气相色谱-三重四级杆串联质谱法确证姜中120种农药残留量

Multi residue Simultaneous determination study of 120 Pesticides in Ginger by Gas Chromatography-tandem mass Spectrometry

【目的】拟建立姜中120种农药同时检测的气相色谱三重四级杆串联质谱的确证方法。【方法】根据基质和农药性质，考察了提取条件和净化方法，优化仪器条件，选择乙腈-乙酸乙酯为提取溶剂，全自动凝胶渗透色谱技术为净化手段，选择多反应监测模式，内标法定量的检测方法。【结果】在0．01-5．0mg／L的范围内，各农药相关系数均大于0．993，添加水平0．002-0．5mg／kg范围内，回收率为69．6％-133．4％，相对标准偏差为4．15％-29．26％。【结论】方法准确性、灵敏度高，适用于姜中农药的多残留检测。

[Aims] One method of simultaneous determining 120 pesticides in ginger by gas chromatography-tandem mass spectrometry was planed to be developed. [Methods] According to the properties of matrices and pesticides, the sample extraction condition, cleanup methods and instrument condition were systematically considered. The finally developed method was that the sample was extracted with acetonitrile-ethyl acetate, and cleaned up by automatic gel permeation chromatography, monitored by the multi reaction monitor, and confirmed with internal standard method. [Results] In the linear range （0.01-5.0 mg/L） of each pesticide, the correlation coefficient was greater than 0.993 for each pesticide. In the range of 0.002-0.5 mg/kg, the corresponding recoveries were 69.6-133.4%, the relative standard deviations were 4.15- 29.26%. [Conclusions] The method was accurate and sensitive, which could be applied to determine multiple pesticides residues in gingers.