采用气相色谱-质谱联用法测定含脂羊毛中有机氯和拟除虫菊酯杀虫剂的残留量.样品经二氧化碳超临界萃取仪萃取后,所得提取液先后经过自动凝胶渗透色谱仪和Bond Elut Si固相萃取柱净化浓缩,所得洗脱液经氮气吹干后定容至1.0 mL,于气相色谱和气相色谱-质谱分析仪测定,外标法定量.11种有机氯和5种拟除虫菊酯杀虫剂的工作曲线呈较好线性关系,检出限(3S/N)在0.022~0.32 mg·kg-1之间,测定下限(10S/N)在0.073~1.07 mg·kg-1之间.在3个标准加入水平下进行了回收率和精密度试验,所得回收率在74.8%~135.2%之间,相对标准偏差(n=6)小于10%.

Hyphenation of GC and MS was applied to the determinations of residual organochlorine and synthetic pyrethroid insecticides in fatty wool.The sample was extracted by carbon dioxide-supercritical fluid extraction,the extract obtained was purified and concentrated by automatic gel permeation chromatography and solid phase extraction with Bond Elut Si SPE column.The eluate from the SPE column was evaporated by N2-blowing and made up to 1.0 mL,which was used for GC-MS analysis.External standard method was adopted in the determination.Working curves of the 11 organochlorine insecticides and 5 pyrethroid insecticides were found to have good linearity.Limits of detection (3S/N) and lower limits of determination (10S/N) for the insecticides were found in range of 0.022-0.32 mg·kg-1 and 0.073-1.07 mg·kg-1,respectively.Tests for recovery and precision were made by standard addition method at 3 different concentration levels,values of recovery found were in the range of 74.8%-135.2% and values of RSD′s (n=6) were less than 10%.