Duodu Godfred Odame, Goonetilleke Ashantha, Ayoko Godwin A
Queensland University of Technology (QUT), Science and Engineering Faculty, School of Chemistry, Physics and Mechanical Engineering, 2 George St, 4001 QLD, Australia.
Queensland University of Technology (QUT), Science and Engineering Faculty, School of Civil Engineering and Built Environment, 2 George St, 4001 QLD, Australia.
Talanta. 2016 Apr 1;150:278-85. doi: 10.1016/j.talanta.2015.12.049. Epub 2015 Dec 19.
Organochlorine pesticides (OCPs) are ubiquitous environmental contaminants with adverse impacts on aquatic biota, wildlife and human health even at low concentrations. However, conventional methods for their determination in river sediments are resource intensive. This paper presents an approach that is rapid and also reliable for the detection of OCPs. Accelerated Solvent Extraction (ASE) with in-cell silica gel clean-up followed by Triple Quadrupole Gas Chromatograph Mass Spectrometry (GCMS/MS) was used to recover OCPs from sediment samples. Variables such as temperature, solvent ratio, adsorbent mass and extraction cycle were evaluated and optimized for the extraction. With the exception of Aldrin, which was unaffected by any of the variables evaluated, the recovery of OCPs from sediment samples was largely influenced by solvent ratio and adsorbent mass and, to some extent, the number of cycles and temperature. The optimized conditions for OCPs extraction in sediment with good recoveries were determined to be 4 cycles, 4.5 g of silica gel, 105 °C, and 4:3 v/v DCM: hexane mixture. With the exception of two compounds (α-BHC and Aldrin) whose recoveries were low (59.73 and 47.66% respectively), the recovery of the other pesticides were in the range 85.35-117.97% with precision <10% RSD. The method developed significantly reduces sample preparation time, the amount of solvent used, matrix interference, and is highly sensitive and selective.
有机氯农药（OCPs）是普遍存在的环境污染物，即使在低浓度下也会对水生生物群、野生动物和人类健康产生不利影响。然而，传统的河流沉积物中有机氯农药测定方法资源消耗大。本文提出了一种快速且可靠的有机氯农药检测方法。采用加速溶剂萃取（ASE）结合柱内硅胶净化，然后进行三重四极杆气相色谱 - 质谱联用（GCMS/MS），从沉积物样品中回收有机氯农药。对温度、溶剂比例、吸附剂质量和萃取循环次数等变量进行了评估和优化。除艾氏剂不受所评估的任何变量影响外，沉积物样品中有机氯农药的回收率在很大程度上受溶剂比例和吸附剂质量影响，在一定程度上还受循环次数和温度影响。确定沉积物中有机氯农药萃取的优化条件为4次循环、4.5克硅胶、105℃以及二氯甲烷：己烷体积比为4:3的混合溶剂。除两种化合物（α - 六六六和艾氏剂）回收率较低（分别为59.73%和47.66%）外，其他农药的回收率在85.35 - 117.97%之间，精密度相对标准偏差（RSD）<10%。所开发的方法显著减少了样品制备时间、溶剂用量、基质干扰，且具有高灵敏度和选择性。
