剧毒杀鼠药氟乙酸(盐)的检验

Determination of fluoroacetic acid(salt)

目的:建立剧毒杀鼠药氟乙酸(盐)的提取、检验方法。方法:对不同检材分别采用甲醇-乙腈提取法、乙醇沉淀蛋白提取法和甲醇直接提取法;对氟乙酸(盐)采用硫酸二甲酯条件下的甲醇衍生化方法;使用配备有 Plot-Q 弹性石英毛细管柱(30 m×0.32 mm)的 HP-GCD 气质联用仪进行分析;以衍生化产物氟乙酸甲酯的保留时间和特征 m/e 数及特征峰面积作为定性、定量的依据。结果:该方法在2.0～350.0μg·mL^(-1)的浓度范围内呈良好线性关系(r=0.9991,n=5),检出限为1.3μg·mL^(-1),方法平均回收率为85%(RSD=6.8%)。结论:该方法与现行的检验方法相比,大大地简化了操作程序,简单易行,条件宽松,结果可靠,提高了检验的灵敏度,在实际案件检验中取得了很好的效果。

Objective： To establish a method of extraction and determination fluoroacetic acid （salt）. Method： Use the alkalescence methanoL/acetonitrle extraction method, ethanol protein precipitation extraction method, and the methanol direct extraction method to different sample. The fluoroacetic acid（salt） were analyzed by methanol derivative method in dimethyl sulfate condition and GC - MS ;Take the derivant - methyl fluoroacetate retention time, m/ e and the area of characteristic peak as the basis of qualitative and quantitive analysis. Results：This method had a good linear within the concentration range of 2. 0 - 350. 0 μg · mL^-1 （ r = 0. 9991, n = 5 ）, the detection limit was 1.3 μg · mL^-1, the average recovery was 85% （RSD = 6. 8% ）. Conclusion：This method is proved to be suitable for application in forensic field, which is easy to deal with, credible and higher sensitivity.