免柱基质固相分散萃取联用高效液相色谱测定喜树果中喜树碱的含量  

Column-free Matrix Solid Phase Dispersion Extraction Based on Cucurbit[7]uril Coupled with High Performance Liquid Chromatography for Determination of Camptothecin Content in Camptotheca acuminate Decne

作　　者：喻琼林 梁坪 简伟 乔婷宜 董南[1,2] YU Qiong-Lin;LIANG Ping;JIAN Wei;QIAO Ting-Yi;DONG Nan(School of Chemistry and Chemical Engineering,Guizhou University,Guiyang 550025,China;Key Laboratory of Macrocyclic and Supramolecular Chemistry of Guizhou Province,Guiyang 550025,China)

机构地区：[1]贵州大学化学与化工学院,贵阳550025 [2]贵州大学化学与化工学院贵州省大环化学及超分子化学重点实验室,贵阳550025

出　　处：《分析化学》2022年第8期1217-1223,共7页Chinese Journal of Analytical Chemistry

基　　金：贵州省科学技术基金项目(No.ZK[2021]一般054);国家自然科学基金项目(No.22164006)资助。

摘　　要：建立了一种简单、快速、环保的免柱基质固相分散萃取(FMSPD)方法用于喜树果中喜树碱的萃取。基于七元瓜环(Q[7])对喜树碱的识别作用,将Q[7]作为FMSPD的固相分散剂,选择性地从喜树果中萃取出喜树碱,并将其转移到水相,采用高效液相色谱-紫外检测器(HPLC-UV)直接测定其含量。对各种影响萃取效率的因素,包括Q[7]的用量、研磨时间、加入水的量以及溶液的pH值进行了考察。在优化的实验条件下,建立的FMSPD-HPLC-UV分析方法的线性范围为1.0~100μg/mL,检出限(S/N=3)为0.15μg/mL,日内和日间精密度分别为4.5%和5.2%。4个浓度水平的加标回收率在97.1%~119.3%范围内。对3个不同产地喜树果中喜树碱的含量进行了测定,F检验法和t检验法表明,本方法与传统超声提取法之间无显著性差异,本方法具有更简单、快速和不使用有机溶剂的优点。A simple,rapid and environmentally friendly method named column-free matrix solid-phase dispersion(FMSPD)was developed for extraction of camptothecin from the fruits of Camptotheca acuminate Decne.Cucurbit[7]uril(Q[7])was used as the sorbent of FMSPD to selectively extract camptothecin,which was transferred into an aqueous solution and was directly detected using high performance liquid chromatography-ultraviolet detector(HPLC-UV)based on the recognition interaction of Q[7]toward the compound.The factors that influenced the extraction efficiency were investigated,including the amount of Q[7],grinding time,volume of added water,and pH value of the solution.Under the optimal experimental conditions,the dynamic linear range of the developed FMSPD-HPLC-UC method was 1.0-100μg/mL,the limit of detection was 0.15μg/mL,and the intra-and inter-day precisions were 4.5%and 5.2%,respectively.The mean recoveries(n=3)at three spiked concentration levels were from 97.1%to 119.3%.The developed method was applied to analyze four kinds of fruits of Camptotheca acuminate Decne.F-and t-tests showed that the results had no significant difference when comparing the traditional ultrasound-assisted extraction method to the novel FMSPD extraction method.However the method developed here was simpler,faster and did not use organic solvents.

关 键 词：七元瓜环 基质固相分散 喜树碱 喜树果 

分 类 号：R284.1[医药卫生—中药学] O657.72[医药卫生—中医学]