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建立了加速溶剂萃取、全自动在线凝胶渗透色谱-浓缩联用系统和氟罗里硅土柱前处理、GC/ECD测定小麦样品中7种多氯联苯(PCBs)和7种有机氯农药(OCPs)的分析方法,并优化了加速溶剂萃取、凝胶渗透色谱净化、GC/ECD的分析条件。结果表明,该方法的样品加标回收率和相对标准偏差分别为:多氯联苯69.8%～87.4%1、.48%～11.0%;有机氯农药70.4%～113.9%3、.54%～17.0%。方法检测限为0.03～0.29μg/kg。用该方法测得小麦样品中7种PCBs质量分数范围为0～157.9μg/kg;7种OCPs质量分数在2.38～10.02μg/kg范围内。该方法快速、灵敏、准确,并且在一个流程中可以同时测定小麦样品中多氯联苯和有机氯农残,适合于大批量样品的测定。
Accelerated solvent extraction, automatic on-line gel permeation chromatography-concentration combined system, and pre-treatment with Florisil silica column were established. Seven kinds of polychlorinated biphenyls (PCBs) and seven organochlorine pesticides (OCPs), and optimize the conditions of accelerated solvent extraction, gel permeation chromatography purification and GC / ECD analysis. The results showed that the recoveries and relative standard deviations (RSDs) of the samples were 69.8% ~ 87.4% 1, 48% ~ 11.0%, 70.4% ~ 113.9%, 3.54% 17.0%. The detection limit was 0.03 ~ 0.29μg / kg. Using this method, the mass fractions of seven PCBs in wheat samples ranged from 0 to 157.9 μg / kg, and the seven OCPs mass fractions ranged from 2.38 to 10.02 μg / kg. The method is fast, sensitive and accurate, and can simultaneously determine PCBs and organochlorine residues in wheat samples in one process, which is suitable for the determination of large quantities of samples.