食品科学

• 安全检测 • 上一篇    下一篇

气相色谱-质谱联用结合QuEChERS法快速筛查大米中多种农药残留

邱伟芬1,张昌娟1,文 良2,方 勇1,胡秋辉1   

  1. 1.南京财经大学食品科学与工程学院,江苏省现代粮食流通与安全协同创新中心,
    江苏高校粮油质量安全控制及深加工重点实验室,江苏 南京 210023;2.深圳出入境检验检疫局,广东 深圳 518045
  • 出版日期:2015-06-25 发布日期:2015-06-12
  • 基金资助:

    江苏高校优势学科建设工程资助项目(PAPD);
    农产品中化学风险物高速分析检测系统的引进及其创新应用项目(农业部948项目;2015-Z47)

Rapid Determination of Pesticide Multi-Residues in Rice by QuEChERS and GC-MS

QIU Weifen1, ZHANG Changjuan1, WEN Liang2, FANG Yong1, HU Qiuhui1   

  1. 1. Collaborative Innovation Center for Modern Grain Circulation and Safety, Key Laboratory of Grains and Oils Quality Control and
    Processing, College of Food Science and Engineering, Nanjing University of Finance and Economics, Nanjing 210023, China;
    2. Shenzhen Entry-Exit Inspection and Quarantine Bureau, Shenzhen 518045, China
  • Online:2015-06-25 Published:2015-06-12

摘要:

采用QuEChERS方法结合气相色谱-质谱联用建立大米中是否存在敌敌畏、草灭达、氧化乐果、五氯硝基苯、敌稗、甲基毒死蜱、杀螟硫磷、甲基吡啶磷、马拉硫磷、毒死蜱、稻丰散、腐霉利、丁草胺、稻瘟灵、三唑磷、联苯菊酯和溴氰菊酯17 种农药的快速筛查方法。样品采用体积分数1%冰乙酸-乙腈提取、无水硫酸镁与氯化钠盐析,经N-丙基乙二胺和十八烷基键合硅胶净化,气相色谱-质谱检测,NAGINATA™软件分析。结果表明:17 种农药在大米中检出限为0.002~0.050 mg/kg。在0.05、0.10 mg/kg和0.20 mg/kg添加水平的平均回收率为80%~110%,相对标准偏差为1.7%~12.3%。该方法耗时短,操作便捷、快速且可靠,适合大米中多种农药残留的快速筛查。采用本方法对25 份大米样品进行测定,检测出毒死蜱、三唑磷和稻瘟灵3 种农药残留,残留量均显著低于GB 2763—2014《食品中农药最大残留限量》规定的限量标准。

关键词: QuEChERS, 气相色谱-质谱联用, NAGINATA&trade, 软件, 农药残留

Abstract:

The combination of QuEChERS and gas chromatography-mass spectrometry (GC-MS) was employed to establish
a new method for the rapid screening 17 pesticide residues in rice, including dichlorvos, molinate, omethoate, quintozene,
propanil, chlorpyrifos-methyl, fenitrothion, pirimiphos-methyl, malathion, chlorpyrifos, phenthoate, procymidone, butachlor,
isoprothiolane, triazophos, bifenthrin and deltamethrin. Samples were extracted with a mixture of acetonitrile/acetic acid (99:1,
V/V) and salted out with anhydrous MgSO4 and NaCl. After the incorporation of N-propyl ethylenediamine (PSA) and C18 sorbent
for the purification process, GC-MS and NAGINATA™ software were used for the detection and analysis, respectively. The results
showed that the limits of detection (LOD) of the 17 pesticide residues using the established method were in the range of 0.002–
0.050 mg/kg, and their average recovery rates in a blank sample were 80%–110% with relative standard deviations (RSDs) of
1.7%–12.3%. This method was sensitive without the need for any complicated pre-treatments or expensive equipment and was
suitable for the fast screening of pesticide residues in rice. Finally, we adopted the new method to detect pesticide residues in
25 rice samples. The results showed that 3 pesticides including chlorpyrifos, triazophos and isoprothiolane were analyzed, and their
levels were lower than the MRL stipulated by the national standard of China (GB 2763—2014).

Key words: QuEchERS, gas chromatography-mass spectrometry (GC-MS), NAGINATA&trade, software, pesticide residues

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