›› 2011, Vol. 38 ›› Issue (8): 48-52.

• 生物技术 • 上一篇    下一篇

分散固相萃取-气相色谱-质谱方法快速检测奶牛饲料中的3种除草剂残留

石丽丽, 李军国, 李俊, 吕小文, 董颖超, 秦玉昌   

  1. 中国农业科学院饲料研究所,北京 100081
  • 收稿日期:2011-01-05 修回日期:1900-01-01 出版日期:2011-08-20 发布日期:2011-08-20
  • 通讯作者: 秦玉昌

QuEChERS Cleanup and Gas Chromatography-Mass Spectrometry Determination of Three Herbicide Residues in Cattle Feed

SHI Li-li, LI Jun-guo, LI Jun, LV Xiao-wen, DONG Ying-chao, QIN Yu-chang   

  1. Feed Research Institute, Chinese Academy of Agricultural Sciences, Beijing 100081, China
  • Received:2011-01-05 Revised:1900-01-01 Online:2011-08-20 Published:2011-08-20

摘要: 建立了奶牛饲料样品中甲草胺、乙草胺、莠去津3种除草剂的气相色谱-质谱(GC-MS)检测方法,样品经分散固相萃取法处理后,取上清液用安捷伦HP-5气相色谱毛细管柱分离,气相色谱-质谱联用仪进行测定。3 种除草剂在 5~500 μg/kg 内线性关系良好。平均添加回收率为94.5%~115.4%,相对标准偏差(RSD) 为4.4%~9.2%,最低检测限为1.5 μg/kg。本方法前处理操作快速简单,可重复性好,满足国内外对饲料中甲草胺、乙草胺和莠去津的快速、准确的检测要求,适合大量样品的准确定量和定性分析。

关键词: 除草剂; 气相色谱-质谱(GC/MS); 多残留; 奶牛饲料

Abstract: A sensitive gas chromatography-tandem mass spectrometric (GC-MS) method has been developed for simultaneous determination of alachlor, acetochlor and atrazine in feed samples. Three herbicides in feed were extracted and enriched efficiently by using the QuECheRS method.The extraction was separated by capillary column (HP-5MS , 30 m × 0. 25 mm ×0. 25 μm) and detected by GC/MS. The good linearities were obtained for 3 herbicides, and the linear range was 0 to 5 μg/ kg. The recoveries were 94.5% to 115. 4 % for the three herbicides, and the relative standard deviation (RSD) were 4.4 % to 9.2 %.The limit of detection(LOD) for the three herbicides were 1.5 μg/ kg. The method is suitable for quantitative and qualitative analysis of three herbicides in a sufficient number of samples with simplicity, sensitivity and repeatability, and which could meet the request of peptide antibiotic residue testing at home and abroad.

Key words: herbicides; GC/ MS; residue; cattle feed

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