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 chromatography- negative chemical ionization mass spectrometry

中文关键词:  气相色谱-质谱  负化学源  丙炔氟草胺  食品

英文关键词:gas chromatography-mass spectrometry  negative chemical ionization  flumioxazin  food

中文摘要:

      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。

英文摘要:

      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.