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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Pressurized hot water extraction coupled to solid-phase microextraction-gas chromatography-mass spectrometry for the analysis of polycyclic aromatic hydrocarbons in sediments
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Pressurized hot water extraction coupled to solid-phase microextraction-gas chromatography-mass spectrometry for the analysis of polycyclic aromatic hydrocarbons in sediments

机译:加压热水萃取-固相微萃取-气相色谱-质谱联用分析沉积物中的多环芳烃

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摘要

A fully automated, environmentally friendly, simple, and sensitive method was developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) in sediment samples. The procedure is based on pressurized hot water extraction (PHWE) followed by solid-phase microextraction (SPME) and determination by gas chromatography-mass spectrometry. For PHWE, parameters such as organic modifier, percentage of organic modifier, temperature, and static extraction time were studied. For SPME, extraction temperature and time, desorption temperature and time, splitless time, ionic strength adjustments, and effect of an organic modifier were studied. When these parameters were selected, the figures of merit were calculated. The detection and quantification limits were between 0.4-15 mu g kg(-1) and 1.2-51 mu g kg(-1), respectively. The linearity of the method was assessed spiking sediment samples at seven levels of concentration ranged between 2.5 mu g kg(-1) and 500 mu g kg(-1) for most of the studied PAHs. The method was validated by two concentration levels reference marine sediment materials (SRM 1944 and SRM 1941b). The obtained results are in very good agreement with the certificate materials. The developed method seems to be suitable for the analysis of PAHs at ultratrace levels in environmental matrices as sediment samples.
机译:开发了一种全自动,环保,简单而灵敏的方法来分析沉积物样品中的多环芳烃(PAH)。该程序基于加压热水萃取(PHWE),然后进行固相微萃取(SPME),并通过气相色谱-质谱法测定。对于PHWE,研究了诸如有机改性剂,有机改性剂百分比,温度和静态萃取时间等参数。对于SPME,研究了萃取温度和时间,解吸温度和时间,不分流时间,离子强度调节以及有机改性剂的效果。选择这些参数后,将计算品质因数。检出限和定量限分别在0.4-15μg kg(-1)和1.2-51μgkg(-1)之间。对于大多数研究的多环芳烃而言,该方法的线性是在浓度范围介于2.5μg kg(-1)和500μg kg(-1)之间的七个浓度水平下评估掺加沉积物样品的。两种浓度水平参考海洋沉积物材料(SRM 1944和SRM 1941b)验证了该方法。获得的结果与证书材料非常吻合。所开发的方法似乎适合于在环境基质中作为沉积物样品以超痕量分析多环芳烃。

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