快速溶剂萃取-气相色谱法同时测定含脂羊毛中的28种有机氯拟除虫菊酯杀虫剂的残留量

建立了快速溶剂萃取-气相色谱法同时测定含脂羊毛中28种有机氯、拟除虫菊酯杀虫剂残留量的方法。在80 ℃、10.34 MPa条件下用正己烷饱和的乙腈快速提取样品,提取物经冷冻除脂、浓缩、固相萃取净化处理后直接用气相色谱分析。结果表明:16种有机氯杀虫剂在0.005～1.0 mg/L范围内,9种拟除虫菊酯杀虫剂及三氯杀螨醇、三氯杀螨砜在0.01～2.0 mg/L范围内,氟氯苯菊酯在0.02～4.0 mg/L范围内,其峰面积与质量浓度呈良好的线性关系。28种有机氯、拟除虫菊酯杀虫剂的平均回收率为67.2%～107.7%,相对标准偏差为2.6%～29.0%。结果表明：该方法具有操作简便、快速方便、灵敏度高等特点,完全可满足含脂羊毛中28种有机氯拟除虫菊酯杀虫剂残留量初筛检测的要求。

Determination of 28 organochlorine and synthetic pyrethroid pesticides in greasy wool using accelerated solvent extraction technique and gas chromatography

A method for the simultaneous determination of 28 organochlorine and synthetic pyrethroid pesticides in greasy wool was developed by accelerated solvent extraction (ASE) coupled with gas chromatography-electron capture detection (GC-ECD). The organochlorine and synthetic pyrethroid pesticides in greasy wool were extracted with acetonitrile saturated with n-hexane at 80 ℃, 10.34 MPa by ASE. The extract was pretreated by a series of procedures such as freezing-lipid filtration, concentration and purification by solid-phase extraction prior to the determination with GC-ECD. The linear ranges were 0.005-1.0 mg/L for 16 organochlorines, 0.02-4.0 mg/L for flumethrin and 0.01-2.0 mg/L for the others. There were good linear relationships between the peak area and concentration in the linear ranges. The average recoveries of 28 organochlorine and synthetic pyrethroid pesticides were 67.2%-107.7%, and the relative standard deviations were 2.6%-29.0%. The method is simple, sensitive and suitable for preliminary screening of organochlorine and synthetic pyrethroid pesticides in greasy wool.