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通过比较d-SPE(PSA+GCB)、SPE(NH2-Carb柱)和SPE(GCB/PSA柱)3种前处理方法的净化效果及方法稳定性,选取了GCB/PSA柱固相萃取作为净化方法。样品经前处理后,采用大体积进样,气相色谱-串联质谱测定,内标法定量。124种农药在浓度为0.010～0.200 mg/kg范围内与峰面积呈线性关系,相关系数均大于0.9800,以10倍信噪比计算,定量限在0.1～19.0μg/kg之间。当农药在样品中添加水平为0.040 mg/kg时,124种农药平均回收率(n=5)为80.0～130.7%,RSD为1.1～2.0%。
The GCB / PSA column solid-phase extraction was selected as the purification by comparing the purification efficiency and the method stability of the three pre-treatment methods: d-SPE (PSA + GCB), SPE (NH2- Carb column) and SPE (GCB / PSA column) method. Samples after pretreatment, the use of large-volume injection, gas chromatography-tandem mass spectrometry, internal standard method. 124 pesticides showed a linear relationship with the peak area in the range of 0.010 ~ 0.200 mg / kg, the correlation coefficients were all greater than 0.9800, and the limit of quantification was between 0.1 ~ 19.0μg / kg with 10 times signal to noise ratio. When the pesticide was added to the sample at a level of 0.040 mg / kg, the average recoveries of 124 pesticides (n = 5) were 80.0 to 130.7% with RSDs of 1.1 to 2.0%.