elution of water（0.1% acetic acid） and acetonitrile at a flow rate of 0.4 m L·min^-1.The column temperature was 35 ℃.The target compounds were analyzed by multiple reaction monitoring（MRM） mode.Results：The linearities between the concentrations of the tested components and the peak areas were good（0.992 3〈r^2〈0.999 9）.The orthogonal partial least squares discriminant analysis（OPLS-DA） score and VIP picture were drawn by OPLS-DA,which indicated that paeoniflorin sulfite,quercetin,catechin,oxypaeoniflora,gallic acid and methyl gallate were the discriminating components between the sulfur smoked and non-sulfur smoked samples of Cortex Moutan.Conclusion：A comprehensive and accurate method for evaluating the quality of Cortex Moutan was established,which could provide reference for the identification of Cortex Moutan with or without sulfur and its quality control.