目的 研究紫杉醇的二级质谱裂解规律,对东北红豆杉及其伤愈组织粗提物中的紫杉醇进行HPLC—ESI—MS/MS分离定性,为天然产物中该化合物的分离分析提供一种快速可靠的方法。方法对HPLC—ESI—MS/MS条件进行优化,研究紫杉醇电喷雾质谱的一级电离规律和二级质谱裂解规律,并结合液相色谱的保留时间判断东北红豆杉及其伤愈组织粗提物中紫杉醇色谱峰的归属。结果 详细阐明了紫杉醇的二级质谱裂解规律,并利用HPLC—ESI—MS/MS法准确快速地分离定性了两种粗提物中紫杉醇。结论 本方法灵敏度高,快速,选择性高,专属性好,能够作为天然产物及其产品中紫杉醇分离定性的一种快速可靠的技术手段。
Aim To study the MS/MS fragmentation mechanism of Taxol, and based on it to establish HPLC-ESI-MS/MS technique to separate and identify Taxol in the crude extracts of Taxus cuspidata and its callus culture, consequently to provide a fast and credible method for the analysis of Taxol in natural products. Methods Optimized the HPLC-ESI-MS/MS parameters for the sample analysis, and then discussed the ionization and cleavage mechanism of Taxol in ESI-MS and ESI-MS/MS, finally identified the Taxol in the samples with retention time, molecular weight and MS/MS spectra. Results Elucidated the MS/MS fragmentation mechanism of Taxol, and developed HPLC-ESI-MS/MS method to analyze Taxol in the two samples. Conclusion The HPLC-ESI-MS/MS method is rapid, highly sensitive and specific, so it is suitable for the separation and identification of Taxol in natural products.