色谱

色谱 ›› 2013, Vol. 31 ›› Issue (2): 117-121.DOI: 10.3724/SP.J.1123.2012.10005

• 研究论文 • 上一篇    下一篇

固相萃取-高效液相色谱-串联质谱联用测定竹笋中残留的7种杀虫剂农药

丁明1,2*, 钟冬莲1, 汤富彬1, 方伟2   

  1. 1. 中国林业科学研究院亚热带林业研究所, 浙江 富阳 311400; 2. 浙江农林大学, 浙江 临安 311300
  • 收稿日期:2012-10-11 修回日期:2012-11-12 出版日期:2013-02-28 发布日期:2013-02-05
  • 通讯作者: 丁明
  • 基金资助:

    国家林业局林业公益性行业科研专项经费(201204414).

Determination of seven pesticide residues in bamboo shoots by high performance liquid chromatography-tandem mass spectrometry coupled with solid-phase extraction

DING Ming1,2*, ZHONG Donglian1, TANG Fubin1, FANG Wei2   

  1. 1. Research Institute of Subtropical Forestry, Chinese Academy of Forestry, Fuyang 311400, China; 2. Zhejiang Agriculture and Forestry University, Lin’an 311300, China
  • Received:2012-10-11 Revised:2012-11-12 Online:2013-02-28 Published:2013-02-05
  • Contact: Ding Ming

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424

被引次数

53

摘要： 建立了高效液相色谱-串联质谱(HPLC-MS/MS)同时测定竹笋中丁烯氟虫腈、毒死蜱、氯虫苯甲酰胺、氟虫腈、吡虫啉、茚虫威和辛硫磷7种农药残留的分析方法。样品用乙腈提取后,经PSA固相萃取小柱净化,采用Atlantis T3色谱柱分离,以0.1%甲酸水溶液(含5 mmol/L乙酸铵)和乙腈为流动相,梯度洗脱分离,在电喷雾离子源正、负离子模式下采用质谱多反应监测(MRM)模式检测。结果表明,7种农药在10～100 μg/L范围内具有良好的线性关系(相关系数r为0.9900～0.9994); 4、8、32 μg/kg添加水平下的平均回收率为76.0%～102.6%;相对标准偏差为3.2%～11.0%;7种农药的检出限为0.02～0.5 μg/kg,定量限为0.08～1.5 μg/kg。该方法准确度、灵敏度高,简单、快速,可满足竹笋中7种杀虫剂残留同时检测的要求。

关键词: 高效液相色谱-串联质谱, 农药残留, 竹笋

Abstract: A simple and efficient method based on solid-phase extraction (SPE) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed for the determination of butylene fipronil, chlorpyrifos, chlorantraniliprole, fipronil, imidacloprid, indoxacarb and phoxim residues in bamboo shoots. The sample was extracted with acetonitrile and purified by a primary secondary amine (PSA) solid-phase extraction cartridge. The detection of targets was performed by HPLC-MS/MS with multiple reaction monitoring (MRM) mode. All the seven pesticides were completely separated in 15 min with an excellent linear relationship. The limits of detection and the limits of quantification for the seven pesticides were 0.02-0.5 μg/kg and 0.08-1.5 μg/kg, respectively. The recoveries of the seven pesticides spiked in a bamboo shoot sample at the levels of 4, 8, 32 μg/kg were in the range from 76.0% to 102.6% (the RSD≤11.0%, n=3). The method was successfully applied to the real bamboo shoot samples. The method has high accuracy and sensitivity, and is simple and quick. It can meet the requirement of the simultaneous determination of the seven pesticides in bamboo shoots.

Key words: bamboo shoots, pesticide residues, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)