食品科学 ›› 2014, Vol. 35 ›› Issue (4): 111-115.doi: 10.7506/spkx1002-6630-201404023

• 分析检测 • 上一篇    下一篇

超高效液相色谱-串联质谱结合QuEChERS方法快速检测柑橘中的残留苯丁锡

朱艳梅1,2,赵其阳1,陈卫军1,焦必宁1,2,3,*,张耀海1   

  1. 1.农业部柑桔产品质量安全风险评估实验室(重庆),西南大学柑桔研究所,重庆 400712;2.西南大学食品科学学院,
    重庆 400715;3.国家柑桔工程技术研究中心,中国农业科学院柑桔研究所,重庆 400712
  • 收稿日期:2013-05-01 修回日期:2014-01-06 出版日期:2014-02-25 发布日期:2014-03-17
  • 通讯作者: 焦必宁 E-mail:bljiao@tom.com
  • 基金资助:

    国家现代农业(柑橘)产业技术体系建设专项(CARS-27);农业部农药检定所残留项目(2012P303)

Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry Combined with QuEChERS for the Quick Detection of Fenbutatin Oxide Residue in Citrus

ZHU Yan-mei1,2, ZHAO Qi-yang1, CHEN Wei-jun1, JIAO Bi-ning1,2,3,*, ZHANG Yao-hai1   

  1. 1. Laboratory of Quality and Safety Risk Assessment for Citrus Products (Chongqing), Ministry of Agriculture, Citrus Research
    Institute, Southwest University, Chongqing 400712, China; 2. College of Food Science, Southwest University,
    Chongqing 400715, China; 3. National Citrus Engineering Research Center, Citrus Research Institute, Chinese Academy of
    Agricultural Sciences, Chongqing 400712, China
  • Received:2013-05-01 Revised:2014-01-06 Online:2014-02-25 Published:2014-03-17
  • Contact: Bining Jiao E-mail:bljiao@tom.com

摘要:

采用改进的QuEChERS方法结合超高效液相色谱-串联四极杆质谱仪,建立快速检测柑橘中残留苯丁锡的方法。样品经乙腈提取、无水MgSO4和NaCl脱水盐析、十八烷基硅胶键合相分散萃取净化,采用BEH C18液相色谱柱分离(2.1 mm×50 mm),等度洗脱,在多反应监测模式下测定,基质匹配标准溶液外标法定量。结果表明:在0.001~1.0 mg/L范围内,苯丁锡含量与峰面积具有良好的线性关系,R2≥0.993 0;方法定量限为2.0 μg/kg;在方法线性范围内,柑橘果肉、果皮和全果中低、中、高3 个添加水平的平均回收率为74.0%~97.7%,相对标准偏差为2.5%~6.9%。该方法操作简单、快速、成本低、环境友好、安全、精确度高,能满足柑橘中痕量苯丁锡残留的快速确证和定量检测要求。

关键词: QuEChERS, 超高效液相色谱-串联质谱, 柑橘, 苯丁锡

Abstract:

The fenbutatin oxide residue in citrus fruits was detected by optimized QuEChERS combined with ultraperformance
liquid chromatography-tandem mass spectrometry (UPLC-MS-MS). Fenbutatin oxide was extracted from the
samples with acetonitrile, salted out with anhydrous MgSO4 and NaCl, cleaned up with octadecyl bonded phase silica gel
and then analyzed by UPLC-MS-MS in multiple reaction monitoring (MRM) mode. The separation of the target pesticide
residue was performed on an BEH C18 column (2.1 mm×50 mm) using a mobile phase consisting of 0.1% formic acidmethanol
by isocratic elution and the matrix-matched external standard calibration was used for quantitation. There was a
linear relation between fenbutatin oxide content and peak area in the range of 0.001–1.0 mg/L (R2 ≥ 0.993 0), and the limit
of quantitation was 2.0 μg/kg. The average recoveries in different matrices (citrus pulp, peel and whole fruits) at three spiked
concentration levels ranged from 74.0% to 97.7% with relative standard deviations (RSDs) of 2.5%–6.9%. This method was
simple, quick, cheap, environmentally friendly and safe. The accuracy and precision could meet the requirements for quick
confirmation and quantitative determination of trace fenbutatin oxide residue in citrus fruits.

Key words: QuEChERS, ultra-performance liquid chromatography-tandem mass spectrometry, citrus, fenbutatin oxide

中图分类号: