衢枳壳HPLC指纹图谱的建立及特征成分分析

Establishment of the HPLC Fingerprints of Citrus Changshan-huyou and Analysis of Its Characteristic Components

关键词:  衢枳壳  混淆品种  指纹图谱  聚类分析  质量评价

Key words:  Citrus changshan-huyou  adulterant  fingerprint  cluster analysis  quality control

摘要:

目的 建立衢枳壳的HPLC指纹图谱方法，并联合聚类分析技术，评价衢枳壳的质量。方法 色谱柱采用Extend XDBC18（250 mm×4.6 mm，5 μm），以乙腈-0.1%甲酸溶液为流动相进行梯度洗脱，检测波长为330 nm，柱温为30℃，流速为1.0 mL·min^-1。结果 通过11批衢枳壳样品建立了对照指纹图谱，得到19个共有峰，利用多级质谱信息，结合对照品和文献对9个共有峰进行指认，同时采用相似度分析和系统聚类分析方法对指纹图谱数据进行模式识别研究。衢枳壳相似度结果为0.995~1.000，并聚为一类，说明其质量较为一致，而其他混淆品差异性较大，另聚为一类。结论 该方法简便、快速，专属性强，可以有效地评价衢枳壳的质量。

Abstract:

OBJECTIVE To establish HPLC fingerprint method of Citrus changshan-huyou, and evaluate its quality combined with cluster analysis. METHODS The HPLC method was adopted with Extend XDB C₁₈(250 mm×4.6 mm, 5 μm) column, isocratic elution with the mobile phase was acetonitrile-0.1%formic acid solution, column temperature was 30℃, the wavelength was 330 nm, the flow rate was 1.0 mL·min^-1. RESULTS The reference HPLC fingerprints were set up through 11 batches of C.changshan-huyou, 19 common peaks were defined in fingerprints. Using MS/MS information, together with the reference standards and literatures, 9 common peaks were identified. Similarity analysis and hierarchical cluster analysis were applied to study the HPLC characteristic fingerprint and chemical pattern recognition. There were high similarity in different samples, similarity were 0.995-1.000, and were clustered together, the quality of C.changshan-huyou were consistent, others with high disparities, were clustered together. CONCLUSION This method is simple, rapid and high reproduction quality. It can provide the foundation for quality control of C.changshan-huyou.