Carro Nieves, García Isabel, Ignacio María, Mouteira Ana
INTECMAR, Instituto Tecnolóxico para o Control do Medio Mariño de Galicia, Consellería de Pesca e Asuntos Marítimos, Xunta de Galicia, Peirao de Vilaxoán s/n., 36611 Vilagarcía de Arousa, Pontevedra, Spain.
Anal Bioanal Chem. 2006 Jul;385(5):901-9. doi: 10.1007/s00216-006-0485-3. Epub 2006 May 17.
Microwave-assisted solvent extraction of persistent organochlorine pesticides (POPs) in marine sediment was developed and optimized by means of two-level factorial designs. Six variables (microwave power, extraction time and temperature, amount of sample, solvent volume, and sample moisture) were considered as factors in the optimization process. The results show that the amount of sample to be extracted and solvent volume are statistically significant for the overall recovery of the studied pesticides, although compromise conditions have to be established with the object of avoiding overpressure in closed vessels. After extraction, a clean up step including the use of a silica cartridge was performed prior to chromatographic determination in order to remove interferences. The optimized procedure was compared to conventional Soxhlet extraction. The MS-MS ion preparation mode was applied to improve the sensitivity and selectivity of the chromatographic technique.
采用二水平析因设计对微波辅助溶剂萃取海洋沉积物中持久性有机氯农药（POPs）的方法进行了开发和优化。在优化过程中，将六个变量（微波功率、萃取时间和温度、样品量、溶剂量和样品含水量）视为因素。结果表明，尽管为避免密闭容器中出现超压需要确定折衷条件，但对于所研究农药的总体回收率而言，待萃取的样品量和溶剂量具有统计学意义。萃取后，在进行色谱测定之前，采用硅胶柱进行净化步骤以去除干扰物。将优化后的方法与传统索氏萃取法进行了比较。采用MS-MS离子制备模式提高了色谱技术的灵敏度和选择性。
