Ma Zhiling, Zhao Wen, Li Lingyun, Zheng Shuning, Lin Huan, Zhang Yanguo, Gao Qingzhen, Liu Su
Institute of Vegetables and Flowers, Chinese Academy of Agricultural Sciences, Supervision and Testing Center for Vegetable Quality, Ministry of Agriculture, Beijing 100081, China.
Se Pu. 2013 Mar;31(3):228-39. doi: 10.3724/sp.j.1123.2012.10029.
An analytical method for the simultaneous determination of 129 pesticides in vegetables and fruits was established based on optimized QuEChERS with gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). The samples were extracted with acetonitrile (containing 1% (v/v) acetic acid), then the extracts were determined by GC-MS/MS in multireaction monitoring (MRM) mode after being cleaned up with mixed solid-phase dispersion, and the external standard method was applied to quantify the pesticides. The results showed that all the 129 pesticides had good linearity in certain ranges with the correlation coefficients ( r2) higher than 0. 98. The average recoveries of the most of 129 pesticides in different matrices were in the range of 66.2% - 124.7% at the spiked level of 10 micro g/kg, with relative standard deviations (RSDs) of 0.9% - 24.4%. The limits of quantification (LOQs) of the method were 0.03 - 16.7 micro g/kg. The results demonstrated that the developed method is simple, rapid, sensitive and high efficient for screening multiple pesticide residues in vegetables and fruits.
基于优化的QuEChERS结合气相色谱-三重四极杆质谱联用仪(GC-MS/MS),建立了同时测定蔬菜和水果中129种农药的分析方法。样品用乙腈(含1%(v/v)乙酸)提取,提取液经混合固相分散净化后,采用GC-MS/MS在多反应监测(MRM)模式下进行测定,采用外标法对农药进行定量。结果表明,129种农药在一定范围内均具有良好的线性关系,相关系数(r2)均高于0.98。在10 μg/kg的加标水平下,129种农药中大多数在不同基质中的平均回收率为66.2% - 124.7%,相对标准偏差(RSD)为0.9% - 24.4%。该方法的定量限(LOQ)为0.03 - 16.7 μg/kg。结果表明,所建立的方法用于蔬菜和水果中多种农药残留的筛查具有简便、快速、灵敏和高效的特点。