大气压气相色谱电离源-离子淌度-飞行时间质谱法测定蔬菜中的8种有机磷农药残留

Determination of 8 kinds of organophosphorus pesticide residues in vegetables by atmospheric pressure gas chromatography-ion mobility spectrum-quadrupole-time of flight- mass spectrometry

中文关键词:  农药残留  大气压气相色谱电离源-离子淌度-飞行时间质谱法  蔬菜

英文关键词:pesticide residues  atmospheric pressure gas chromatography-ion mobility spectrum-quadrupole- time of flight-mass spectrometry  vegetables

中文摘要:

      目的 建立大气压气相色谱电离源-离子淌度-飞行时间质谱法定量测定蔬菜中8种有机磷农药残留的分析方法。方法 样品经乙腈提取, DisQuE净化后浓缩至净干, 丙酮定容, 离子淌度结合非数据依赖扫描模式进行数据采集分析, 利用四维数据(保留时间、精确质量数、碎片离子和离子淌度)对目标化合物进行定性分析, 母离子外标标准曲线法进行定量分析。结果 8种农药残留在5.0~200 ng/mL范围内具有良好的线性关系, 相关系数(r)为0.9988~0.9993, 方法检出限为0.003 mg/kg, 定量限为0.01 mg/kg; 平均回收率70.7%~113.4%, 精密度RSD≤6.57%。结论 本研究所建立的方法操作简便, 具有良好的回收率、准确性和灵敏度, 抗干扰能力强, 适用于蔬菜中农药残留筛查和定量。

英文摘要:

      Objective To establish a method for the determination of 8 organphosphorus pesticide residues in vegetables by atmospheric pressure gas chromatography-ion mobility spectrum-quadrupole-time of flight-mass spectrometry (APGC-IMS-QTof). Methods The sample was extracted by acetonitrile, purified by DisQuE, concentrated to dry and dissolved in acetone. Four-dimensional datasets (retention time, accurate precursor mass, accurate product ion mass and ion mobility spectrum) were acquired in the high definition data independent mode and the quantitative analysis was carried out by external standard method. Results The linear relationship of the 8 kinds of pesticides was good within the range of 5.0-200 ng/mL, with the correlation coefficient (r) between 0.9988 and 0.9993. The limit of detection (LOD) was 0.003 mg/kg, and the limit of quantification (LOQ) was 0.01 mg/kg. The average recoveries were 70.7%-113.4% with relative standard deviation≤6.57%. Conclusion This method is simple and characterized with good recovery, accuracy and sensitivity, which is suitable for the detection of pesticide residues in vegetables.