基于高分辨质谱技术结合化学计量学的灰贝特征性成分与特色质量评价方法研究

Study on Characteristic Components and Quality Evaluation Methods of Lime-dried Fritillaria thunbergii Using High-Resolution Mass Spectrometry and Chemometrics

关键词:  浙贝母  灰贝  生物碱  高效液相色谱联用四极杆飞行时间质谱(HPLC-QTOF-MS)  特色质量评价方法

Key words:  Fritillaria thunbergii.  lime-dried Fritillaria thunbergii  alkaloids  HPLC-QTOF-MS  characteristic quality evaluation methods

摘要:

目的 研究灰贝中特征性的生物碱成分,制定灰贝特色质量评价方法。方法 采用高效液相色谱联用四极杆飞行时间质谱(HPLC-QTOF-MS)对19批来源于相同批次浙贝母鲜品的药材、浙贝片、灰贝进行成分分析,采用Agilent MassHunter Profinder10.0和Mass Profiler Professional 15.1 (MPP)等软件对数据进行处理。结果 主成分分析结果显示灰贝、浙贝片和药材的生物碱含量存在显著差异,偏最小二乘法判别分析得分图显示三类样本可以明显区分,筛选VIP值大于1的化合物作为候选特征成分。针对差异显著的特征成分进行结构分析,初步鉴定了7个灰贝特征性化合物,其中特征性成分P5/P2以及P11/P2的峰面积比值可以区分灰贝和浙贝药材和浙贝片,可用于建立灰贝的特色质量评价方法。结论 研究发现了灰贝特征性的生物碱成分并建立了专属性质量评价方法,为制定灰贝的特色标准奠定了基础。

Abstract:

OBJECTIVE To study the characteristic alkaloidal components in lime-dried Fritillaria thunbergii (LDFT) and to develop a specialized quality evaluation method. METHODS High performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC-QTOF-MS) was used to analyze the composition of 19 batches of herbs, Fritillaria thunbergii pieces, and LDFT that derived from the same batch of fresh Fritillaria thunbergii. Data were processed using software such as Agilent MassHunter Profiler 10.0 and Mass Profiler Professional 15.1 (MPP). RESULTS The results of principal component analysis showed significant differences in the content of alkaloids between LDFT, Fritillaria thunbergii pieces, and herbs. The partial least squares discriminant analysis score plot shows that the three types of samples can be clearly differentiated. Compounds with variable influence on projection(VIP) greater than 1 were screened as candidate characterization components. Structural analysis was conducted on the significantly different characteristic components, and seven distinctive compounds of LDFT were preliminarily identified. The peak area ratios of characteristic components P5/P2 and P11/P2 can distinguish LDFT from the other two types of samples. These ratios can be used to establish a specialized quality evaluation method for LDFT. CONCLUSION The research identified characteristic alkaloid components of LDFT and established a specialized quality evaluation method, laying the foundation for setting standards for the distinctive features of LDFT.