气相色谱-质谱法同时测定水果中14种农药残留

Simultaneous determination of 14 pesticide residues in fruits by gas chromatography-mass spectrometry

目的 建立一种气相色谱-质谱法,对水果中14种农药残留进行测定。方法 样本经固相萃取净化,TG-1701MS石英毛细管色谱柱程序升温分离,质谱选择离子模式定量。结果 检出限为0.002~0.01 mg/kg,线性相关系数r均达到0.995,相对标准偏差为1.4%~5.5%,回收率为71.6%~115.1%。对80个水果样品中14种农药残留进行检测,两批次检测出甲胺磷,含量分别为0.04、0.05 mg/kg;一批次检测出水胺硫磷为0.02 mg/kg;两批次检测出三唑磷,均为0.22 mg/kg。结论 建立了14种农药同时分析的检测方法,对实际样品农药残留测定有一定实用价值。

Objective To establish a method for the determination of 14 pesticide residues in fruits using gas chromatography-mass spectrometry. Methods The samples were purified by solid-phase extraction, separated by TG-1701 MS quartz capillary column in temperature-programmed mode, and quantified by mass spectrometry in selected ion mode. Results The detection limit was 0.002-0.01 mg/kg, the linear correlation coefficient r reached 0.995, the relative standard deviation(RSD) was 1.4%-5.5%, and the recovery rate was 71.6%-115.1%. 80 fruit samples were detected, and methamidophos was detected twice at 0.04 and 0.05 mg/kg, respectively. Isocarbophos was detected once at 0.02 mg/kg, and triazophos was detected twice, both at 0.22 mg/kg. Conclusion A method for simultaneous determination of 14 pesticides is established, and it has certain practical value for the determination of pesticide residues in actual samples.