食品科学 ›› 2009, Vol. 30 ›› Issue (14): 215-218.doi: 10.7506/spkx1002-6630-200914045

• 分析检测 • 上一篇    下一篇

谷物中15种除草剂多残留检测方法的建立及应用

田宏哲,周艳明,刘朋宇,陈 柏   

  1. 沈阳农业大学分析测试中心
  • 收稿日期:2008-11-28 修回日期:2009-01-15 出版日期:2009-07-15 发布日期:2010-12-29
  • 通讯作者: 田宏哲 E-mail:tthz2@yahoo.com.cn

Development and Application of Multi-residue Analysis of 15 Herbicides in Grains

TIAN Hong-zhe,ZHOU Yan-ming,LIU Peng-yu,CHEN Bai   

  1. (Analysis and Testing Center, Shenyang Agricultrual University, Shenyang 110161, China)
  • Received:2008-11-28 Revised:2009-01-15 Online:2009-07-15 Published:2010-12-29
  • Contact: TIAN Hong-zhe E-mail:tthz2@yahoo.com.cn

摘要:

采用高效液相色谱- 离子阱质谱建立同时测定谷物中15 种除草剂残留量的方法。样品经乙腈提取,氟罗里硅土固相萃取柱净化,然后采用HPLC-ESI-MS/MS 进行测定。15 种除草剂在0.01~10mg/kg 范围内呈良好线性,相关系数为0.9834~0.9997。15 种除草剂的定量限为0.002~0.07mg/kg,平均加标回收率为74.44%~115.56%,相对标准偏差为0.37%~13.79%。采用本实验所建立的方法对市售谷物样品进行测定,确定了其中所存在的除草剂残留量。

关键词: 除草剂, 多残留分析, 谷物

Abstract:

This study developed a specific high-performance liquid chromatography-electrospray ionization ion trap mass spectrometric (HPLC-ESI-MS/MS) method that allowed simultaneous determination of 15 herbicide multi-residues in grain samples. Residues of the herbicides were extracted from grains with acetonitrile, cleaned up using florisil-SPE, and then determined by HPLC-ESI-MS/MS. The method showed high degree of linearity (the correlation coefficients were 0.9834-0.9997) over the range of 0.01-10 mg/kg for the analytes. The limit of quantifications ranged from 0.002 to 0.07 mg/kg. The average recoveries for the herbicides in spiked samples were between 74.44% and 115.56% with a relative standard deviations from 0.37% to 13.79%. The method developed was applied to detect the targets in real samples, and several herbicide residues were identified.

Key words: herbicide, multi-residue analysis, grain

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