粮谷中21种薰蒸剂残留量同时检测的顶空气相色谱方法的研究

采用气相色谱法电子俘获检测器,顶空进样装置建立了同时测定玉米、糙米、花生、大豆、小豆5种粮谷中三氯甲烷等21种熏蒸剂残留量的检测方法。21种熏蒸剂在0.05～10μg/mL范围内线性良好,线性相关系数均大于0.999。除顺-1,3-二氯丙烯和反-1,3-二氯丙烯为0.01mg/kg外,其余测定低限均为0.005mg/kg。在0.005～0.1mg/kg添加水平范围内,回收率范围为70.0%～95.5%。实验结果表明,建立的该检测方法样品用量少,操作简便,快速,分离完全,成本低,易普及,该方法定性、定量准确,完全满足国外检测要求,可广泛用于粮谷中熏蒸剂的检验。

Simultaneous determination of 21 kinds of fumigant residues in grain by headspace gas chromatography method

The simultaneous determination method of chloroform and other 21 kinds of fumigant residue in 5 kinds of grain for corn,rice,peanut,soybean and bean was developed by using gas chromatography with electron capture detector and headspace sampling device in this paper.The good linear relationship of 21 fumigants is indicated in a range of 0.05～10 μg/mL,and the linear correlation coefficients are greater than 0.999.The limit of detection is 0.005 mg/kg,except that the limits of detection are 0.01 mg/kg for cis-1,3-dichloropropene and anti-1,3-dichloropropene.In a level of 0.005～0.1 mg/kg,the recovery is between 70.0%～95.5%.The experimental results indicate that this method is being with less sample,easy to operate,fast,completely separated,low cost,and easy to popularize;and the methods of qualitative,quantitative are accurate.The developed method fully meets the requirements of foreign testing and can be widely used in the depth of fumigants in cereals test.