食品科学 ›› 2011, Vol. 32 ›› Issue (18): 296-299.doi: 10.7506/spkx1002-6630-201118066

• 分析检测 • 上一篇    下一篇

高效液相色谱串联质谱法测定蔬菜中苯醚甲环唑的残留量

王 远,邢丽杰,郝家勇,鲁立良,唐宗贵,罗小玲*   

  1. 新疆农垦科学院,农业部食品质量安全监督检验测试中心
  • 出版日期:2011-09-25 发布日期:2011-09-24
  • 基金资助:
    新疆生产建设兵团科技支疆项目(2009ZJ16)

Determination of Difenoconazole Residues in Vegetables by HPLC-MS/MS

WANG Yuan,XING Li-jie,HAO Jia-yong,LU Li-liang,TANG Zong-gui,LUO Xiao-ling*   

  1. (Food Quality Supervision and Testing Center of Ministry of Agriculture, Xinjiang Academy of Agricultural Reclamation Science, Shihezi 832000, China)
  • Online:2011-09-25 Published:2011-09-24

摘要: 建立高效液相色谱-串联质谱检测蔬菜中苯醚甲环唑残留的分析方法。样品采用乙腈提取,经石墨碳黑-氨基串联固相萃取(GCB/NH2 SPE)柱净化,液相色谱分离多反应监测模式下测定,外标法定量。结果显示:苯醚甲环唑质量浓度在1~500ng/mL范围内线性关系良好。苯醚甲环唑在不同基质中平均回收率为79.3%~108.0%,相对标准偏差为2.7%~8.5%,检出限为0.001mg/kg。该方法灵敏度高,准确度、精密度好,满足样品测定的定性、定量要求。

关键词: 苯醚甲环唑, 液相色谱-串联质谱, 蔬菜, 固相萃取

Abstract: A method was established to determine difenoconazole residues in vegetables by high performance liquid chromatography-mass/mass (HPLC-MS/MS). Difenoconazole residues were extracted from vegetables by acetonitrile and cleaned up by carbon/amino solid phase extraction (GCB/NH2-SPE) cartridge. The chromatographic separation was achieved by HPLC and the determination was performed by tandem mass spectrometry in a multiple reaction-monitoring mode. The external standard method was used for the quantification of difenoconazole. A good linear relationship was established in the difenoconazole concentration range of 1-500 ng/mL. The recovery rates of difenoconazole from different spiked samples were in the range of 79.3%-108.0% with relative standard deviations (RSD) of 2.7%-8.5% and the limit of detection for difenoconazole was 0.001 mg/kg. Therefore, the developed method can be used to qualitatively and quantitatively analyze difenoconazole residues in vegetables with satisfactory sensitivity, accuracy and precision.

Key words: difenoconazole, high performance liquid chromatography-mass/mass (HPLC-MS/MS), vegetables, solid phase extraction (SPE)

中图分类号: