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顶空-固相微萃取结合气相色谱-质谱联用技术用于樱桃酒中挥发性化合物测定的优化与应用

Optimization and application of headspace-solid-phase micro-extraction coupled with gas chromatography-mass spectrometry for the determination of volatile compounds in cherry wines.

作者信息

Xiao Zuobing, Zhou Xuan, Niu Yunwei, Yu Dan, Zhu Jiancai, Zhu Guangyong

机构信息

School of Perfume and Aroma Technology, Shanghai Institute of Technology, Shanghai 201418, PR China; Shanghai Research Institute of Fragrance and Flavor Industry, Shanghai 200232, PR China.

School of Perfume and Aroma Technology, Shanghai Institute of Technology, Shanghai 201418, PR China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2015 Jan 26;978-979:122-30. doi: 10.1016/j.jchromb.2014.12.006. Epub 2014 Dec 13.

DOI:10.1016/j.jchromb.2014.12.006
PMID:25544009
Abstract

A simple, rapid and solvent-free multi-residue method has been developed and applied to confirm and quantify a series of volatile compounds in five cherry wines by gas chromatography coupled with mass spectrometry (GC-MS). Four parameters (e.g., coating material of fiber, temperature and time of extraction, and addition of sodium chloride in the solution) of headspace solid-phase micro-extraction (HS-SPME) were optimized, resulting in the best extraction condition including 50/30 μm DVB/CAR/PDMS fiber, 45 min and 50 °C of SPME, and 2g of sodium chloride addition in the wine during the extraction. The SPME had LODs and LOQs ranging from 0.03 to 7.27 μg L(-1) and 0.10 to 24.24 μg L(-1) for analytic compounds, respectively. Repeatability and reproducibility values were all below 19.8%, with mean values of 12.7% and 10.5%, respectively. Regression coefficients (R(2)) of detective linearity of the standard curves was higher than 0.9852. Moreover, relative recoveries of analytical targets were achieved in a range of 60.7-125.6% with good relative standard deviation values (≤20.6%). In addition, a principal component analysis (PCA) was used to analyze the aroma profiles of the wines, which indicated that five samples were distinctly divided into two groups based on their different geographical origins and volatile compounds.

摘要

已开发出一种简单、快速且无溶剂的多残留方法,并应用于通过气相色谱-质谱联用(GC-MS)对五种樱桃酒中的一系列挥发性化合物进行确证和定量。对顶空固相微萃取(HS-SPME)的四个参数(如纤维涂层材料、萃取温度和时间以及溶液中氯化钠的添加量)进行了优化,得到最佳萃取条件,包括50/30μm DVB/CAR/PDMS纤维、45分钟的SPME萃取时间、50℃的萃取温度以及萃取过程中在酒中添加2g氯化钠。对于分析化合物,SPME的检测限(LOD)和定量限(LOQ)分别为0.03至7.27μg L⁻¹和0.10至24.24μg L⁻¹。重复性和再现性值均低于19.8%,平均值分别为12.7%和10.5%。标准曲线检测线性的回归系数(R²)高于0.9852。此外,分析目标物的相对回收率在60.7 - 125.6%范围内,相对标准偏差值良好(≤20.6%)。另外,采用主成分分析(PCA)对葡萄酒的香气特征进行分析,结果表明五个样品根据其不同的地理来源和挥发性化合物明显分为两组。

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