色谱

色谱 ›› 2014, Vol. 32 ›› Issue (3): 314-317.DOI: 10.3724/SP.J.1123.2013.12013

• 技术与应用 • 上一篇    

气相色谱-负化学源质谱联用法测定水产品及食用油中氟乐灵的残留量

王莉1, 夏广辉2,3, 沈伟健2, 吴斌2, 张睿2, 陆慧媛2, 沈崇钰2, 赵增运2   

  1. 1. 江苏省泰州市姜堰区疾病预防控制中心, 江苏 泰州 225500;
    2. 江苏出入境检验检疫局食品实验室, 江苏 南京 210001;
    3. 中国药科大学生物化学教研室, 江苏 南京 210000
  • 收稿日期:2013-12-12 修回日期:2014-01-13 出版日期:2014-03-08 发布日期:2014-03-04
  • 通讯作者: 沈伟健
  • 基金资助:

    国家质检总局科技计划项目（2011KJ39，2012KJ31）；科技部科技支撑项目（2011BAK10B04）.

Determination of trifluralin residue in aquatic products and edible oils by gas chromatography-negative chemical ionization mass spectrometry

WANG Li1, XIA Guanghui2,3, SHEN Weijian2, WU Bin2, ZHANG Rui2, LU Huiyuan2, SHEN Chongyu2, ZHAO Zengyun2   

  1. 1. Jiangyan District Disease Prevention and Control Center of Taizhou City of Jiangsu Province, Taizhou 225500, China;
    2. Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China;
    3. Department of Biochemistry, China Pharmaceutical University, Nanjing 210000, China
  • Received:2013-12-12 Revised:2014-01-13 Online:2014-03-08 Published:2014-03-04

PDF

307

被引次数

16

摘要：

建立了一种可用于水产品及食用油中氟乐灵残留量分析的分散型固相萃取-气相色谱-负化学离子源质谱方法。水产品及食用油经乙腈提取，4 ℃冷藏后，采用分散型固相萃取法净化，由气相色谱-负化学离子源质谱选择离子监测技术进行测定与确证，同位素内标法定量。在1~40 μg/L范围内氟乐灵农药的线性关系良好；方法定量限（LOQ）为0.02 μg/kg；对鳗鱼、烤鳗、梭子蟹、小龙虾、猪油和橄榄油等6种复杂基质进行1.0、2.0和3.0 μg/kg等3个水平的添加回收试验，平均回收率均处于80%~100%之间，RSD≤10.3%；无干扰现象出现。该方法可作为水产品及食用油中氟乐灵残留检测的确证方法。

关键词: 分散型固相萃取, 氟乐灵, 气相色谱-负化学离子源质谱联用, 食用油, 水产品, 选择离子监测

Abstract:

A confirmatory method was established for the determination of trifluralin residue in aquatic products and edible oils with the technique of offline disperse solid phase extraction and gas chromatography-negative chemical ionization mass spectrometry (DSPE-GC-MS/NCI). Trifluralin was extracted from aquatic products and edible oils with acetonitrile, and liquid-liquid partitioning formed by adding anhydrous magnesium sulfate followed by a simple cleanup step known as dispersive solid-phase extraction. The aliquot was analyzed by GC-MS/NCI using isotope internal standard method. The method was reliable and stable. The recoveries of trifluralin were in the range from 80% to 100% at three spiked levels of 1.0, 2.0, and 3.0 μg/kg, and the RSDs were not more than 10.3%. The linearity of method was good from 1 to 40 μg/L, and the LOD was 0.02 μg/kg. This method can be used as a conclusive evidence method for the determination of trifluralin residue in aquatic products and edible oils.

Key words: aquatic products, disperse solid phase extraction (DSPE), edible oils, gas chromatography-negative chemical ionization mass spectrometry (GC-MS/NCI), selected ion monitoring (SIM), trifluralin

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