气相色谱-串联质谱法检测蔬菜中8种氨基甲酸酯类农药残留

Detection of 8 carbamate pesticide residues in vegetables by gas chromatography-mass spectrometry

目的建立气相色谱-串联质谱(gaschromatography-massspectrometry,GC-MS)同时测定蔬菜样品中8种氨基甲酸酯农药残留的检测方法。方法样品加入内标溶液后,经乙腈提取,氯化钠分层,上清液用石墨化炭黑固相分散萃取净化,残留农药经DB-5MS毛细管色谱柱分离,气相色谱-质谱联用仪检测分析。结果 8种氨基甲酸酯农药在0.01~1.0μg/mL范围内的加标线性关系良好,相关系数均大于0.99,方法检出限为0.01 mg/kg,加标回收率范围在72.58%~98.48%之间,相对标准偏差为4.38%~12.63%。结论该方法灵敏度好,选择性高,操作简单,定性定量准确可靠,适合多种蔬菜样品中氨基甲酸酯农药的多残留检测。

Objective To develop a method for simultaneous determination of 8 carbamate pesticides residues in vegetable samples by gas chromatography-mass spectrometry(GC-MS). Methods After adding internal standard solution, the sample was extracted by acetonitrile, and stratified by sodium chloride. The supernatant was purified by graphitized carbon black solid phase dispersion extraction, the residual pesticide was separated by DB-5 MS capillary column, and detected and analyzed by gas chromatography-mass spectrometry. Results The linearity of 8 carbamate pesticides was good in the range of 0.01–1.0 g/mL, the correlation coefficient was greater than 0.99, the detection limit was 0.01 mg/kg, the recovery rate was in the range of 72.58%–98.48%, and the relative standard deviation was 4.38%–12.63%. Conclusion This method is simple, sensitive, selective and accurate and could be applied for simultaneous detection of varieties of carbamate pesticides in vegetable samples.