[关键词]
[摘要]
目的 建立基于谱效关系的藏药材全缘叶绿绒蒿Meconopsis integrifolia全草(非花入药部位)(HMI)的质量标志物研究方法,为其质量控制提供依据。方法 测定10批次HMI提取物的UPLC指纹图谱、UPLC-ESI-Q-TOF-MS/MS法对化学成分进行指认,测定10批样品的总抗氧化能力、ABTS自由基清除能力、DPPH自由基清除能力、超氧阴离子自由基抑制能力,采用主成分分析法筛选能更大程度反映HMI提取物的抗氧化能力指标,采用灰色关联度法关联抗氧化能力指标与指纹图谱共有峰的相关性,综合分析筛选质量标志物,HSCCC法分离鉴定所筛选化学成分的结构。结果 从HMI提取物指纹图谱确定了29个共有峰,UPLC-ESI-Q-TOF-MS/MS法指认了样品中的18种化学成分,包括16种黄酮类成分和2种生物碱类成分;主成分分析法筛选出DPPH清除能力能更大程度反映HMI提取物的抗氧化能力;灰色关联度分析表明29个共有峰与DPPH清除能力的关联度均大于0.5,综合分析确认槲皮素-3-O-β-D-葡萄糖基-(1→6)-β-D-葡萄糖苷和槲皮素-3-O-[2'''-O-乙酰基-β-D-半乳糖基-(1→6)-β-D-葡萄糖苷]作为HMI的质量标志物,其中槲皮素-3-O-[2'''-O-乙酰基-β-D-半乳糖基-(1→6)-β-D-葡萄糖苷]为新化合物。结论 基于谱效关系的HMI质量标志物的研究,对阐明药效物质基础、筛选与药效相关的核心质量标志物,保证药材质量的可控性和合理应用有重要意义。
[Key word]
[Abstract]
Objective To establish a study method for discovering quality marker of herb Meconopsis integrifolia (Non flower parts) based on spectrum-effect relationship for its quality control. Methods UPLC fingerprints and UPLC-ESI-Q-TOF-MS/MS method were used to identify the chemical components of 10 batches of HMI extracts. The total antioxidant capacity, ABTS free radical scavenging ability, DPPH free radical scavenging ability and superoxide anion free radical suppression ability of 10 batches of sample were determined. Principal component analysis was used to screen antioxidant capacity index for HMI. Grey relational analysis was used to analyze the correlation between antioxidant capacity index and common peak of fingerprint spectrum. Then, quality marker could be preliminarily discovered by comprehensive analysis associated with antioxidant capacity index and efficacy-related constituents. Finally, the constituents were separated by HSCCC. Results A total of 29 common peaks were identified from fingerprints of HMI extracts. 18 constituents were identified by UPLC-ESI-Q-TOF-MS/MS analysis, including 16 flavonoids and two alkaloids. DPPH scavenging ability was screened by principal component analysis which could reflect the antioxidant capacity of HMI extracts. Grey relational analysis showed that the correlations between the 29 common peaks and DPPH scavenging ability were all greater than 0.5. The quality markers of HMI were quercetin 3-O-β-D-glucopyrannosy-(1→6)-β-D-glucopyranoside and quercetin 3-O-[2'''-O-acetyl-β-D-galactopyranosyl-(1→6)-β-D-glucopyranoside] by comprehensive analysis. Among them, quercetin 3-O-[2'''-O-acetyl-β-D-galactopyranosyl-(1→6)-β-D-glucopyranoside] is a new compound. Conclusion Study on the quality marker of HMI based on the spectrum-effect relationship is of great significance for elucidating the pharmacodynamic material basis, screening core quality marker related to medicinal effect, and ensuring the safety and rational application of traditional medicines.
[中图分类号]
R286.2
[基金项目]
国家重点研发计划"哈萨克医、彝医、羌医防治脊柱退行性疾病和痛风研究"(2018YFC1708005);西南民族大学中央高校平台建设项目(2020PTJS26002)