Department of Analytical Chemistry, University of A Coruña, Campus da Zapateira, E-15071 A Coruña, Spain.
Chemosphere. 2010 Apr;79(7):698-705. doi: 10.1016/j.chemosphere.2010.02.052. Epub 2010 Mar 17.
This work proposes a pressurized hot water extraction (PHWE) followed by solid phase microextraction (SPME) and determination by gas chromatography-mass spectrometry method for the analysis of organochlorine pesticides in sediment samples. For SPME, extraction temperature and time, desorption temperature and desorption time, and effect of an organic modifier were studied. For PHWE, parameters such as organic modifier, percentage of organic modifier, temperature, and static extraction time were studied. When these parameters were selected, the figures of merit were calculated in order to assess the performance of the proposed method. Quantitative recoveries (80-115%) and satisfactory precisions were obtained. The detection and quantification limits were between 0.11 and 16 microg kg(-1) and between 0.24 and 22 microg kg(-1), respectively with good linearity between LOQs and 500 microg kg(-1) for most of the studied pesticides. The method was validated by the analysis of a reference marine sediment material (SRM 1944). The obtained results are in excellent agreement with the certificate material. Another sediment reference material (SRM 1941b), with a very low concentration of pesticides was also analyzed with good results. In addition, this method was successfully applied to the analysis of three marine sediment samples. The developed method seems to be a nearly full automated, environmental friendly, sensitive, simple and less-time consuming method. Moreover this method, look for the implementation of the principles of green analytical chemistry and has demonstrated to be suitable for the analysis of organochlorine pesticides at trace levels in environmental matrices as sediment samples.
本工作提出了一种加压热水提取（PHWE），随后采用固相微萃取（SPME）和气相色谱-质谱法分析沉积物样品中的有机氯农药。对于 SPME，研究了萃取温度和时间、解吸温度和时间以及有机改性剂的影响。对于 PHWE，研究了有机改性剂、有机改性剂的百分比、温度和静态萃取时间等参数。选择这些参数后，计算了特征值以评估所提出方法的性能。得到了定量回收率（80-115%）和令人满意的精密度。检测限和定量限分别在 0.11 和 16 μg kg(-1)之间以及在 0.24 和 22 μg kg(-1)之间，对于大多数研究的农药，在 LOQs 和 500 μg kg(-1)之间具有良好的线性关系。该方法通过对参考海洋沉积物材料（SRM 1944）的分析进行了验证。得到的结果与证书材料非常吻合。还对另一种农药浓度非常低的沉积物参考材料（SRM 1941b）进行了很好的分析。此外，该方法还成功地应用于三种海洋沉积物样品的分析。该方法似乎是一种几乎完全自动化、环境友好、灵敏、简单且耗时较短的方法。此外，该方法符合绿色分析化学原则，适用于痕量环境基质（如沉积物样品）中有机氯农药的分析。
