改进的无溶剂微波提取-全二维气相色谱/飞行时间质谱分析油菜籽和花生中挥发油

食品科学 ›› 2012, Vol. 33 ›› Issue (22): 162-166.

改进的无溶剂微波提取-全二维气相色谱/飞行时间质谱分析油菜籽和花生中挥发油

赵方方1,2,3，李培武1,2,3,4,5,*，王秀嫔1,2,4，张文1,2,4，刘景坤1,5

1.中国农业科学院油料作物研究所 2.农业部油料作物生物学与遗传育种重点实验室 3.农业部生物毒素检测重点实验室 4.农业部油料产品质量安全风险评估实验室(武汉) 5.农业部油料及制品质量监督检验测试中心

收稿日期:2011-08-24 修回日期:2012-10-08 出版日期:2012-11-25 发布日期:2012-11-20
通讯作者: 李培武 E-mail:peiwuli@oilcrops.cn
基金资助:
国家自然科学基金;农业行业专项;中国农业科学院院所长基金

Analysis of Volatile Components from Rapeseeds and Peanuts Using Improved Solvent-Free Microwave Extraction-Comprehensive Two-Dimensional Gas Chromatography/Time-of-Flight Mass Spectrometry

Received:2011-08-24 Revised:2012-10-08 Online:2012-11-25 Published:2012-11-20
Contact: Pei-Wu Li E-mail:peiwuli@oilcrops.cn

摘要/Abstract

摘要： 建立了改进的无溶剂微波提取-全二维气相色谱/飞行时间质谱分析油菜籽和花生中挥发油的方法。使用羰基铁粉作为提取剂提取油料样品中的挥发油，实现无溶剂快速提取。经优化得到，羰基铁粉与样品的质量比为1:5；全二维气相色谱/飞行时间质谱(GC×GC/TOF MS)选择柱系统DB-5MS柱和DB-17柱，调制周期4s，初始温度35℃。将改进的无溶剂微波提取法(ISFME)与常规的无溶剂微波提取法(CSFME)进行比较。结果表明ISFME法更快捷，提取两种油料挥发油只需20min，而CSFME法需要50min；而且ISFME法能耗明显小于CSFME法。经 GC×GC/TOF MS鉴定得出，两种方法提取样品挥发油的主要化学成分一致，均鉴定出大量杂环类物质、氧化挥发物(醇、醛、酮、酸、酯、烃)、含S、N物和苯环类物质等成分，其中杂环类占主要地位。ISFME法提取挥发油的氧化挥发物相对含量较多，更易于生成较多的香味物质。

关键词: 羰基铁粉, 无溶剂微波提取法, 油料, 挥发油, 全二维气相色谱/飞行时间质谱

Abstract: A new method for the analysis of volatile components from rapeseeds and peanuts was established using improved solvent-free microwave extraction (ISFME)-comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry (GC×GC/TOF-MS). Carbonyl iron powder was used for the solvent-free extraction of volatile oil from rapeseeds and peanuts and its optimized ratio to crop seeds was 1:5 (m/m). A GC×GC/TOF-MS system equipped with DB-5MS and DB-17 columns was used and the modulation period and initial temperature were set as 4 s and 35 ℃, respectively. Compared with the conventional solvent-free microwave extraction (CSFME) method, the improved CSFME (ICSFME) method was time saving, and only 20 min was required for oil extraction from rapeseed and peanut compared with 50 min for the CSFME method. Moreover, the improved CSFME required less energy consumption. The volatile oil extracted by both methods had the same chemical composition as determined by GC×GC/TOF-MS. Many heterocyclic compounds as well as oxidized volatiles (alcohol, aldehydes, ketone, acid, ester and hydrocarbon) and sulfur-containing, nitrogen-containing and benzene ring-containing compounds were identified and heterocyclic compounds were predominant among these compounds. The volatile oil obtained by the ICSFME method showed a higher relative content of oxidized volatiles, which contributed to the formation of more flavor-active substances.

Key words: carbonyl iron powder, solvent-free microwave extraction, oilseed, essential oil, comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry

中图分类号:

TS207.3

赵方方1,2,3，李培武1,2,3,4,5,*，王秀嫔1,2,4，张?文1,2,4，刘景坤1,5. 改进的无溶剂微波提取-全二维气相色谱/飞行时间质谱分析油菜籽和花生中挥发油[J]. 食品科学, 2012, 33(22): 162-166.

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