为快速准确检测土壤中21种低浓度多氯联苯(PCBs)的含量,建立了以丙酮-正己烷(1:1,V/V)为萃取剂超声提取,四通道色谱分离仪对提取液进行分离和净化的前处理方法。采用氮吹法将前处理的样品浓缩至50斗L以下,以PCB54作为内标。利用气相色谱一郇Ni微电子捕获检测器(GC—ECD)进行定量测定。土壤中21种PCBs的回收率为68.6%~102.3%,相对标准偏差为2.2%.9.9%,方法检出限为1.21—4.67μg/kg。采用所建方法对长江三角洲地区经长期植物修复后的PCBs污染土壤和无污染的农田土壤进行检测,结果显示,修复后的土壤PCBs总量为99.884-3.97μg/kg,无污染农田土壤PCBs总量为69.01±2.19μg/kg。
A quick method for the determination of low levels of 21 polychlorinated biphenyls (PCBs) in soil samples was established under the condition of quality assurance/quality control (QA/QC). PCBs in micro soil samples were extracted with a mixture of hexane - acetone ( 1 : 1, V/V) by ultra-phonic technique, and then were purified by four-channel purification chromatograph, which was developed independently in our laboratory. Extracts were concentrated to 50 μL under a gentle nitrogen stream and detected by GC-ECD with the internal standard PCB 54. The recoveries rates, RSD (relative standard deviations) and MDL( method detection limits) for 21 PCBs were 68.6% ~ 102. 3% , 2. 2% - 9.9% , and 1.21 - 4.67 μg/kg, respectively, which met the demands for US EPA PCBs recoveries. PCBs contaminated soil after long-term phytoremediation in the Yangtze River Delta and non-contaminated farmland soil in the same area were detected by this method. The total concentrations of PCBs in two soil samoles were 99.88 ± 3.97 μg/kg and 69.01 ± 2. 19μg/kg respectively.