色谱 ›› 2014, Vol. 32 ›› Issue (7): 784-788.DOI: 10.3724/SP.J.1123.2014.03034

• 技术与应用 • 上一篇    

介孔氧化铝净化-气相色谱法同时测定蔬菜、水果及茶叶中16种有机磷农药残留

胡业琴1, 郗存显2,3, 曹淑瑞2,3, 王国民2,3, 李贤良2,3, 张雷2,3, 张云怀1   

  1. 1. 重庆大学化学化工学院, 重庆 400030;
    2. 重庆出入境检验检疫局, 重庆 400020;
    3. 重庆市进出口食品安全工程技术研究中心, 重庆 400020
  • 收稿日期:2014-03-24 修回日期:2014-05-06 出版日期:2014-07-08 发布日期:2014-06-25
  • 通讯作者: 张云怀,E-mail:xp2031@163.com.
  • 基金资助:

    国家质量监督检验检疫总局科技计划项目(2012IK198).

Simultaneous determination of 16 organophosphorous pesticides in vegetables, fruits and tea by gas chromatography coupled with clean-up by mesoporous alumina as solid-phase extraction adsorbent

HU Yeqin1, XI Cunxian2,3, CAO Shurui2,3, WANG Guomin2,3, LI Xianliang2,3, ZHANG Lei2,3, ZHANG Yunhuai1   

  1. 1. College of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400030, China;
    2. Chongqing Entry-Exit Inspection and Quarantine Bureau, Chongqing 400020, China;
    3. Chongqing Engineering Technology Research Center of Import and Export Food Safety, Chongqing 400020, China
  • Received:2014-03-24 Revised:2014-05-06 Online:2014-07-08 Published:2014-06-25

摘要:

利用气相色谱检测技术,建立了能应用于白菜、生菜、南瓜、洋葱、番茄、白萝卜、苹果、梨及茶叶等不同基质中16种有机磷农药残留的检测方法。样品采用乙酸乙酯提取,经以合成的介孔氧化铝作吸附剂的固相萃取柱净化,DB-1701毛细管柱分离,气相色谱-火焰光度检测器检测。结果表明,蔬菜、水果及茶叶基质中16种有机磷农药在10~2000 μg/L范围内具有良好的线性关系(R2>0.997);平均回收率为83.2%~103.8%,相对标准偏差为2.0%~9.9%。该方法灵敏度高、准确度高、重复性好,可适用于蔬菜、水果及茶叶基质中16种有机磷残留量的同时测定。

关键词: 茶叶, 固相萃取, 介孔氧化铝, 气相色谱, 蔬菜, 水果, 有机磷农药

Abstract:

A gas chromatographic method based on solid-phase extraction was developed for the simultaneous determination of 16 organophosphorous pesticides in vegetables, fruits and tea, including cabbage, lettuce, pumpkin, onion, tomato, turnip, apple, pear and tea. The samples were extracted with ethyl acetate, and clean-up with mesoporous alumina as solid-phase extraction adsorbent. The separation of target compounds was performed on a DB-1701 capillary column, and the quantitative analysis of the organophosphorous pesticides was carried out by gas chromatography with flame photometric detection. The results showed that the calibration curves of the 16 organophosphorous pesticides were linear in the range of 10-2000 μg/L with good correlation coefficients (R2>0.997). The recoveries of the pesticides in different samples at three spiked levels ranged from 83.2% to 103.8% with the relative standard deviations of 2.0%-9.9%. This method has high sensitivity, high accuracy and good repeatability, and can be applied to the determination of the organophosphorus pesticide residues in vegetables, fruits and tea.

Key words: fruits, gas chromatography (GC), mesoporous alumina, organophosphorous pesticides, solid-phase extraction (SPE), tea, vegetables

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