色谱

色谱 ›› 2012, Vol. 30 ›› Issue (06): 555-559.DOI: 10.3724/SP.J.1123.2012.01034

• 研究论文 • 上一篇    下一篇

液相色谱-串联质谱法测定黄瓜和苹果中氟啶虫酰胺及其代谢产物残留量

陈国, 孙亚米, 杨挺, 吴银良*   

  1. 宁波市农业科学研究院, 浙江 宁波 315040
  • 收稿日期:2012-01-20 修回日期:2012-03-19 出版日期:2012-06-28 发布日期:2012-06-20
  • 通讯作者: 吴银良,博士,高级工程师,研究方向为农兽药残留分析. Tel: (0574)87928060, E-mail: wupaddyfield@tom.com.
  • 基金资助:

    宁波市自然科学基金项目(No. 2009A610183)和宁波市农业攻关项目(No. 2010C10029和2010C10026).

Simultaneous determination of flonicamid and its metabolites in cucumbers and apples by liquid chromatography-tandem mass spectrometry

CHEN Guo, SUN Yami, YANG Ting, WU Yinliang*   

  1. Ningbo Academy of Agricultural Science, Ningbo 315040, China
  • Received:2012-01-20 Revised:2012-03-19 Online:2012-06-28 Published:2012-06-20

PDF

329

被引次数

12

摘要： 建立了黄瓜和苹果中氟啶虫酰胺及其3种代谢产物［N-(4-trifluoromethylnicotinoyl)glycine(TFNG)、4-tri-fluoromethylnicotinic acid(TFNA)和4-trifluoromethylnicotinamide(TFNA-AM)］同时测定的液相色谱-串联质谱分析方法。样品用磷酸盐缓冲液提取两次,调节pH值至1.5～2.0后,再用乙酸乙酯提取,液相色谱-串联质谱分析。采用Acquity BEH C18色谱柱分离,0.1%甲酸水-甲醇作为流动相进行梯度洗脱,电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测,外标法定量。氟啶虫酰胺、TFNG、TFNA和TFNA-AM的检出限分别为0.17、0.20、0.35和0.60 μg/kg。在黄瓜和苹果样品中添加5.0～2000 μg/kg水平的氟啶虫酰胺、TFNG、TFNA和TFNA-AM,其平均添加回收率在82.9%～104.1%范围内,批内分析相对标准偏差(RSD)在3.6%～6.9%之间。4种物质的峰面积与其浓度在0.50～200 μg/L范围内均呈良好的线性关系,线性回归系数均大于0.998。前处理步骤仅用有机溶剂6 mL。整个方法具有高灵敏度、准确、稳定的特点。

关键词: 残留分析, 代谢产物, 氟啶虫酰胺, 黄瓜, 苹果, 液相色谱-串联质谱

Abstract: A method was developed for the simultaneous determination of flonicamid and its metabolite ［N-(4-trifluoromethylnicotinoyl)glycine (TFNG), 4-trifluoromethylnicotinic acid (TFNA) and 4-trifluoromethylnicotinamide (TFNA-AM)］ in cucumbers and apples by liquid chromatography-tandem mass spectrometry (LC-MS/MS) with liquid-liquid extraction. The sample was extracted twice with phosphate buffer solution (pH 7.0), and the extract was adjusted to pH 1.5-2.0, then an aliquot of the extract (3 mL) was extracted with ethyl acetate. The final extract was dried under nitrogen and the residue was dissolved in 0.1% formic acid in water/methanol (80/20, v/v). The sample was analyzed by LC-MS/MS and quantified with the external standard calibration curve method. The detection limits of flonicamid, TFNG, TFNA and TFNA-AM were 0.17, 0.20, 0.35 and 0.60 μg/kg, respectively. The average recoveries of flonicamid and its metabolites in cucumbers and apples were 82.9%-104.1%. In the intra-assay, the relative standard deviations were 3.6%-6.9% at the spiked levels of 5.0-2000 μg/kg. There were good linear correlations (the calibration coefficients were above 0.998) between the peak areas and the concentrations of flonicamid and its metabolites in the range of 0.5-200 μg/L. The volume of organic solvent used in the whole pretreatment procedure was only 6 mL. The method is accurate, highly sensitive and stable for the determination of flonicamid and its metabolites.

Key words: apples, cucumbers, flonicamid, metabolite, residue analysis, liquid chromatography-tandem mass spectrometry (LC-MS/MS)