基于UPLC-MS的牡丹皮药材质量评价研究

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 C₁₈色谱柱（2.1 mm&#215;100 mm，1.7 μm），流动相为0.1%甲酸水溶液-乙腈，梯度洗脱，流速0.4 mL&#183;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 < r² < 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&#215;100 mm,1.7 μm),with gradient elution of water (0.1% acetic acid) and acetonitrile at a flow rate of 0.4 mL&#183;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 < r² < 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.