CAJ | 학술논문

建立玉米、大豆和土壤中氟噻乙草酯残留的液质串联快速分析检测方法。样品中的氟噻乙草酯经乙腈提取，N-丙基乙二胺(PSA)和多壁碳纳米管(MWCNTs)净化，利用超高压液相色谱-串联质谱(UPLC-MS/MS)在多反应监测模式下进行检测。以碎片离子对404.0/274.0定性、离子对404.0/344.0进行外标法定量。仪器在0.001~1.0 mg/kg范围内，具有良好线性关系。在0.001~1.0 mg/kg添加水平范围内，氟噻乙草酯在玉米、大豆和土壤中的平均回收率为95.8%~105.0%，变异系数为3.1%~7.8%。该方法的检出限(LOD)为0.007~0.014μg/kg，定量限为(LOQ)为1.0μg/kg。本方法简便、快速、准确，能满足国内外法规的要求，可用于玉米、大豆和土壤样品中氟噻乙草酯的农药残留确证检测。
건립옥미、대두화토양중불새을초지잔류적액질천련쾌속분석검측방법。양품중적불새을초지경을정제취，N-병기을이알(PSA)화다벽탄납미관(MWCNTs)정화，이용초고압액상색보-천련질보(UPLC-MS/MS)재다반응감측모식하진행검측。이쇄편리자대404.0/274.0정성、리자대404.0/344.0진행외표법정량。의기재0.001~1.0 mg/kg범위내，구유량호선성관계。재0.001~1.0 mg/kg첨가수평범위내，불새을초지재옥미、대두화토양중적평균회수솔위95.8%~105.0%，변이계수위3.1%~7.8%。해방법적검출한(LOD)위0.007~0.014μg/kg，정량한위(LOQ)위1.0μg/kg。본방법간편、쾌속、준학，능만족국내외법규적요구，가용우옥미、대두화토양양품중불새을초지적농약잔류학증검측。
A rapid analytical method for determining fluthiacet-methyl residue in maize, soybean and soil was established based on ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). The fluthiacet-methyl from maize, soybean and soil samples, which was extracted by acetonitrile and cleaned up by primary secondary amine (PSA) and multi-walledcarbon nanotubes (MWCNTs), was determined by ultra performance liquid chromatography-tandem mass spectrometry under multiple reaction monitoring mode, and the qualitative ion pair was 404.0/274.0, the quantitative ion pair was 404.0/344.0. The method had good linear relationship in the concentration range of 0.001~1.0 mg/kg. The average recoveries of fluthiacet-methyl in maize, soybean and soil were in the range of 95.8%~105.0% at spiked levels from 0.001~1 mg/kg, with relative standard deviations of 3.1%~7.8%. The limits of detections (LOD) on maize, soybean and soil was 0.007~0.014 μg/kg, while the limits of quantification (LOQ) was 1 μg/kg. The method is simple, rapid, and accurate, which can meet the requirements of the domestic and international legislation. The method adapts to confirm residues of fluthiacet-methyl pesticides in maize, soybean and soil samples.