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机构地区:[1]农业部食品质量监督检验测试中心(武汉),武汉430064
出 处:《湖北农业科学》2016年第24期6575-6577,6587,共4页Hubei Agricultural Sciences
基 金:农业部农药检定所农药登记残留试验项目
摘 要:建立QuEChERS结合超高效液相色谱串联质谱(UPLC-MS/MS)法测定了番茄中吡蚜酮和吡丙醚残留量的分析方法。样品用乙腈超声提取,QuEChERS法提取和净化,UPLC-MS/MS分析检测。结果表明,在0.005~0.5 mg/L范围内,吡蚜酮的相关系数为0.994 5,吡丙醚的相关系数为0.999 6,该方法的线性关系良好。在0.02、0.2、1.0 mg/kg 3个添加浓度下,吡蚜酮的平均添加回收率为87.5%~106.1%,RSD值在2.2%~3.1%之间;吡丙醚的平均添加回收率为82.2%~89.1%,RSD值在1.6%~14.7%之间。吡蚜酮的检出限为1.0×10^(-3) mg/kg,吡丙醚的检出限为2.0×10^(-4) mg/kg。该方法适用于番茄中吡蚜酮和吡丙醚残留量的测定。A method of QuEChERS combined with ultra performance liquid chromatography-tandem mass spectrometry(UPLCMS/MS) was developed for the determination of pymetrozine and pyriproxyfen residues in tomato. The tomato samples were extracted with acetonitrile by ultrasonic wave, extracted purified by QuEChERS method and analyzed by UPLC-MS/MS. The linear ranges of pymetrozine and pyriproxyfen were 0.005~0.5 mg/L, and the correlation coefficient of pymetrozine was 0.994 5,and pyriproxyfen was 0.999 6. When the spiked levels were 0.02,0.2 and 1.0 mg/kg,the average recoveries of pymetrozine ranged from 87.5% to 106.1% with the relative standard deviation(RSD) from 2.2% to 3.1%,and the average recoveries of pyriproxyfen ranged from 82.2% to 89.1% with the relative standard deviation(RSD) from 1.6% to 14.7%. The limit of detection(LOD) of pymetrozine was 1.0×10^(-3)mg/kg, and pyriproxyfen was 2.0×10^(-4)mg/kg. The method can be used for determination of pymetrozine and pyriproxyfen residues in tomato.
关 键 词:超高效液相色谱串联质谱(UPLC-MS/MS) QUECHERS 番茄 吡蚜酮 吡丙醚
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