关键词: 云南红豆杉, 10-去乙酰基巴卡亭 Ⅲ, 紫杉醇, 基质固相萃取, 高效液相色谱分析

Abstract: This research aimed to establish an analytical method for the quantification of 10-deacetylbaccatin Ⅲ(10-DAB Ⅲ)and Taxol in Taxus yunnanensis. The method of matrix solid phase dispersion coupled with high performance liquid chromatography(MSPD-HPLC)was used for the respective quantification of 10-DAB Ⅲ and Taxol of T. yunnanensis. The influences of various parameters were investigated, including 12 types of solid-phase dispersants(silica gel, florisil, acid alumina, neutral alumina, alkaline alumina, C₁₈, C₁₈-ME, C₁₈-G1, C₁₈-HC, Diol, Xamide, Xion), the mass of the dispersants, and the type, concentration, and volume of the eluent on the analysis of the two components. After optimization of these conditions, the methodology was validated. Additionally, a comparative analysis was conducted with the conventional ultrasonic extraction and hot reflux extraction pretreatment methods to ascertain their effectiveness of our novel method. The results were as follows:(1)Among the 12 solid-phase dispersants examined, alkaline alumina yielded a superior extraction detection rate for 10-DAB Ⅲ and Taxol when used in a 3:1 ratio with the sample mass and 6 mL of methanol as the eluent.(2)The developed 10-DAB Ⅲ and Taxol analysis method in T. yunnanensis demonstrated that excellent linearity(r≥0.999 9)with limit of detection(LOD)and limit of quantification(LOQ)for 10-DAB Ⅲ and Taxol ranging from 0.023 9 to 0.030 1 μg·mL^-1 and from 0.142 to 0.178 μg·mL^-1, respectively. The average recoveries of the target analytes varied between 93.6% and 109.0%.(3)A comparative analysis revealed that negligible differences in extraction detection of the two taxanes between the three methods. However, the MSPD method stood out due to its lower solvent consumption, simple operation, short analysis time and high purification efficiency, making it more suitable for the rapid analysis of T. yunnanensis raw materials. Therefore, this study presents a rapid and efficient analytical method for the extraction and analysis of 10-DAB Ⅲ and Taxol in T. yunnanensis, using alkaline alumina as a dispersant, providing a significant contribution to the quantitative analysis of taxanes in this species.

Key words: Taxus yunnanensis, 10-DAB Ⅲ, Taxol, MSPD, HPLC