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目的建立气相色谱-质谱联用(GC/MC)检测4.5%高效氯氰菊酯(beta-cypermethrin)农药中邻二甲苯(ox)、间二甲苯(mx)、对二甲苯(px)的实验室方法,为含有二甲苯农药中毒的鉴定和诊治提供参考。方法选用外标标准曲线法对二甲苯三种同分异构体进行定量分析。优化的GC-MS色谱条件,达到二甲苯三种同分异构体完全分离,分别配制二甲苯ox、mx和px三种异构体的不同浓度梯度的标准溶液绘制标准曲线。标准样品及特征离子比对进行同分异构体定性,在选择离子模式下选用峰面积进行定量。结果二甲苯三种同分异构体在0.5~300 ng/ml之间线性均良好,线性相关系数(R2)均大于0.999。ox、mx和px的检出限(LOD)分别为0.48、0.46和0.42 ng/ml;定量限(LOQ)分别为1.61、1.54和1.40 ng/ml。方法的平均回收率大于94.2%,精密度相对标准偏差小于6.4%。结论 GC/MC外标标准曲线法用选择离子模式检测4.5%高效氯氰菊酯中二甲苯含量的方法灵敏性好、操作简便,可为农药中毒有机溶剂二甲苯成分法医学鉴定提供参考。
Objective To establish a laboratory method for the determination of ox, mx and px in a 4.5% beta-cypermethrin pesticide by gas chromatography-mass spectrometry (GC / MC) For xylene pesticide poisoning identification and diagnosis provide a reference. Methods Quantitative analysis of three isomers of xylene by external standard curve method was carried out. Optimized GC-MS chromatographic conditions, to achieve complete separation of the three isomers of xylene, were prepared xylene ox, mx and px isomers of different concentration gradient of the standard solution to draw a standard curve. Isotopic characterization is performed on standard samples and characteristic ion ratios, and peak area is used for quantification in selected ion mode. Results The three isomers of xylene showed a good linearity between 0.5-300 ng / ml with a linear correlation coefficient (R2) greater than 0.999. The limit of detection (LOD) for ox, mx and px were 0.48, 0.46 and 0.42 ng / ml, respectively. The LOQs were 1.61, 1.54 and 1.40 ng / ml, respectively. The average recovery of the method was greater than 94.2%, and the relative standard deviation of precision was less than 6.4%. Conclusion The method of GC / MC standard curve method for the determination of xylene in 4.5% beta-cypermethrin by ion-selective mode is sensitive and easy to operate. It can be used as a reference for the forensic identification of xylene components of pesticide poisoning organic solvents.