色谱

色谱 ›› 2015, Vol. 33 ›› Issue (10): 1019-1025.DOI: 10.3724/SP.J.1123.2015.05013

• 研究论文 • 上一篇    下一篇

固相萃取-超高效液相色谱-串联质谱法同时测定果蔬中6种酰胺类农药残留量

马琳, 陈建波, 赵莉, 占绣萍   

  1. 上海市农业技术推广服务中心, 农业部农药质量监督检验测试中心(上海), 上海 201103
  • 收稿日期:2015-05-21 出版日期:2015-10-08 发布日期:2012-05-09
  • 通讯作者: 赵莉
  • 基金资助:

    上海市农委科技攻关项目(沪农科攻字(2015)第4-6号).

Determination of six amide pesticide residues in vegetables and fruits by solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry

MA Lin, CHEN Jianbo, ZHAO Li, ZHAN Xiuping   

  1. Shanghai Agriculture Technology Extension & Service Centre, Pesticide Quality Supervision and Inspection Testing Centre (Shanghai), Ministry of Agriculture, Shanghai 201103, China
  • Received:2015-05-21 Online:2015-10-08 Published:2012-05-09

PDF

127

被引次数

31

摘要：

建立了同时测定果蔬中6种酰胺类农药的固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)方法。样品经乙腈高速匀浆提取、Florisil固相萃取柱净化,采用超高效液相色谱-串联质谱法测定6种农药。质谱分析采用电喷雾电离,正负双离子扫描,多反应监测(MRM)模式。结果表明:6种农药在0.0005~1.00 mg/L范围内均呈现良好的线性关系,相关系数均大于0.999;在0.01、0.1和1.0 mg/kg(氟苯虫酰胺为0.001、0.01和0.1 mg/kg) 3个浓度添加水平下的平均回收率为72.4%~119.4%,相对标准偏差(n=5)小于15%;定量限为0.01 mg/kg(溴氰虫酰胺、双炔酰菌胺、啶酰菌胺、氟吡菌胺和噻呋酰胺)和0.001 mg/kg(氟苯虫酰胺)。该方法简单、快速、重现性好、灵敏度高,可满足果蔬中6种酰胺类农药残留检测的要求。

关键词: 残留, 超高效液相色谱-串联质谱, 固相萃取, 蔬菜, 水果, 酰胺类农药

Abstract:

A solid phase extraction coupled with ultra high performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS) method was developed for simultaneous determination of six amide pesticides, cyantraniliprole, mandipropamid, boscalid, fluopicolide, thifluzamide and flubendiamide, in vegetables and fruits. After extraction with acetonitrile, purification with Florisil SPE cartridges and dissolution with methanol, the targets in the sample solutions were analyzed by UPLC-MS/MS on an Agilent Proshell 120 EC-C18 column with a mixture of 0.1% formic acid solution and methanol as the mobile phases under gradient elution conditions. The mass spectrometer operated in multiple reaction monitoring (MRM) mode with the negative and positive modes. Good linearity was obtained for the six amide pesticides at the mass concentrations of 0.0005-1.00mg/L with the correlation coefficients more than 0.999. The fortified recoveries were in the range of 72.4%-119.4% with the concentration levels at 0.01, 0.1 and 1.0 mg/kg for cyantraniliprole, mandipropamid, boscalid, fluopicolide, thifluzamide, and 0.001, 0.01 and 0.1 mg/kg for flubendiamide. The relative standard deviations (RSDs) were less than 15% and the limits of quantification were 0.01 mg/kg for cyantraniliprole, mandipropamid, boscalid, fluopicolide, thifluzamide, and 0.001 mg/kg for flubendiamide. All the above observations indicate that the established analytical method is simple, efficient and sensitive, and suitable for the determination of the six amide pesticides in vegetables and fruits.

Key words: amide pesticides, fruits, residues, solid phase extraction (SPE), ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), vegetables

中图分类号: