UPLC—MS/MS法测定四种果蔬中螺虫乙酯残留量

Determination of spirotetramat in four fruits and vegetables by UPLC—MS/MS

建立一种UPLC—MS/MS法测定花菜、大白菜、莴苣和橙子4种果蔬中螺虫乙酯的快速方法。样品用2%甲酸乙腈溶液提取,经过C18、石墨化碳和MgSO4粉末吸附后,用C18色谱柱分离,以0.1%甲酸水溶液和乙腈作为流动相进行梯度洗脱。质谱条件是正离子模式电离,多反应监测,外标法定量。结果表明,螺虫乙酯在0.25-20.00ng/mL呈线性相关,R2为0.992-0.996,回收率为91.7%-114.3%,相对标准偏差为2.84%-7.10%,检出限为0.5μg/kg。该方法分析快速,灵敏,定性定量准确,可以满足螺虫乙酯残留量的测定。

A method of determination of spirotetramat in lettuce, broccoli, cabbage and orange by Ultra Performance Liquid Chroma- tography-Tandem Mass Spectrometry was developed. Samples were extracted with 2% （V/V） folic acid/acetonitrile and then cleaned up by Cl8 powers, Pesticarb and anhydrous magnesium sulfate （Mg- SO4）. The UPLC analyses were performed on a C18 column with multistep gradient elution with 0.1% （V/V） folic acid aqueous and acetonitrile as the mobile phase, combined with positive electrospray ionization （ESI＋） and multiple reactions monitoring （MRM） mode. The linear range was 0. 25 - 20 ng/mL, and the correlation coefficients were 0. 992 - 0. 996. The average recovery ranged from 91.7% to 114. 2%, and the relative standard deviations were between 2.84% to 7. 10%. The detection limit was 0. 5 μg/kg. The method is easy, rapid, sensitive and suitable for the determination of spirotetramat in the four fruits and vegetables.