目的建立人乳中有机氯农药六六六和滴滴涕的检测方法,并对北京、兰州和杭州三个地区的蓄积水平现状进行分析。方法人乳样品用乙腈提取,经过酸化的硅胶固相萃取柱净化、浓缩后,采用气相色谱仪检测。结果 8种农药的线性范围在5~200 ng/mL,相关系数0.9955~0.9994,定量限均小于2.6μg/kg,平均回收率在70%~122%,相对标准偏差在3.91%~10.77%。结论本方法结合磺化法和固相萃取法,能有效去除基质中的杂质。通过方法学验证证明,本方法操作简单、精确、快速,适用于人乳中有机氯的检测。随着六六六、滴滴涕等持久性有机氯农药的禁用或严格限用,人乳中持久性有机氯农药的蓄积水平明显降低。 Objective To establish a method for the determination of organochlorine pesticides (BHC) and DDT in human milk and to analyze the status of accumulation in Beijing, Lanzhou and Hangzhou. Methods Human milk samples were extracted with acetonitrile and purified by acidified silica gel solid phase extraction column. After concentration, the samples were detected by gas chromatography. Results The linear range of the eight pesticides ranged from 5 ng / mL to 200 ng / mL. The correlation coefficients ranged from 0.9955 to 0.9994. The limit of quantification was less than 2.6 μg / kg. The average recoveries ranged from 70% to 122% with relative standard deviations between 3.91% and 10.77%. Conclusion This method combined with sulfonation and solid-phase extraction, can effectively remove the impurities in the matrix. The methodological verification proves that the method is simple, accurate and rapid, and is suitable for the detection of organochlorine in human milk. With the banned or severely restricted use of persistent organic chlorine pesticides such as 666 and DDT, the level of persistent organochlorine pesticides in human milk is significantly reduced.