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目的:建立蔬果中25种有机磷农药残留全自动固相萃取/气相色谱质谱分析方法。方法:采乙腈均浆提取样品中的有机磷类农药,通过全自动固相萃取仪提取净化,用气质联用进行分析。结果:25种有机磷农药在0.05 mg/kg～5.0 mg/kg范围内均有较好的线性,相关系数均在0.99以上,最低检出限为0.004 mg/kg,25种有机磷农药回收率加标0.5 mg/kg时,为80.2%～98.7%之间,加标1.0 mg/kg时,为74.2%～99.8%之间,变异系数RSD,加标0.5 mg/kg时,为1.1%～4.8%之间,加标1.0 mg/kg时,为1.5%～6.8%之间。结论:此法简便,快速,净化效果好,回收率高,可同时测定水果、蔬菜中的多种有机磷农药残留。
Objective: To establish a method for the automatic determination of 25 organophosphorus pesticide residues in vegetables and fruits by gas chromatography-mass spectrometry. Methods: Organophosphorus pesticides were extracted from the samples by acetonitrile homogenization, purified by automatic SPE extraction and analyzed by GC / MS. Results: All the 25 organophosphorus pesticides showed good linearity in the range of 0.05 mg / kg ~ 5.0 mg / kg with the correlation coefficients above 0.99 and the lowest detection limit of 0.004 mg / kg. The recoveries of 25 organophosphorus pesticides When spiked with 0.5 mg / kg, the coefficient of variation (RSD) ranged from 80.2% to 98.7%, with a spike of 1.0 mg / kg, ranging from 74.2% to 99.8% 4.8%, spiked 1.0 mg / kg, between 1.5% and 6.8%. Conclusion: This method is simple, rapid, good purification effect, high recovery, and can simultaneously determine a variety of organophosphorus pesticide residues in fruits and vegetables.