双溶剂微池顶空萃取气相色谱-质谱联用分析竹叶花椒中挥发性成分

GC-MS analysis of volatile components in Zanthoxylum armatum by double solvent micro cell headspace extraction

设计了一种新型微池顶空萃取装置,用于溶剂顶空萃取,解决了溶剂顶空萃取稳定性差的问题,建立了竹叶花椒中挥发性风味成分的乙酸乙酯和正己烷双溶剂的微池顶空萃取方法。当乙酸乙酯、正己烷的初始体积分别为40.0和60.0μL时,在50℃下萃取30 min,2种萃取剂剩余量均接近10.0μL,可满足后续气相色谱-质谱联用(gas chromatography-mass spectrometry,GC-MS)分析。使用GC-MS对竹叶花椒萃取物中挥发性风味成分进行了分析,正己烷萃取相和乙酸乙酯萃取相可分别鉴定出27种和30种挥发性风味成分,除去重复鉴定出的22种,共鉴定出35种,接近顶空固相微萃取鉴定出的34种。该法测得竹叶花椒中主要挥发性风味成分芳樟醇的相对含量(43.38%)明显优于顶空固相微萃取(26.02%),进一步使用雷达区域分布图对各类挥发性风味成分的数量及相对含量进行统计分析,双溶剂微池顶空萃取共鉴定出18种变化较大的烯烃类化合物(相对含量为74.42%)优于顶空固相微萃取鉴定出的15种(相对含量为42.47%),其次是醇类、酯类,而醛类、酮类、烷烃类、醚类和芳香烃则变化差异不大。该研究为食品挥发性成分的测定提供了一种稳定高效、简单快速的新方法。

A new type of micro cell headspace extraction device was designed and prepared to solve the stability problem of volatile solvent in liquid headspace phase extraction.A micro cell headspace solvent extraction method with ethyl acetate and n-hexane double extractants was proposed for the the extraction of volatile components in Zanthoxylum armatum.When the initial volumes of ethyl acetate and n-hexane were 40.0 and 60.0μL,respectively,the residual quantities of the two extractants were close to 10.0μL under the condition of 50°C for 30 min and could meet the requirements of subsequent GC-MS analysis.Analysis was performed on the volatile flavor components in Zanthoxylum armatum extract by GC-MS,27 and 30 volatile flavor components can be separately identified by the n-hexane extraction phase and the ethyl acetate extraction phase.Twenty-two types repeatedly identified were removed,and a total of 35 components were obtained from the two solvents which close to those identified by headspace solid-phase microextraction(34).The relative content of linalool(43.38%),which was the main volatile flavor component in Zanthoxylum armatum,was found to be significantly increased compared with headspace solid-phase microextraction(26.02%).Further statistical analysis of the amount and relative content of various volatile flavor components using radar regional distribution maps showed that a total of 18 kinds of olefinic compounds(relative content of 74.42%)were identified by dual-solvent microcell headspace extraction,which was better than those identified by headspace solid phase microextraction(relative content was 42.47%).This tendency was followed by alcohols and esters,but aldehydes,ketones,alkanes,ethers and aromatic hydrocarbons had little change.This work provides a stable,efficient,simple and rapid new method for the analysis of the volatile components in food.