食品科学 ›› 2009, Vol. 30 ›› Issue (10): 149-152.doi: 10.7506/spkx1002-6630-200910029

• 分析检测 • 上一篇    下一篇

高效液相荧光法测定“北京烤鸭”鸭皮中的多环芳烃

廖倩1,高振江2,张世湘3,李开雄1   

  1. 1. 新疆石河子大学食品学院
    2. 中国农业大学工学院
    3. 中国农业大学食品科学与营养工程学院
  • 收稿日期:2008-07-26 修回日期:2008-10-08 出版日期:2009-05-15 发布日期:2010-12-29
  • 通讯作者: 李开雄 E-mail:liaoqian1984@126.com
  • 基金资助:

    国家自然科学基金项目(30571312)

Determination of Polycyclic Aromatic Hydrocarbons in Skin of “Peking Roast Duck” by High Performance Chromatography-Fluorescence Detection

LIAO Qian1,GAO Zhen-jiang2,ZHANG Shi-xiang3,LI Kai-xiong1,*   

  1. (1. College of Food, Shihezi University, Shihezi 832000, China;2. College of Engineering, China Agricultural University, Beijing
    100083, China;3. College of Food Science and Nutritional Engineering, China Agricultural University, Beijing 100083, China)
  • Received:2008-07-26 Revised:2008-10-08 Online:2009-05-15 Published:2010-12-29
  • Contact: LI Kai-xiong1,* E-mail:liaoqian1984@126.com

摘要:

采用气体射流冲击加热新技术烤制“北京烤鸭”,对其烤制过程中可能产生的三种多环芳烃(PAHs)含量进行检测,建立一套适合于烤鸭类高脂肪、高蛋白食品中PAHs 的提取与检测的方法。方法:匀浆鸭皮样品前处理采用2mol/L KOH 甲醇- 水(8:2,V/V)皂化,异辛烷萃取,甲醇- 水(1:1,V/V)洗涤,N,N- 二甲基甲酰胺- 水-异辛烷(1:1:1,V/V)反萃取和Florisil 固相萃取小柱净化,最后进行HPLC 分析。结果:标品实验回收率在83.59%~92.97%,当样品加标水平分别为1、2、2μg/kg 时,回收率在73.85%~80.31%,RSD < 10%,三种PAHs 检测量在0.56~3.19μg/kg。结论:该方法净化效果较好,重现性高,检测灵敏度和准确度均满足分析要求,样品中苯并[a]芘的含量远远低于国家规定对烟熏烧烤类食品不能超过5μg/kg 的标准。

关键词: “北京烤鸭”, 气体射流冲击, 多环芳烃(PAHs), 高效液相荧光检测(HPLC-FD)

Abstract:

In the process of “Peking Roast Duck” with a novel heating technique, namely air jet impingement, polycyclic aromatic hydrocarbons (PAHs) may be formed. A method of HPLC coupled with fluorescence detector was developed for the determination of PAHs in fat- and protein-rich foods, such as “Peking Roast Duck”. Homogenized duck skin samples were pretreated by using methanol containing 2 mol/L KOH-water (8:2, V/V) for saponification, issoctane for extraction, methanolwater (1:1, V/V) for washing, DMF-water-issoctane (1:1:1, V/V) for liquid-liquid partition, and Florisil solid-phase column for cleaning up. Results showed that the recoveries of benzo[a]pyrene (B[a]P), dibenzo[a,h]anthracene (DB[a.h]A) and 7,12- dimethylbenzene[a] anthracene (7,12-DMB[a]A) in blank sample at the spiked amounts of 2 × 10-8 and 1 × 10-7 g were between 83.59% and 92.97%, and their recoveries at the spiked amount of 1, 2 and 2 μg/kg respectively, were 73.85% to 80.31%, and the RSDs were less than 10%. Their contents in roasted duck ranged from 0.56 to 3.19 μg/kg, but no these three compounds were found in raw duck. Our results suggested the high clean-up efficiency and recovery of this method and the sensitivity and accuracy of detection could meet the requirements for analysis of trace compounds in complex matrices. The B[a]P content of 0.56 μg/kg is far less than the maximum limit value of 5 μg/kg in the smoked and roasted foods in term of the national standards.

Key words: “Peking Roast duck”, air-jet impingement, polycyclic aromatic hydrocarbons (PAHs), high performance chromatography-fluorescence detection (HPLC-FD)

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