基于QuEChERS-液相色谱-串联质谱法测定稻米中嘧草醚和双草醚残留

CHINESE JOURNAL OF CHROMATOGRAPHY(2017)

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Abstract
采用改良的QuEChERS-液相色谱-串联质谱(LC-MS/MS)技术,建立了稻米中嘧草醚和双草醚残留量的检测方法.样品经酸化乙腈提取,由十八烷基键合硅胶(C18)吸附剂净化.以0.1%(体积分数)甲酸水(含5 mmol/L乙酸铵)-乙腈为流动相进行梯度洗脱,经ZORBAX SB C18色谱柱实现目标化合物的基线分离.采用电喷雾正离子(ESI+)模式扫描,动态多反应监测(dynamic MRM)技术定性分析,外标法定量.结果表明:在稻米基质中,嘧草醚和双草醚在各自的线性范围内线性关系良好(r2≥0.996);嘧草醚和双草醚的检出限(LOD)分别为0.8和3 μg/kg.在3个添加水平下,嘧草醚和双草醚的平均回收率分别为76.6%~85.6%和73.0%~86.7%,相对标准偏差(RSD)分别为0.9%~3.4%和1.2%~5.5%(n=6).该方法简便、快速、灵敏,适用于稻米中嘧草醚和双草醚的同时分析.
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Key words
QuEChERS, liquid chromatography-tandem mass spectrometry (LC-MS/MS), pyriminobac-methyl, bispyribac-sodium, rice
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