气相色谱-负化学源质谱法测定食品中残留的丙炔氟草胺

Determination of flumioxazin residue in foods by gas chromatographynegative chemical ionization mass spectrometry

目的建立气相色谱-负化学源质谱法(gas chromatography-negative chemical ionization-mass spectrometry,GC-NCI-MS)测定食品中残留的丙炔氟草胺的方法。方法样品经乙腈提取,固相萃取净化,丙酮+正己烷(1:1,V:V)洗脱,采用纯溶剂校正曲线外标法定量,由GC-NCI-MS在选择离子监测模式下进行测定。结果丙炔氟草胺在0.01~1.00 mg/L范围内有良好的线性关系(r>0.999),最低检出限为0.0006 mg/kg,在0.01、0.02、0.10 mg/kg 3个添加水平下丙炔氟草胺的回收率为92.5%~107%,相对标准偏差均≤10.1%(n=6)。结论该方法灵敏度,准确度和精密度均较高,能消除复杂基质带来的干扰,适合多种食品中丙炔氟草胺检测的确证分析。

Objective To establish a method for the determination of flumioxazin residue in foods by gas chromatography-negative chemical ionization-mass spectrometry(GC-NCI-MS).Methods The samples were extracted by acetonitrile,purified by solid phase extraction and eluted by acetone+n-hexane(1:1,V:V).It was quantified by pure solvent calibration curve external standard method and determined by GC-NCI-MS under the selective ion monitoring mode.Results Flumioxazin had a good linear relationship in the range of 0.01~1.00 mg/L(r>0.999),and the minimum limit of detection was 0.0006 mg/kg.The recovery rates of flumioxazin in the 3 added levels of 0.01,0.02 and 0.10 mg/kg were 92.5%to 107%,and the relative standard deviations were≤10.1%(n=6).Conclusion The method has high sensitivity,accuracy and precision,it can eliminate interference caused by complex matrices,and is suitable for confirmatory analysis of flumioxazin in various foods.