气相色谱高分辨飞行时间质谱法快速筛查水果中283种农药残留

Rapid screening of 283 pesticide residues in fruits by gas chromatography time-of-flight mass spectrometry

中文关键词:  气相色谱高分辨飞行时间质谱法  农药  多残留  水果

英文关键词:gas chromatography high resolution time-of-flight mass spectrometry  pesticide  multi-residue  fruit

中文摘要:

      目的 建立气相色谱高分辨飞行时间质谱法(gas chromatography time-of-flight mass spectrometry, GC-TOF/MS)快速筛查水果中283种农药残留量的分析方法。方法 利用气相色谱高分辨飞行时间质谱结合MassHunter、PCDL软件建立283种农药的EI精确质量谱库, 试样经QuEChERS方法进行萃取净化后, 采用EI全扫描监测, 通过PCDL谱库全离子筛查模式检索, 以保留时间、特征离子精确质量数、分子离子同位素信息等作为定性依据。由谱库选择质量数较大、丰度比较高的精确质量离子为定量离子, 进行定量测定。 结果 在空白苹果、葡萄、橙3种水果中添加10、20、40 μg/kg 3个浓度水平下, 方法的平均回收率65.9%~129.1%, 相对标准偏差(relative standard deviation, RSD)2.8%~11.6%, 方法的最低检出浓度可达0.5~ 10 μg/kg。结论 该方法简便、快速、灵敏、精密度好, 是水果中常见农药残留有效快速筛查技术。

英文摘要:

      Objective To establish a method for the rapid simultaneous screening of 283 pesticide residues in the fruits by gas chromatography time-of-flight mass spectrometry(GC-TOF/MS). Methods A total of 283 pesticides were injected to GC-TOF/MS to create the personal compound database, which exact mass of ions from the first-stage mass spectrum, using MassHunter and PCDL software. The fruit sample was extracted and purified using QuEChERS approach. Extracts were analyzed by GC-TOF/MS operating in high resolution TOF mode with electron ionization. The qualitative screening and quantitative analysis fulfilled by full scan mode, based on an accurate-mass database, which included the retention time, characteristic ion precise mass and molecular ion isotope. Results The three different concentrations levels of 10, 20 and 40 μg/kg were spiked to apple, grape, orange samples. The average recoveries ranged from 65.9% to 129.1%, with relative standards deviation (RSD) of 2.8%~11.6%. The limits of detection were in the range of 0.5~10 μg/kg for the pesticides. Conclusion The experimental results show that the multi-residue analytical method is simple, rapid, sensitive and accurate, it may be effectively applied to the monitoring of the common pesticides in the fruit samples.