提出了毛细管气相色谱测定人血清中有机氯农药残留量的方法.利用正己烷超声提取人血清样品中有机氯农药六六六和滴滴涕,所得萃取液作气相色谱测定,用甲酸及浓硫酸净化、磺化处理后,电子捕获检测器检测.在优化的试验条件下,8种有机氯农药同分异构化合物组分在20 min内能够很好的分离,其质量浓度与色谱峰面积在0.4~10 μg·L-1浓度范围内呈线性关系,检出限(3S/N)在0.07~0.30 μg·L-1之间.方法的日内的相对标准偏差为2.9%~5.4%,日间的相对标准偏差为4.5%~8.9%.方法的加标回收率在81.5%~117.6%范围.

Gas chromatography with capillary column was applieed to the determination of residual amounts of organochlorine pesticides in human serum.The sample was diluted with formic acid and extracted with n-hexane ultrasonically.The upper organic layer was taken and sulfonated with conc.H2SO4.The sulfonated solution layer was separated and evaporated to near dryness in a vacuum dryer.The residue was taken up with 1 mL of n-hexane and used for GC analysis,with electron capture detector.Four isomers each of the pesticides DDT and BHC were separated satisfactorily and determined within 20 min.Linear relationships between values of peak area and mass concentration of the 8 isomeric compounds were obtained in the range of 0.4-10 μg·L-1,with values of detection limit (3S/N) ranged from 0.07 to 0.30 μg·L-1.Values of intraday and interday RSD′s (n=6) found were in the ranges of 2.9%-5.4% and 4.5%-8.9% respectively.Recovery was tested by standard addition method,giving values in the range of 81.5%-117.6%.