摘要: 为建立红豆杉（Taxus wallichiana var. chinensis）中10-去乙酰基巴卡亭Ⅲ（10-DAB Ⅲ） 和紫杉醇（ Taxol） 的分析方法， 该文采用基质固相萃取- 高效液相色谱法方法 （MSPD-HPLC）对云南红豆杉中的10-DAB Ⅲ及Taxol 进行定量分析，考察包括硅胶、佛 罗里硅土、酸性氧化铝、中性氧化铝、碱性氧化铝、C18、C18-ME、C18-G1、C18-HC、Diol、 Xamide、Xion 共12 种样品预处理分散剂及各种分散剂的质量、洗脱剂的种类、洗脱剂的 浓度、洗脱剂体积对两种成分分析的影响，并对优化后的条件进行方法学验证，同时与超 声提取、热回流提取预处理方法进行比较分析证明其有效性。结果表明：（1）考察的12 种固相分散剂中，碱性氧化铝具有良好的目标化合物萃取检出量，且当碱性氧化铝与样品 的质量比为3∶1，6 mL 甲醇为洗脱剂洗脱时，10-DAB Ⅲ和Taxol 的萃取检出量较高。（2） 建立的红豆杉枝叶中10-DAB Ⅲ和Taxol 的分析方法具有良好的线性关系（r 0.999 9）， 10-DAB Ⅲ和Taxol 的检出限与定量限分别介于0.023 9~0.030 1 gmL-1 和0.142~0.178 gmL-1 之间；3 个水平标准物质浓度加入测定样品回收率的结果显示各目标分析物平均加 样回收率在93.6%~109.0%之间。（3）该方法与超声提取、热回流提取预处理分析结果的 比较证明，3 种方法对2 种紫杉烷类化合物的萃取检出量基本无差别，但MSPD 法溶剂消 耗少、操作简单，分析时间短，净化效率高，可应用于红豆杉原料的快速分析。该文以碱 性氧化铝为分散剂应用于云南红豆杉紫杉烷类化合物的萃取，建立了快速、高效的红豆杉 中10-DAB Ⅲ和紫杉醇的分析方法，为红豆杉中的紫杉烷类化合物的定量分析提供了依据。
Abstract: This research aimed to establish an accurate analytical methods for the quantification of 10-deacetylbaccatin III (10-DAB Ⅲ) and taxol in Taxus wallichiana var. chinensis. The method utilized matrix solid-phase dispersion coupled with high performance liquid chromatography for the respective quantification of 10-DAB Ⅲ and Taxol. The influence of various parameters was investigated, including the 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. (1) Results indicated that 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 method demonstrated excellent linearity (r 0.999 9) with detection and quantification limits for 10-DAB III and Taxol ranging from 0.023 9 to 0.030 1 gmL-1 and 0.142 to 0.178 gmL-1, respectively. The average recoveries of the target analytes varied between 93.6% and 109.0%. (3) A comparative analysis revealed 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 Taxus 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 Taxus yunnanensis, using alkaline alumina as a dispersant, providing a significant contribution to the quantitative analysis of taxanes in this species.
| [V1] | 2023-09-20 21:04:56 | ChinaXiv:202309.00166V1 | 下载全文 |
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