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首页> 外文期刊>Analytical methods >Automated pressurized liquid extraction (PLE) and automated power-prep~(TM) clean-up for the analysis of polycyclic aromatic hydrocarbons, organo-chlorinated pesticides and polychlorinated biphenyls in marine samples
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Automated pressurized liquid extraction (PLE) and automated power-prep~(TM) clean-up for the analysis of polycyclic aromatic hydrocarbons, organo-chlorinated pesticides and polychlorinated biphenyls in marine samples

机译：自动化加压液体萃取（PLE）和自动化power-prep™净化技术，用于分析海洋样品中的多环芳烃，有机氯农药和多氯联苯

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An accurate and precise analytical method for the determination of polychlorinated biphenyls (PCBs), polycyclic aromatic hydrocarbons (PAHs), and organo-chlorinated pesticides (OCPs) in fish and shellfish based on automated pressurized liquid extraction (PLE) and automated power-prep~(TM) clean-up has been developed. After extraction, the extract was passed through gel permeation chromatography (GPC) using 12 g of Bio-beads SX-3 for fat removal. GC/MS (NCI) was selected for OCPs and PCBs due to its high sensitivity and selectivity of NCI to chlorinated compounds and GC/MS (El) for PAHs. The method was validated using spiked surrogates of ~(13)C-PCBs, deuterated PAH (d-PAHs) and fish reference material (EDF-2525). All of the recoveries are within the acceptance levels and in accordance with the US-EPA standard methods. The calibration ranges for most of the compounds were from 50 to 1000 μg ml~(-1) for PAHs, 10 to 103 μg ml~(-1) for PCBs and 10 to 200 μg ml~(-1) for OCPs. The limits of detection ranged between 0.01 and 0.28 μg g~(-1) (w/w) for PCBs, 0.03-2.48 μg g~(-1) (w/w) for OCPs and 0.1 to 1.0 μg g~(-1) (w/w) for PAHs. Analytical criteria, such as repeatability and reproducibility were evaluated through a range of biological matrices and fish reference material analysis. The feasibility of extraction using a power-prep~(TM)/PLE system combined with power-prep~(TM) automated clean-up demonstrated a validated method for the analysis of biota samples.
机译：一种基于自动加压液体萃取（PLE）和自动电源制备技术来测定鱼和贝类中多氯联苯（PCB），多环芳烃（PAH）和有机氯农药（OCP）的准确而精确的分析方法〜 （TM）清理已开发。提取后，将提取物通过凝胶渗透色谱（GPC），使用12 g Bio-beads SX-3去除脂肪。 GC / MS（NCI）被选作OCP和PCB的原因是NCI对氯化物的敏感性和选择性高，而PAHs的GC / MS（E1）具有很高的选择性。使用〜（13）C-PCBs的加标替代物，氘代PAH（d-PAHs）和鱼类参考材料（EDF-2525）验证了该方法。所有回收率均在接受水平之内，并符合US-EPA标准方法。大多数化合物的校准范围对于PAHs为50至1000μgml〜（-1），对于PCBs为10至103μgml〜（-1），对于OCP为10至200μgml〜（-1）。 PCB的检测限范围为0.01至0.28μgg〜（-1）（w / w），OCP的检测限为0.03-2.48μgg〜（-1）（w / w），而0.1至1.0μgg〜（- 1）（w / w）多环芳烃。通过一系列生物基质和鱼类参考物质分析评估了分析标准，例如重复性和再现性。使用power-prep- / PLE系统结合power-prep-TM自动净化进行萃取的可行性证明了一种用于分析生物样品的经验证的方法。

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