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[摘要]
目的 研究并建立不同产地丹参茎叶UPLC指纹图谱,采用电喷雾离子源-四极杆-飞行时间质谱(ESI-QTOF/MS)对其特征峰进行定性研究,为丹参地上茎叶资源的综合开发利用提供科学依据。方法 采用UPLC法构建丹参茎叶的指纹图谱,色谱条件为ACQUITY UPLC BEH C18(100 mm×2.1 mm,1.7 μm)色谱柱,以乙腈-0.1%甲酸水为流动相梯度洗脱,体积流量0.4 mL/min,检测波长280 nm,柱温35℃。质谱检测采用负离子模式;电压3.0 kV;离子源温度120℃;雾化温度400℃;雾化气800 L/h。同时应用相似度评价、聚类分析和主成分分析(PCA)对实验数据进行处理,以分析5个不同产地12批丹参茎叶样品间的相似性及差异性,并通过UPLC/Q-TOF/MS对丹参茎叶共有峰进行了定性分析。结果 获得丹参茎叶UPLC特征图谱,共有峰13个。12批丹参茎叶的相似度为0.823~0.997,聚类分析、PCA结果与相似度分析结果一致。结论 丹参茎叶UPLC指纹图谱的构建和化学模式的识别为其质量控制和丹参非药用部位利用价值的挖掘提供科学依据。
[Key word]
[Abstract]
Objective To study and establish the UPLC of Salvia miltiorrhiza stems and leaves (SMSL) and analyze the specific peaks composition by ESI-QTOF/MS, and provide scientific basis for the comprehensive development and utilization of resources SMSL. Methods The fingerprint of SMSL was established by UPLC, the samples were conducted by Acquity UPLC BEH C18 (100 mm×2.1 mm, 1.7 μm) and eluted with acetonitrile and 0.1% formic acid at the flow rate of 0.4 mL/min. The detection wavelength was set at 280 nm and column temperature was 35℃. Negative ion mode was chosen for qualitative analysis. The capillary voltage was set at 3.0 kV. The nebulization gas was set to 800 L/h at 400℃, and the source temperature was 120℃. The similarity evaluation, cluster analysis (CA), and principal component analysis (PCA) were used to deal with the experimental data, in order to find out the similarities and differences among the 12 batches of SMSL from five different areas. Results The specific chromatogram of SMSL was obtained, and 13 common peaks were identified by ESI-QTOF/MS. Similarities of the 12 batches of samples were 0.823-0.997, the results of CA and PCA were consistent with similarity evaluation. Conclusion The establishment of UPLC fingerprint of SMSL and the application of chemical pattern recognition can provide a more comprehensive reference for the quality control of SMSL and the utilization value of non-medicinal parts of S. miltiorrhiza.
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[基金项目]
江苏省“333高层次人才培养工程”资助项目(BRA2015391)