海洋沉积物中有机氯农药的微波提取技术研究
首发时间:2008-04-23
摘要:建立了微波提取海洋沉积物样品中有机氯农药的气相色谱-电子捕获检测器(GC-ECD)的检测方法。对海洋沉积物样品中有机氯农药微波提取影响因素进行了研究,如提取剂类型、微波提取时间、微波提取温度以及微波功率等。结果表明,在微波功率为500W、提取温度为70℃的条件下,用50mL体积比为3:2的丙酮-正己烷混合液,提取海洋沉积物样品20min,有机氯农药的平均回收率在75.43%~97.51%之间,相对标准偏差在0.89%~5.18%之间,检出限在0.052×10-9~0.581×10-9之间;微波提取法与索氏提取法相当,具有较好的准确度和灵敏度。
关键词: 海洋沉积物 有机氯农药 微波提取 气相色谱-电子捕获检测器
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Study on Organochlorine Pesticides in Marine Sediments by Microwave Extraction
Abstract:This paper introduces a method for determination of organochlorine pesticides (OCPs) in the sample of marine sediments by microwave extraction (ME) and gas chromatography with electric capture detector (GC-ECD). The determination of organochlorine pesticides in the marine sediments with gas chromatography-electric capture detector is founded by the parameters of microwave extraction being optimized with a series of experiments on influence of factors such as the kinds of extractant, time of extraction, the power and temperature of extraction. Meanwhile, microwave extraction are compared with Soxhlet extraction for organochlorine pesticides in the marine sediments.The results show the microwave extraction method has good precision and accuracy and sensitivity under the optimum conditions including the power of 500 watt, the temperature at 70℃,the time for 20 minutes, the extractant of 50 mL acetone-hexane mixture of volume ratio from three to two,and the ranges of the average recoveries of organochlorine pesticides in marine sediments with the microwave extraction are from 75.43% to 97.51%, and the ranges of relative standard deviation are from 0.89% to 5.18%, and the ranges of the limits of detection for the method are from 0.052×10-9 to 0.581×10-9.
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