Qu Li, Li You, Zeng Jing, Sheng Yonggang, Yi Xionghai, Cheng Jia
Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China; Fudan University, Shanghai 200032, China.
Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China.
Se Pu. 2017 Jul 8;35(7):778-784. doi: 10.3724/SP.J.1123.2017.01012.
A method of gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed for the simultaneous determination of 20 pyrethroid residues in vegetable foods. The samples were extracted by acetone--hexane (1:1, v/v), cleaned up by activated charcoal column and quantified by external standard method. The correlation coefficients () of all the 20 pyrethroid pesticides in the range of 0.005-1.0 mg/L were not less than 0.990. The limits of detection (LODs) were 2.0 μ g/kg when signal/noise () > 3. The limits of quantification (LOQs) were 5.0 μ g/kg ( > 10). For recovery test, there were three levels (low, medium and high) spiked in 11 matrices. The average recoveries of the method were 75.2%-107% and the relative standard deviations (RSDs, =6) were 3.08%-12.1%. The results demonstrated that the method is simple and has specific pretreatment steps. The method is suitable for the screening and confirmation of the 20 pyrethroid pesticides in vegetable foods.
建立了一种气相色谱 - 串联质谱法(GC-MS/MS)同时测定蔬菜类食品中20种拟除虫菊酯类农药残留。样品用丙酮 - 正己烷(1:1,v/v)提取,经活性炭柱净化,采用外标法定量。20种拟除虫菊酯类农药在0.005 - 1.0 mg/L范围内的相关系数()均不小于0.990。当信噪比()> 3时,检测限(LOD)为2.0 μg/kg。定量限(LOQ)为5.0 μg/kg(> 10)。在回收率试验中,在11种基质中添加了三个水平(低、中、高)。该方法的平均回收率为75.2% - 107%,相对标准偏差(RSD,=6)为3.08% - 12.1%。结果表明,该方法操作简便,具有特定的预处理步骤。该方法适用于蔬菜类食品中20种拟除虫菊酯类农药的筛查和确证。