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建立了气相色谱-串联质谱技术对烟草中15种苯氧羧酸类除草剂农药残留量的分析方法。样品采用乙腈提取、Carbon TPT固相萃取柱净化、三甲基硅烷化重氮甲烷衍生化,采用气相色谱-串联质谱对15种苯氧羧酸类除草剂进行测定,通过保留时间、选择离子及相对丰度定性,外标法定量。结果表明,15种苯氧羧酸类除草剂在20~1 000μg/L浓度范围内均呈良好线性关系,相关系数大于0.992,检出限为0.9~3.3μg/kg,定量下限为3.2~10.8μg/kg。在20,100,200μg/kg 3个加标水平下的平均回收率为71.5%~105.6%,相对标准偏差(RSD)为4.5%~14.9%。该方法简便、快速、灵敏,适用于烟草中15种苯氧羧酸类除草剂的同时检测。
A gas chromatography-tandem mass spectrometry (GC-MS / MS) method was developed for the analysis of pesticide residues in 15 kinds of phenoxycarboxylic acid herbicides in tobacco. The samples were extracted with acetonitrile, purified with Carbon TPT solid phase extraction cartridge and derivatized with trimethylsilyldiazomethane. Fifteen phenoxycarboxylic acid herbicides were determined by gas chromatography-tandem mass spectrometry. The retention time, selected ions and Relative abundance of qualitative, external standard method. The results showed that all 15 kinds of phenoxycarboxylic acid herbicides had a good linearity in the concentration range of 20-1 000μg / L, the correlation coefficient was greater than 0.992, the detection limit was 0.9-3.3μg / kg and the lower limit of quantitation was 3.2-10.8 μg / kg. The average recoveries at the three spiked levels of 20, 100 and 200 μg / kg ranged from 71.5% to 105.6% and the relative standard deviations (RSDs) ranged from 4.5% to 14.9%. The method is simple, rapid and sensitive and is suitable for the simultaneous detection of 15 phenoxycarboxylic acid herbicides in tobacco.