食用油脂中挥发性卤代烃的HS-SPME-GC联用分析

doi:10.7506/spkx1002-6630-201106056

食品科学 ›› 2011, Vol. 32 ›› Issue (6 ): 242-246.doi: 10.7506/spkx1002-6630-201106056

食用油脂中挥发性卤代烃的HS-SPME-GC联用分析

赵鸿雁¹，郭莹莹¹，李磊¹,*，乙小娟²，孙建刚²，陈君义²

1.南京医科大学公共卫生学院 2.张家港出入境检验检疫局

收稿日期:2010-05-11 修回日期:2011-02-14 出版日期:2011-03-25 发布日期:2011-03-03
通讯作者: 李磊 E-mail:lilei@njmu.edu.cn
基金资助:
江苏出入境检验检疫局项目(2009KJ34)

Determination of VHHs in Edible Oils by HS-SPME followed by GC-ECD

ZHAO Hong-yan1，GUO Ying-ying1，LI Lei1,*，YI Xiao-juan2，SUN Jian-gang2，CHEN Jun-yi2

1. School of Public Health, Nanjing Medical University, Nanjing 210029, China；
2. Zhangjiagang Entry-exit Inspection and Quarantine Bureau, Zhangjiagang 215600, China

Received:2010-05-11 Revised:2011-02-14 Online:2011-03-25 Published:2011-03-03
Contact: LI Lei E-mail:lilei@njmu.edu.cn

摘要/Abstract

摘要： 目的：建立进出口油脂中挥发性卤代烃(VHHs)的顶空-固相微萃取-气相色谱(HS-SPME-GC)联用分析方法。方法：采用Supelco公司5种SPME纤维头对食用油脂进行顶空萃取，比较不同萃取纤维的萃取效率，分别考察萃取温度、时间、顶空体积等对萃取效果的影响。用毛细管色谱柱分离萃取成分、气相色谱-电子捕获检测器(GC-ECD)进行检测。结果：优选的SPME纤维头为75μm碳分子筛-聚二甲基硅氧烷(CAR/PDMS)。于15mL顶空萃取瓶中加入9mL食用油，在60℃恒温水浴中萃取30min后，290℃解吸3min进行GC分析。方法检测限为0.02～1.4ng/mL，回收率在89%～105%之间，相对标准偏差(RSD)小于8.5%(n=5)。结论：该方法具有操作简便、快捷、灵敏度高、检测限低、不使用有机溶剂等特点，适合于食用油脂中挥发性卤代烃的检测。

关键词: 食用油脂, 顶空-固相微萃取, 挥发性卤代烃, 气相色谱, 联用技术

Abstract: Objective: To establish a method for the extraction and determination of five volatile halogenerated hydrocarbons (VHHs) in edible oil by headspace solid-phase microextraction (HS-SPME) and gas chromatography-electron capture detector (GC-ECD). Methods: Samples were subjected to headspace extraction with 5 types of fiber (Supelco Inc.). Extraction efficiencies of different fibers were compared, and the effects of extraction temperature, extraction time, and solvent volume were investigated. The chromatographic separation was carried out on a capillary column equipped to a gas chromatography system with electron capture detector. Results: CAR/PDMS fiber of 75μm was the selected fiber. After pouring 9 mL of edible oil in a 15 mL vial, the extraction was conducted at the equilibrium temperature of 60 ℃ and extraction time of 30 min. The desorption of fiber was performed at 290 ℃ for 3 min. The detection limit of the established method ranged from 0.02 (tetrachloroethylene) to 1.4 ng/mL (trichloro ethane). The average recovery rate was in the range of 89%－105% with a relative standard derivation (RSD) of less than 8.5%. Conclusion: This method is simple, practical, and sensitive, which is suitable for the determination of VHHs in edible oil.

Key words: edible oil, headspace solid-phase microextraction, volatile halogenerated hydrocarbons, gas chromatography, hyphenated technology

中图分类号:

R155.5

赵鸿雁1，郭莹莹1，李磊1,*，乙小娟2，孙建刚2，陈君义2. 食用油脂中挥发性卤代烃的HS-SPME-GC联用分析[J]. 食品科学, 2011, 32(6 ): 242-246.

ZHAO Hong-yan1，GUO Ying-ying1，LI Lei1,*，YI Xiao-juan2，SUN Jian-gang2，CHEN Jun-yi2. Determination of VHHs in Edible Oils by HS-SPME followed by GC-ECD[J]. FOOD SCIENCE, 2011, 32(6 ): 242-246.

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食用油脂中挥发性卤代烃的HS-SPME-GC联用分析

Determination of VHHs in Edible Oils by HS-SPME followed by GC-ECD

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