高效液相色谱-串联质谱法测定蔬菜中氟啶脲
HPLC-MS/MS Determination of Chlorfluazuron in Vegetables
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摘要: 提出了高效液相色谱-串联质谱法测定蔬菜中氟啶脲残留量.样品中氟啶脲经乙腈提取,弗罗里硅土柱净化后,以甲醇-水(90+10)混合溶液为流动相,经Agilent Eclipse XDB-C8(150 mm×4.6 mm,5 μm) 色谱柱分离.在负离子模式下,用多反应监测技术测定.氟啶脲的峰面积与其质量浓度在1~50 μg·L-1范围内呈线性关系,测定下限(10S/N)为0.01 mg·kg-1.在3个标准加入水平下进行了回收率和精密度试验,加标回收率在91.7%~97.3%之间,相对标准偏差(n=6)小于5%.Abstract: HPLC-MS/MS was applied to the determinations of residual chlorfluazuron in vegetables.The sample was extracted with acetonitrile and the extract obtained was purified on Florisil column.The eluate was separated by gradient elution with methanol (90+10 by vol) solution on Agilent Eclipse XDB-C8(150 mm×4.6 mm,5 μm) column,and detected by multiple reaction monitoring (MRM) in negative ion mode.Linear relationship between the peak area and the mass concentration of chlorfluazuron was obtained in the range of 1-50 μg·L-1,with detection limit (10S/N) 0.01 mg·kg-1.Tests for recovery and precision were made by standard addition method at 3 different concentration levels,values of recovery found were in the range of 91.7%-97.3% and values of RSD′s (n=6) were less than 5%.