【摘要】 建立了同时检测糙米中多种农药残留的分析方法。采用乙腈提取,使用N-丙基乙二胺键合固相吸附材料(PSA)和C18硅胶胶联吸附剂分散固相萃取(dispersive-SPE)净化,高效液相色谱-电喷雾串联质谱,正离子模式检测,内标法定量。30种农药在0.05~2 mg/kg范围内线性良好,方法检出限和定量限分别为0.5~20μg/kg和2~60μg/kg,30种农药平均回收率在73%~109%之间,相对标准偏差<10%,均能够满足农药残留分析的要求。更多还原

【Abstract】 A method based on dispersive-SPE determining pesticide residues in unpolished rice by high performance liquid chromatography-electrospray ionization mass spectrometry was developed.The mass spectrometer was operated with electrospray in the positive ion mode(ESI+).The target analytes were quantified by internal standard method and matrix-matched standard solution used to compensate for matrix effect.The sample was extracted by acetonitrile and cleaned up by dispersive solid phase extraction using primary secondary amine(PSA) and C18-bonded silica dispersant sorbent.Good linears were obtained ranging from 0.05 to 2 mg/kg.Detection and quantification limits were 0.5～20 μg/kg and 2～60 μg/kg respectively.Average recoveries ranged from 73% to 109% and relative standard deviations were less than 10% at three fortified levels.更多还原