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采用气相色谱法-质谱联用技术和固相萃取前处理方法,建立了甲基毒死蜱农药残留的检测方法。样品采用乙腈萃取目标组分,经固相萃取柱净化,并由HP-5MS柱(30m×0.25mm×0.25μm)进行分离,利用选择性离子监测(SIM)的方式,内标法定量。分别对小米、大米、高粱、小麦、玉米、燕麦、大麦七种样品进行0.0125mg/kg(检出限)、0.0375mg/kg、0.0625mg/kg、0.125mg/kg四个水平的加标回收试验,回收率均在85.3~104.2%之间,RSD均在0.9~5.0之间。试验证明该方法稳定可靠,样品前处理方法更加简单,分析时间短,灵敏度和准确度高,可以满足甲基毒死蜱农药残留分析的要求。
Gas chromatography-mass spectrometry and solid-phase extraction pretreatment methods were used to establish a method for the determination of pesticide residues in methyl chlorpyrifos. The sample was extracted with acetonitrile and purified by solid phase extraction (SPE). The sample was separated on a HP-5MS column (30 × 0.25 × 0.25 μm) and quantified by internal standard method using selective ion monitoring (SIM). Seven spiked samples of millet, rice, sorghum, wheat, corn, oats and barley were spiked at the four levels of 0.0125mg / kg (detection limit), 0.0375mg / kg, 0.0625mg / kg and 0.125mg / kg respectively Test, recovery rates were between 85.3 ~ 104.2%, RSD were between 0.9 ~ 5.0. The test proves that the method is stable and reliable, the sample pretreatment method is simple, the analysis time is short, the sensitivity and accuracy are high, which can meet the requirements of pesticide residue analysis of methyl chlorpyrifos.