基于HPLC-Q-TOF-MS结合多元统计分析的防风与水防风快速识别模型建立及差异性标志物的核磁鉴定

Establishment of Rapid Classification Model Between Saposhnikoviae Radix and Libonotidis Radix by HPLC-Q-TOF-MS Coupled with Multivariate Statistical Analyses and Identification of Discrimination Marker by NMR

关键词:  防风  水防风  高效液相色谱-串联四级杆飞行时间质谱  核磁共振  主成分分析  聚类分析  Xanthalin

Key words:  Saposhnikoviae Radix  Libonotidis Radix  HPLC-Q-TOF-MS  NMR  principal component analysis  cluster analysis  Xanthalin

摘要:

目的 分析防风与水防风的差异化学成分,建立专属性检测方法。方法 采用高效液相色谱-串联四级杆飞行时间质谱(HPLC-Q-TOF-MS)技术测定不同产地的防风与水防风的质谱数据。通过软件对数据进行峰匹配、峰对齐和噪声过滤处理后,提取质谱特征峰,结合主成分分析和聚类分析建立快速识别模型。并根据一级质谱精确质荷比和二级质谱碎片信息,结合核磁共振的化学位移、谱线强度和偶合常数进行特征峰鉴别。结果 特征峰的主成分分析和聚类分析结果均表明防风与水防风存在显著差异,分离并鉴定出水防风差异性标志物为Xanthalin。结论 从化学成分角度建立防风与水防风辨识的新方法,该方法灵敏、准确、可靠,可用于防风的质量控制。

Abstract:

OBJECTIVE To analyze the difference of chemical compositions in Saposhnikoviae Radix and Libonotidis Radix, and to establish a specific identification method. METHODS The mass spectrometry data of Saposhnikoviae Radix and Libonotidis Radix from different habitats were acquired by HPLC-Q-TOF-MS. After the characteristic peaks were extracted with mass spectrometry data peak matching, peak alignment and noise filtering, the rapid classification model was established by principal component analysis and cluster analysis. The characteristic chemical composition were identified according to MS accurate mass and MS/MS spectrometry fragmentation information, combined with the chemical shift, spectral intensity and coupling constant in NMR. RESULTS The results of principal component analysis and cluster analysis were indicated significant differences in the characteristic peaks between Saposhnikoviae Radix and Libonotidis Radix. The discrimination marker of Xanthalin was isolated and identified in Libonotidis Radix. CONCLUSION From the perspective of chemical composition, this results provide experimental data for establishing a new method of the identification Saposhnikoviae Radix and Libonotidis Radix. The method is sensitive, accurate and reliableand for the quality control of Saposhnikoviae Radix.