详细信息
复杂天然产物的二维制备液相色谱分级系统构建及应用研究
Construction of Two-Dimensional Preparative Liquid Chromatography System and Its Application in Complex Nature Products
文献类型:期刊文献
中文题名:复杂天然产物的二维制备液相色谱分级系统构建及应用研究
英文题名:Construction of Two-Dimensional Preparative Liquid Chromatography System and Its Application in Complex Nature Products
作者:王亮[1];许展鹏[2];王嘉乐[1];郑杨光?[1];吴达[1];强子晴[2];张凌怡[2]
机构:[1]上海烟草集团有限责任公司,上海201315;[2]华东理工大学化学与分子工程学院,上海200237
年份:2026
卷号:42
期号:2
起止页码:203
中文期刊名:分析科学学报
外文期刊名:Journal of Analytical Science
收录:;北大核心:【北大核心2023】;
语种:中文
中文关键词:天然产物;二维制备液相色谱;分级分离
外文关键词:Natural products;Online preparative two-dimensional liquid chromatography;Fractionation and separation
摘要:天然产物提取物组成复杂,其中含有大量生物活性物质,对其进行分级研究,可以极大地降低样品复杂程度,对于天然产物的深度应用研究具有重要意义。本文构建了一种基于捕集柱阵列的在线二维制备液相色谱系统,应用于天然产物的分级分离研究。系统中采用稀释捕集技术,通过捕集柱阵列捕获第一维馏分,并将馏分进一步反冲至第二维分离柱实现二维分离。系统考察不同种类色谱固定相对样品的分离能力,最终确定SP207ss-C18反相色谱-反相色谱(RPLC-RPLC)的二维分离模式。采用“一维台阶梯度-二维线性梯度”的洗脱策略,不仅可有效降低高丰度组分干扰,提升二维制备系统选择性和分辨率,也使得所发展的方法更加稳定,适宜于规模化生产。以天然产物提取的烟用香原料为样品,经二维分级分离,成功获得41个馏分,采用超高效液相色谱-质谱(UHPLC-MS)结合气相色谱-质谱(GC-MS)鉴定含有5-(羟甲基)糠醛、棕榈酸、苯甲醛、茴香醛、肉桂醛、蛇床子素等组分。本文所构建的系统可为天然产物分级和纯化提供有效工具。
Natural products contain lots of bioactive substances,exhibiting rich structural diversity and bioactivity.The fractionation by chromatography can decrease the complexity of samples,showing great significance to the deep research of nature products.This study developed an online preparative two-dimensional liquid chromatography(2D-LC)system based on a trapping column array for the fractionation of the extract of natural products.The system employed a dilution-trapping technique,where the eluates from the first-dimension column were captured by the trapping column array and subsequently back-flushed into the second-dimension column for further separation.By investigating separation ability of different stationary phases,the SP207ss-C18(RPLC-RPLC)2D separation system was constructed.An innovative elution strategy combining“step gradient elution in the first dimension”and“linear gradient elution in the second dimension”was designed to effectively reduce interference from high-abundance components while improving selectivity and resolution.The strategy also increases the stability of the 2D system,facilitating scale production.The system successfully isolated and purified 41 fractions from the extract of natural products,which are used as potential fragrant ingredients in cigarettes.By combining results of UHPLC-MS and GC-MS,5-hydroxymethylfurfural,oalmitic acid,benzaldehyde,p-anisaldehyde,cinnamaldehyde and osthole were identified.This method provides an efficient tool for the fractionation and separation of nature products.
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