UPLC-QTOF-MS结合主成分分析法用于白芍饮片的分级科学性研究

目的:考察传统白芍饮片的分级与化学成分是否具有相关性。方法:利用超高效液相色谱-四极杆飞行时间-质谱(UPLC-QTOF-MS)进行测定,采用Markerlynx软件对不同等级的白芍饮片的质谱数据进行主成分分析,找出对区分等级有贡献的标记色谱峰。LC-MS条件:采用ACQUITY UPLC^® HSS T3(2.1 mm×100 mm,1.7 μm)色谱柱,流动相为0.1%甲酸水溶液(A)-乙腈(B),梯度洗脱(0~10 min,15%B→80%B;10~20 min,80%B→95%B;20~20.1 min,95%B→15%B;20.1~25 min,15%B),流速0.4 mL·min^-1,柱温40 ℃;质谱采用离子化模式为ESI⁺,毛细管电压3.5 kV,锥孔电压40 V,离子源温度120 ℃,扫描范围m/z 100~1000。结果:根据LC-MS质谱信息,不同等级的白芍样品分别聚在不同的区域,3个等级的白芍饮片基本实现完全分离,显示各等级白芍饮片有化学成分差异。结论:传统白芍饮片的分级与化学成分具有相关性。该方法可以用于区分白芍饮片的商品等级。

Objective:To investigate whether there is correlation between the traditional classification of Radix Paeoniae Alba prepared Chinese crude drug and its chemical composition.Methods: The sample was analyzed on a UPLC coupled with QTOF mass spectrometry.The UPLC-MS data of samples were subjected to principal component analysis (PCA) in order to find the marker constituents.LC-MS conditions were as follows:The chromatographic column was ACQUITY UPLC^® HSS T3 (2.1 mm×100 mm,1.7 μm),the mobile phase was composed of 0.1% formic acid (A) and acetonitrile (B) with gradient elution (0-10 min,15%B→80%B;10-20 min,80%B→95%B;20-20.1 min,95%B→15%B;20.1-25 min,15%B),the flow rate was 0.4 mL·min^-1,the column temperature was 40 ℃;the ionization mode was ESI⁺,the capillary voltage was 3.5 kV,and the cone voltage was 40 V;the ion source temperature was set at 120 ℃ at a scanning range of m/z 100-1000.Results: According to the information of LC-MS,different grades of samples were clustered into different regions.A complete separation was basically achieved in three grades of the Radix Paeoniae Alba prepared Chinese crude drug which showed the difference of chemical compositions.Conclusion: There is a correlation between traditional classification of Radix Paeoniae Alba prepared Chinese crude drug and chemical compositions.This method can be used to classify commercial specifications of Radix Paeoniae Alba prepared Chinese crude drug.