QuEChERS-高效液相色谱-串联质谱法测定果蔬中多效唑残留

建立了果蔬中多效唑的QuEChERS-高效液相色谱-串联质谱法检测方法。样品用乙腈快速提取,NaCl和无水MgSO4除水后,经PSA和石墨炭黑净化,用高效液相色谱-串联质谱法分析。采用正离子多反应监测模式检测,定性离子对为m/z 294.2/70.0、294.2/125.0,采用m/z 294.2/70.0进行定量分析。在0.05、0.5、1 mg/kg添加水平下,样品平均回收率为79.6%~94.9%;相对标准偏差为3.6%~11.4%;在梨、苹果、桃、西红柿和黄瓜中的检出限分别为0.4、0.5、0.4、0.4、0.5μg/kg。结果表明:本方法简便、快速、安全、价格低廉,重复性良好,可用于果蔬样品中多效唑残留的快速确证检测。

Determination of Paclobutrazol Residues in Fruits and Vegetables by QuEChERS-High Performance Liquid Chromatography-Triple Quadrupole Tandem Mass Spectrometry

A method was developed for the determination of paclobutrazol residues in fruits and vegetables by using
QuEChERS-high performance liquid chromatography-triple quadrupole tandem mass spectrometry (HPLC-MS-MS).
Paclobutrazol residues in fruit samples were extracted with acetonitrile, dehydrated with sodium chloride and anhydrous
magnesium sulfate, cleaned up by dispersive solid phase extraction on primary secondary amine and graphitized carbon
black, and detected by HPLC-MS-MS under a multiple reaction-monitoring mode. The qualitative results were obtained
based on the characteristic m/z 294.2/70.0 and m/z 294.2/125.0, and the quantitative results were based on the characteristic
m/z 294.2/70.0. The recoveries of paclobutrazol were in the range from 79.6% to 94.9% at three spiked levels of 0.05, 0.5
and 1 mg/kg from five fruits and vegetable matrixes (pear, apple, peach, tomato and cucumber), with relative standard
deviations (RSDs) between 3.6% and 11.4%, and the limits of detection were 0.4, 0.5, 0.4, 0.4 and 0.5 μg/kg, respectively.
The method is simple, quick, safe, reproducible and applicable to detect and confirm paclobutrazol residues in fruit and
vegetable samples.