超高效液相色谱-串联四级杆质谱联用法测定甘蔗中噻虫胺 的残留

本研究建立了超高效液相色谱串联质谱（UPLC-MS/MS）法检测甘蔗中噻虫胺残留量的方法。甘蔗植株、茎 秆及嫩稍样品经乙腈-水（V∶V=2∶1）提取，Envi-Carb 复合 PSA 固相萃取小柱净化，ACQUITY UPLC BEH C18 色谱 柱分离，电喷雾正离子源（ESI+ ）多反应监测（MRM）模式检测，外标法定量。结果表明：采用 Envi-Carb 固相萃取 小柱，以乙腈为淋洗液，在小柱中添加 PSA 净化效果最好。在甘蔗植株、茎秆及嫩稍中分别添加 0.04、0.4、1 mg/kg 噻虫胺，平均回收率为 81.4%~109.1%，相对标准偏差（RSD）为 0.9%~10.9%。该方法的最小检出量为 0.4 ng，在甘蔗 中的最低检出浓度（LOD）为 0.04 mg/kg，能满足农药残留检测的要求。

UPLC-MS/MS Method for Determination of Clothianidin Residue in Sugarcane

A method for the detection of clothianidin residue in sugarcane was developed by solid-phase Extraction (SPE) and ultra high-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS). When the samples were leached with acetonitrile-water (V∶V=2∶1), cleaned up with ENVI CARB, added a moderate amount of PSA to the column, the purification of the extracts were found to be the most suitable. The results showed that the average recovery in sugarcane was 81.4%–109.1% with relative standard deviations of 0.9%–10.9% at spiked levels of 0.04, 0.4 and 1 mg/kg. The limit of quantification in sugarcane was 0.04 mg/kg. This method could meet the requirement for the determination of residual clothianidin.