Florisil分散固相萃取-HPLC-MS/MS联用法测定果蔬中氯吡脲的残留

采用高效液相色谱-串联质谱法快速测定水果、蔬菜中的氯吡脲残留量。样品经乙腈均质提取，无水硫酸镁和Florisil作为吸附剂净化，经0.22 μm微孔滤膜过滤，用0.1%甲酸溶液和乙腈为流动相梯度洗脱，C18柱分离，采用电喷雾正离子多反应监测模式检测，外标法定量。结果表明，氯吡脲在0.5～40 μg/L质量浓度范围内与峰面积呈良好的线性关系（R＞0.999），定量限为1.0 μg/kg，在添加量为1.0、5.0、20 μg/kg时，平均回收率为85.9%～97.9%，相对标准偏差为2.8%～8.7%（n=6）。该方法分析速度快、灵敏度高、重复性好，适用于水果、蔬菜中氯吡脲残留量的测定。

Determination of Forchlorfenuron Residues in Vegetables and Fruits by Florisil Dispersive Solid Phase Extraction-High Performance Liquid Chromatography-Tandem Mass Spectrometry

High performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was applied to the rapid
determination of residual amounts of forchlorfenuron in vegetables and fruits. The samples were extracted with acetonitrile
while stirring, purified with the adsorbents Florisil and anhydrous magnesium sulfate, and filtered through 0.22 μm millipore
membrane. The filtrate was separated on a C18 column using gradient elution with a mobile phase consisting of 0.1% formic
acid and acetonitrile, detected by electrospray ionization (ESI) in the positive mode using multiple reaction monitoring
(MRM), and quantified by an external standard method. The developed method showed a good linear relationship in the
range of 0.5–40 μg/L for forchlorfenuron, with a correlation coefficient higher than 0.999. The limit of quantitation (LOQ)
for forchlorfenuron was 1.0 μg/kg. The average recovery rates were 85.9%–97.9% at spiked levels of 1.0, 5.0, and 20 μg/kg,
with relative standard deviation (RSD, n = 6) ranging from 2.8% to 8.7%. This method is fast, highly sensitivity, repeatable
and suitable for the determination of forchlorfenuron residues in vegetables and fruits.