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目的:建立了蔬菜中灭多威的气相色谱-质谱分析方法,有利于开展蔬菜中农药灭多威残留量的监测。方法:蔬菜样品采用乙腈提取,经无水硫酸钠滤纸过滤、浓缩,再经弗罗里硅土固相萃取柱净化,采用气相色谱-质谱法进行检测分析。结果:质谱分析通过105、88、58、47、42几个碎片特征峰可对灭多威进行准确定性。灭多威含量在0~100 mg/L范围内线性关系良好,r=0.9991,方法加标回收率为80.69%～106.50%,相对标准偏差为6.01%～9.51%,方法的检出限为4μg/Kg。结论:该方法可用于蔬菜中灭多威残留量的检测,灵敏度高、定性定量准确,能够快速诊断。
OBJECTIVE: To establish a method for the determination of methomyl in vegetables by gas chromatography-mass spectrometry, which is conducive to the monitoring of pesticide residues in vegetables. Methods: The samples of vegetables were extracted with acetonitrile, filtered through anhydrous sodium sulfate filter paper and concentrated. The samples were purified with Florisil solid-phase extraction (SPE) column and detected by gas chromatography-mass spectrometry. Results: Mass spectrometry through 105,88,58,47,42 several debris peaks can be methomyl accurate characterization. The calibration curve of methomyl was linear in the range of 0-100 mg / L, r = 0.9991. The recoveries were 80.69% -106.50% and the relative standard deviations were 6.01% ~ 9.51%. The detection limit was 4μg / Kg. Conclusion: The method can be used for the detection of methomyl residue in vegetables with high sensitivity, accurate qualitative and quantitative analysis and rapid diagnosis.