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首页> 外文期刊>Journal of AOAC International >Sample preparation based on matrix solid-phase dispersion and solid-phase extraction cleanup for the determination of organochlorine pesticides in fish.
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Sample preparation based on matrix solid-phase dispersion and solid-phase extraction cleanup for the determination of organochlorine pesticides in fish.

机译：基于基质固相分散和固相萃取净化的样品前处理用于测定鱼中的有机氯农药。

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A method based on matrix solid-phase dispersion (MSPD) and SPE to determine 20 organochlorine pesticides (OCPs) in fish tissues (muscle and liver) was optimized in terms of the sorbents and elution solvents used for the analysis. The following analytical components were evaluated: ENVI-CarbTM and ENVI-18 as dispersing agents, Florisil and Florisil over alumina as cleanup adsorbents and hexane and hexane-ethyl acetate (80 + 20) as elution solvents. The pesticides were determined by GC with electron capture detection. The best results were obtained with ENVI-Carb as a dispersing agent and an ENVI-FlorisilReg. co-column using 40 ml hexane-ethyl acetate (80 + 20) as the elution solvent. Analytical recoveries ranged between 75 and 130%, except for beta-HCH in fish liver, and the RSD values were <15% for most of the pesticides studied. Furthermore, sensitivity was sufficient (LOD of <300 mg/kg) for all OCPs under study, in compliance with the tolerance limits of the US FDA for OCPs in fish. The results were compared with those obtained by microwave-assisted extraction (MAE) and pressurized liquid extraction (PLE) in order to evaluate the performance of the MSPD procedure. The MPSD methodology was shown to be easy to use and fast, with a clear advantage relative to cost, because it does not need the expensive equipment required for MAE and PLE.
机译：根据用于分析的吸附剂和洗脱溶剂，优化了一种基于基质固相分散体（MSPD）和SPE的方法来测定鱼类组织（肌肉和肝脏）中的20种有机氯农药（OCP）的方法。评价了以下分析成分：ENVI-CarbTM和ENVI-18作为分散剂，Florisil和Florisil在氧化铝上作为清洁吸附剂，己烷和己烷-乙酸乙酯（80 + 20）作为洗脱溶剂。通过电子捕获检测GC测定农药。使用ENVI-Carb作为分散剂和ENVI-FlorisilReg可获得最佳结果。使用40 ml己烷-乙酸乙酯（80 + 20）作为洗脱溶剂的色谱柱。除鱼肝中的乙型六氯环己烷外，分析回收率介于75％至130％之间，并且大多数所研究的农药的RSD值均<15％。此外，对所有正在研究的OCP来说，灵敏度都足够（LOD <300 mg / kg），符合美国FDA对鱼类中OCP的耐受极限。将结果与通过微波辅助萃取（MAE）和加压液体萃取（PLE）获得的结果进行比较，以评估MSPD程序的性能。事实证明，MPSD方法易于使用且速度快，相对于成本具有明显优势，因为它不需要MAE和PLE所需的昂贵设备。

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