超高效液相色谱串联质谱法测定烟草中的噁霉灵残留

为降低烟草中噁霉灵检测中的基质干扰,提高检测灵敏度和和稳定性,通过试验建立了以QuEChERS为样品前处理方法、液相色谱串联质谱仪为检测仪器的烟草中噁霉灵残留检测方法。样品加水浸润后,经丙酮提取、盐析试剂包除水、石墨化炭黑除杂后,采用Agilent ZORBAX 300SB-C8液相色谱柱（2.1 mm×100 mm,1.8 μm）分离,甲醇-水程序洗脱,ESI雾化,串联质谱MRM检测。结果发现,该方法在0.0025~0.0500 mg/L范围内线性良好,决定系数r²=0.9996,定量检测限1.06 μg/L,回收率在90.8%~92.0%之间,相对标准偏差为5.1%。运用该方法测定烟草中的噁霉灵,操作简单,检测精度高,满足CORESTA对烟草农残检测的要求。

Determination of Hymexazol Residues in Tobacco by UPLC-MS/MS

In order to reduce matrix interference and improve detection sensitivity and stability, a method for determination of hymexazol residues in tobacco was established using QuEChERS as sample pretreatment method and liquid chromatography tandem mass spectrometer as detection instrument. The samples were extracted by acetone after moistened with water, then bytreated with salting-out reagent to remove water and purified by graphitized carbon black (GCB). After separated by Agilent ZORBAX 300SB- C8 column (2.1 mm×100 mm, 1.8 μm) with methanol-water as the mobile phase,the extracts were detected by an electrospray ionization (ESI) tandem mass spectrometry in the multiplereaction-monitoring (MRM) mode. The results showed that good linearity was obtained in the range of 0.0025-0.0500 mg/L, the linear correlation coefficient (r²) was 0.9996, the quantitative detection limit was 1.06 μg/L, the recovery ratio was between 90.8%-92.0%, and the relative stantdard deviation was 5.1%. With simple operation and high detection accuracy, this method is suitable for hymexazol determination in tobacco, which meets CORESTA's requirements for tobacco pesticide residue detection.