基于气相色谱法的含脂羊毛中4种拟除虫菊酯药物残留测定

 为了研究建立气相色谱－电子捕获检测器测定含脂羊毛中4种拟除虫菊酯杀虫剂残留的国家标准方法。在空白含脂毛中分别添加4个浓度水平（0.06 μg/g、0.30 μg/g、2.00 μg/g、5.00 μg/g）的4种拟除虫菊酯农药混标，以正己烷+乙醚（体积比2:1）为提取溶剂，中性氧化铝固相萃取柱和弗罗里硅土柱净化，以4 ml正己烷+乙酸乙酯（体积比95:5）进行洗脱，气相色谱－电子捕获检测器测定，外标法定量。结果显示：4种农药的最小检出量分别为0.020 μg/g、0.060 μg/g、0.024 μg/g和0.030 μg/g，平均回收率79.4%~101.2%，相对标准偏差1.20%~3.08%，分离良好，干扰峰少，结果准确，且操作简便、快捷，溶剂使用量小、符合环保要求。

Determination of 4 pyrethroid pesticide residues in greasy wool based on gas chromatography

n order to study and establish the national standard method of 4 kinds of pyrethroid pesticide residues in greasy wool by a gas chromatography - ECD method, the greasy wool?were added 4 levels mixed?standard reagent (0.06?μg/g,?0.30?μg/g,?2.00?μg/g,?5.00?μg/g),?which contains?4 kinds of pyrethroids, then the sample was extracted by n-hexane and aether（Volume ratio2:1）, and then purified by a neutral alumina column and an florisil column and eluted by 4ml of n-hexane and ethyl acetate（Volume ratio95:5）, finally detected by gas chromatography -ECD, the quantitative results were obtained based on external standard method. The result shows that the limits of detection of 4 kinds of pesticides were 0.020 μg/g, 0.060 μg/g, 0.024 μg/g and 0.030 μg/g respectively, the recoveries range were from 79.4% to 101.2%, the relative standard deviations were between 1.20% and 3.08%.So the method is an favorable separation effect, less disturbance, accurate, easy, quick, less use of solvent and environmental friendly.