通过考察提取溶剂、毛细管柱、净化条件及共溶出干扰物等因素对十氯酮测定的影响,建立了二氯甲烷液-液富集萃取、硫酸净化分离、气相色谱法(GC)-电子捕获检测器(ECD)测定海水介质中有机氯农药类持久性有机污染物十氯酮残留分析方法.1L海水经50 mL二氯甲烷萃取富集,浓缩后采用硫酸净化,以1%(体积分数)甲醇/正己烷混合溶液转移定容后,采用DB-5非极性毛细管柱进行GC分离,电子捕获检测器可测定其中十氯酮的含量;该方法采用外标法定量,在5~100 μg/L范围内呈线性,线性相关系数为0.998 9.低、中、高3个浓度水平的平均加标回收率为81% ~ 108%,相对标准偏差为1.2% ~5.1%(n=6).方法的检出限为0.6 ng/L.结果表明,该方法灵敏度高,线性关系好,可以满足简便、快速、准确测定海水中十氯酮的要求.
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