GC-MS检测蜂蜜中双甲脒残留量的方法研究

The Methods of Detection of Amitraz and Its Metabolite(2, 4-xylidine) Residues in Honey Based on Gas Hromatography-Mass Spectrometry

试验通过改变提取溶剂体积和前处理步骤,建立了一种快速、节约、高效的GC-MS检测蜂蜜中双甲脒残留量方法。经验证,该方法检出限为17.2μg/kg,定量限为57.3μg/kg,在20~320 ng/mL线性范围内双甲脒及其代谢物的峰面积与浓度呈良好线性关系,相关系数达0.999以上。当加标浓度在80 ng/mL时,双甲脒回收率达到92.8%~99.1%,2,4-二甲基苯胺回收率达到84.6%~88.9%。在600μg/kg含量水平下连续测定6针,其相对标准偏差为0.816%。该方法简单可靠,适合实验室进行样品的批量处理。

In order to change the solvent extraction volume and processing steps, establish a rapid, economical and efficient GC-MS method to measure the amitraz and its metabolite（2, 4-xylidine） residues in honey. Verified, the method detection limit was 17.2 μg/kg, quantitative limit was 57.3 μg/kg, and the linear ranged from 20 to 320 ng/mL. Amitraz and its Metabolite（2, 4-xylidine） had good linear relationship between peak area and concentration, and the correlation coefficient was more than 0.999. When the standard addition concentration was 80 ng/mL, amitraz recovery was 92.8%-99.1%, and 2, 4-dimethylaniline recovery was 84.6%-88.9%. Under 600 μg/kg levels, the result of the continuous determination of 6 needle relative standard deviation was 0.816%. This method was simple and reliable, suitable for laboratory for the batch processing of the sample.