微波辅助GO/Fe_(3)O_(4)/ZIF-8磁固相萃取-气相色谱-质谱联用 分析薰衣草中的挥发性成分  

Microwave-assisted GO/Fe_(3)O_(4)/ZIF-8 Magnetic Solid Phase Extraction Combined with Gas Chromatography-Mass Spectrometry for Determination of Volatile Components in Lavender

作　　者：陈萍 李丹丹 符继红[1] 蒋欣幸 CHEN Ping;LI Dan-Dan;FU Ji-Hong;JIANG Xin-Xing(College of Chemical Engineering,Xinjiang University,Urumqi 830046,China)

机构地区：[1]新疆大学化工学院,乌鲁木齐830046

出　　处：《分析化学》2022年第5期747-756,I0012-I0016,共15页Chinese Journal of Analytical Chemistry

基　　金：新疆维吾尔自治区自然科学基金项目(No.2020D01C032);国家自然科学基金项目(No.21565024)资助。

摘　　要：建立了一种微波辅助氧化石墨烯/四氧化三铁/2-甲基咪唑锌盐(GO/Fe_(3)O_(4)/ZIF-8)磁固相萃取(MSPE)的新型样品前处理技术(GO/Fe_(3)O_(4)/ZIF-8-MSPE),结合气相色谱-质谱联用(GC-MS)实现了对薰衣草中挥发性成分的快速分析。合成的磁性材料GO/Fe_(3)O_(4)/ZIF-8中,Fe_(3)O_(4)纳米粒子具有磁性分离和微波吸收的双重作用,极大地提高了GO/Fe_(3)O_(4)/ZIF-8的萃取效率。优化了GO/Fe_(3)O_(4)/ZIF-8-MSPE的萃取参数,获得的最佳萃取条件为:5 mg GO/Fe_(3)O_(4)/ZIF-8为吸附材料、乙酸乙酯为解吸附溶剂、微波功率600 W和微波提取时间10 min。对GO/Fe_(3)O_(4)/ZIF-8-MSPE结合GC-MS的方法进行方法学考察,检测薰衣草挥发性成分的线性范围为0.01~1.20 mg/mL,相关系数(R_(2))大于0.9988,检出限(LOD)为0.15~0.56 ng,定量限(LOQ)为4.00~4.29 ng。在最佳萃取条件下,对2012年和2017年两个不同采摘批次的21个薰衣草的挥发性成分进行分析,共鉴定出49种化合物。采用主成分分析(PCA)进行了分析,结果表明,GO/Fe_(3)O_(4)/ZIF-8-MSPE提取、GC-MS检测结合PCA可快速有效地鉴别不同采摘年份的薰衣草样品。实验结果表明,GO/Fe_(3)O_(4)/ZIF-8-MSPE萃取方法是一种快速、灵敏、简单的样品前处理技术,适合于分析天然产物中的挥发性成分。A novel microwave-assisted graphene oxide/ferroferric oxide/2-methylimidazole zinc salt magnetic solid phase extraction(GO/Fe_(3)O_(4)/ZIF-8-MSPE)method was successfully developed for determination of volatile constituents in lavender using gas chromatography-mass spectrometry(GC-MS).Fe_(3)O_(4)nanoparticles had the dual effects of magnetic separation and microwave absorption.The effective parameters of GO/Fe_(3)O_(4)/ZIF-8-MSPE were optimized.Under the optimal conditions including 5 mg of GO/Fe_(3)O_(4)/ZIF-8 as adsorbent,ethyl acetate as desorption solvent,microwave power of 600 W and extraction time of 10 min,the limits of detection and limits of quantification were in the ranges of 0.15-0.56 ng and 4.00-4.29 ng,respectively.The developed method was successfully applied to analyze 21 kinds of lavender from two different harvest years(2012 and 2017),and a total of 49 kinds of compounds were identified.The results of principal component analysis(PCA)provided a clear separation between those lavender samples harvested in different years.The results showed that the GO/Fe_(3)O_(4)/ZIF-8-MSPE was a fast,sensitive and simple method for determination of volatile constituents in plant materials.

关 键 词：GO/Fe_(3)O_(4)/ZIF-8 挥发性成分 主成分分析 磁固相萃取 薰衣草 

分 类 号：O657.63[理学—分析化学]