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Simultaneous extraction of polycyclic aromatic hydrocarbons and polychlorinated biphenyls in agricultural soils by pressurized liquid extraction and determination by gas chromatography coupled to tandem mass spectrometry

机译:加压液体萃取-气相色谱-串联质谱法同时测定农业土壤中多环芳烃和多氯联苯

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摘要

A simple and rapid method based on pressurized liquid extraction has been validated for the simultaneous extraction of polychlorinated biphenyls (PCBs) and polycyclic aromatic hydrocarbons (PAHs) from agricultural soil samples. Effective extraction was carried out in less than 17 min for all the studied compounds, and good recoveries were obtained for PAHs and PCBs, ranging from 70% to 112%, when blank samples were spiked at 2.5 μg kg~(-1), except for naphthalene with recoveries close to 40%. The separation and determination were performed by gas chromatography coupled to tandem mass spectrometry using a triple quadrupole mass analyzer. The target compounds were detected by electron impact with selected reaction monitoring, and mass spectrometric conditions were optimized in order to increase selectivity and sensitivity. The developed method was validated, and matrix-matched calibration was used for quantification purposes. Repeatability and interday precision ranged from 0.9% to 16.8% and from 1.6% to 22.3%, respectively. Limits of quantification ranged from 0.07 to 2.50 μg kg~(-1). The proposed method was applied to the analysis of agricultural soil samples collected from Almeria (Spain), and PAHs and PCBs were detected in some samples at concentrations ranging from 0.1 to 210 μg kg~(-1).
机译:已经验证了一种基于加压液体萃取的简单,快速的方法,可以从农业土壤样品中同时萃取多氯联苯(PCB)和多环芳烃(PAH)。所有空白化合物的有效萃取均在不到17分钟的时间内进行,当空白样品的浓度为2.5μgkg〜(-1)时,多环芳烃和多氯联苯的回收率在70%至112%范围内。萘的回收率接近40%。分离和测定是通过使用三重四极杆质量分析仪的气相色谱与串联质谱联用进行的。通过电子碰撞和选定的反应监测来检测目标化合物,并优化质谱条件以提高选择性和灵敏度。验证了开发的方法,并将基质匹配的校准用于定量目的。重复性和日间精度分别为0.9%至16.8%和1.6%至22.3%。定量限为0.07至2.50μgkg〜(-1)。该方法用于从西班牙阿尔梅里亚省采集的农业土壤样品的分析,并且在一些样品中检测到的PAHs和PCBs的浓度范围为0.1至210μgkg〜(-1)。

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