摘要
目的建立胡黄连UPLC指纹图谱,为科学评价及有效控制其质量提供可靠方法。方法采用Waters Acquity UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7μm),以0.5%乙酸水溶液(A)-乙腈(B)为流动相梯度洗脱;体积流量0.3 m L/min,柱温为32℃,检测波长为295 nm,对25批以胡黄连名称出售的药材进行检测。通过相似度评价,结合聚类分析(HCA)和主成分分析(PCA),对不同批次胡黄连药材进行质量评价。ESI-Q-TOF/MS正、负2种离子模式扫描对其化学成分定性分析。结果 22批胡黄连药材与3批混淆品的指纹图谱明显不同。通过建立的22批胡黄连药材UPLC指纹图谱确证了16个共有峰,并对12个共有峰进行了明确化学成分指认;胡黄连药材的相似度为0.939~0.998;通过聚类分析可大致聚成3类;PCA结果支持了HCA结果;并结合偏最小二乘法判别分析(PLS-DA)方法发现区分胡黄连样品的4个标志性化合物,指认出1、9、12号峰分别为藏黄连酚苷C、胡黄连苷I和胡黄连苷III。结论胡黄连的UPLC指纹图谱的构建和化学模式的识别为药材质量控制提供更全面的参考。
Objective To establish the UPLC fingerprint for effective quality control and scientific evaluation of Picrorhiza scrophulariiflora. Methods The analysis was performed on Waters ACQUITY UPLC BEH C18 column（100 mm × 2.1 mm, 1.7 μm）, using acetonitrile-0.5% glacial acetic acid aqueous solution as mobile phase for gradient elution, with the flow rate at 0.3 m L/min, the column temperature at 32 ℃, and the detection wavelength at 295 nm. Total of 25 batches of P. scrophulariiflora and its adulterants were analyzed. Similarity evaluation combined with hierarchical clustering analysis（HCA） and principal components analysis（PCA） were used to evaluate the quality of herbs from different batches. Ultra-performance liquid chromatographyquadrupole time-of-flight tandem mass spectrometry（UPLC-Q-TOF/MS） was used for qualitative analysis in the positive and negativeion modes. Results There were significant differences in fingerprint chromatogram among P. scrophulariiflora and its adulterants. There were 16 common peaks in UPLC fingerprint of 22 batches of P. scrophulariiflora, and 12 peaks among which were carried out for chemical components identification with the similarity at 0.939—0.998. Twenty-two samples could be classified into three clusters. The PCA result was consistent with that of HCA. The four symbolic compounds in samples were verified by PLS-DA analysis, which identified that No.1, 12, 9 peaks were picroside I, picroside III, and scrophenoside C. Conclusion The establishment of UPLC fingerprint and the recognition of chemical pattern of P. scrophulariiflora can provide a more comprehensive reference for the quality control of herbs.
出处
《中草药》
CAS
CSCD
北大核心
2018年第3期685-693,共9页
Chinese Traditional and Herbal Drugs
关键词
胡黄连
混淆品
超高效液相色谱
指纹图谱
相似度分析
聚类分析
主成分分析
偏最小二乘法
Picrorhiza scrophulariiflora Pennell
adulterant
UPLC
fingerprint
similarity evaluation
hierarchical clusteringanalysis
principal components analysis
partial least squares discrimination analysis
