食品科学 ›› 2006, Vol. 27 ›› Issue (11): 449-454.

• 分析检测 • 上一篇    下一篇

蔬菜中有机磷农药多残留分析:方法检出限的对比研究

 蔡潞莎,  胡奇,  芮三亚   

  1. 南京市农产品质量监督检验站
  • 出版日期:2006-11-15 发布日期:2011-11-28

Comparative Study on Different Defined Method Detection Limits for Multi-organophorous Pesticide Residues Analysis in Vegetables

 CAI  Lu-Sha,   Hu-Qi,   Rui-San-Ya   

  1. Nanjing Quality Surveillance and Testing Station for Agriculture Products,Nanjing 210036,China
  • Online:2006-11-15 Published:2011-11-28

摘要:  对甲胺磷、乙酰甲胺磷、乐果、甲基对硫磷、毒死蜱等有机磷农药在蔬菜中的多残留分析的三种不同定义的方法检出限(即简单的信噪比法,EPA法和欧盟与IUPAC推荐的校正曲线法(Ccα)进行了比较研究:给出了不同定义的方法检出限的详细的估算步骤;提供了本方法中上述各种农药的不同定义的方法检出限的数据,并对这些数据进行了比较与讨论;提出了应当根据不同的目的,采用不同定义的方法的检出限对方法进行合理的验证和评价,以期经济实用并能与国际上的有关法规规定进行有现实意义的接轨比较。结果表明:在加标水平为0.1和0.5mg/kg时,本文方法的各有关农药的平均回收率在70%~120%之间,相对标准偏差在13%以内。本文方法中甲胺磷、乙酰甲胺磷、乐果、甲基对硫磷、毒死蜱的二倍信噪比法的试剂空白和青菜基质的检出限分别为0.007、0.007、0.002、0.003、0.002和0.01、0.009、0.009、0.009、0.008mg/kg,美国EPA定义的检出限(青菜基质)分别为0.01、0.01、0.01、0.01、0.009mg/kg,欧盟和IUPAC推荐的校正曲线法的检出限(Ccα,青菜基质)分别为0.02、0.02、0.02、0.02、0.01mg/kg。结果还表明:本文方法的Ccα能够满足最近欧盟EU2003/118/EC对有关农残规定的严格要求。

关键词: 有机磷农药, 蔬菜农药多残留分析, 检出限, 乙酰甲胺磷, 甲基对硫磷

Abstract:  A comparative study was made on three different defined method detection limits ( MDL or LOD ),i.e. simple signal to noise ratio,EPA,and EU/IUPAC(Ccα) methods,for the determination of multi-organophorous pesticides residues such as methamidaphos,acephate,dimethoate,methyl parathion and chlorpyrifos in vegetables. Detailed estimation procedures,group data for various defined“ Method Detection Limit” and brief comments and discussion on each method are given. It is suggested that an appropriate defined method detection limit for method validation and evaluation should be chosen according to the objective of the determination so as to achieve the best economics and reasonable comparison with related international regulations. The results from this study show that an average recovery of 70%~120% with relative standard deviation less than 13% is achieved for the spiking levels of 0.1mg/kg to 0.5mg/kg. For methamidaphos,acephate,dimethoate,methyl parathion and chloryrifos,the method detection limit (MDL) or limit of detection (LOD) for this method as defined by two times signal to noise ratio in reagent blank and in Chinese cabbage matrix is 0.007,0.007,0.002,0.003,0.002 and 0.01,0.009,0.009,0.009,0.008mg/kg,respectively,or by EPA(in Chinese cabbage matrix) is 0.01,0.01,0.01,0.01,0.009mg/kg,and the Ccα as defined by EU and IUPAC(in Chinese cabbage matrix) is 0.02,0.02,0.02,0.02,0.01mg/kg,respectively. The results also show that the Ccα for various pesticide residues in this work could satisfy the more severe demands set by EU 2003/118/EC.