固相萃取净化-气相色谱法检测人乳中持久性有机氯农药

Detection of persistent organochlorine pesticides in human milk by solid-phase extraction and gas chromatography

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 detection method of organochlorine pesticides in human milk and to analyse their concentration in mature human milk from Beijing, Lanzhou and Hangzhou. Methods Human milk samples were extracted with acetonitrile. After purification and enrichment with acidificated silicone solid phase extraction column, the samples were analyzed by using gas chromatography. Results Linear ranges of eight pesticides were between 5 and 200 ng/mL, the correlation coefficients were 0.9955~0.9994, the limits of quantification were below 2.6 μg/kg. The average recoveries were 70%~122%, relative standard deviations were 3.91%~10.77%. Conclusion The matrix can be completely removed from human milk by combining usage of acidification and solid phase extraction. A method validation showed that this simple, accurate and rapid method was suitable for the analysis of the organochlorine pesticides in human milk. Since the usage of organochlorine pesticides are forbidden, the accumulation level of organochlorine pesticides in the human milk are decreased obviously.