Solid-phase Extraction Of Polycyclic Aromatic Hydrocarbons Research Articles

Determination of anthracene, phenanthrene, and fluorene in tap water and sediment samples by fluorescence spectroscopy on nylon membranes and second-order calibration

A fast and sensitive strategy was developed for the quantification of anthracene (ANT), phenanthrene (PHE), and fluorene (FLU), which are polycyclic aromatic hydrocarbons (PAHs), in tap water and sediment samples. In this method, solid-phase extraction of PAHs on a nylon membrane was accomplished by filtration using a lab-made propulsion system. Fluorescent signals were measured on the non-pressurized membrane surface. Parallel factor analysis (PARAFAC) was used to model the tridimensional tensors of excitation-emission fluorescence matrices and resolve spectral overlapping between samples and concomitants. PAHs mass transfer across the membrane was increased by adding methanol to sample solutions. Matrix interferences were effectively modeled using PARAFAC under optimized conditions, providing precise and accurate results. Study results, such as recovery percentages between 91% and 104%, root mean square error of prediction (RMSEP) values between 0.034-0.87 and 25–264), and limit of detection (LD) values between 0.11-0.62 and 10.6–94.2 for water (μg L−1) and sediment (μg kg−1) samples, respectively, indicate that the proposed method can be used to successfully quantify PAHs in real samples.

Preparation of graphene oxide incorporated monolithic chip based on deep eutectic solvents for solid phase extraction

A monolithic chip incorporated with graphene oxide (GO) based on deep eutectic solvents (DESs) was developed for solid phase extraction (SPE). The carboxylated GO was modified with p-aminostyrene (pAS) by amidation, and the obtained GO (pAS–COOH–GO) was covalently incorporated into poly(butyl methacrylate-co-ethylene glycol dimethyl methacrylate) monolithic chip. Due to the high viscosity characteristics of DESs, a uniform pAS–COOH–GO incorporated monolithic chip with good permeability can be achieved. A systematic study of the preparation parameters on the performance of the resulting monolith was carried out, including the content of pAS–COOH–GO, DESs composition and porogen ratio. The resulting pAS–COOH–GO incorporated monolith was characterized by nitrogen adsorption, scanning electron microscopy, and transmission electron microscopy. The GO-doped monolithic chip can be used for SPE of polycyclic aromatic hydrocarbons (phenanthrene, anthracene, fluoranthene, pyrene, benzo(a)anthracene, benzo(a) pyrene, dibenzo(a,h)anthracene and inden(1,2,3,-cd)pyrene). The recoveries were all higher than 90%, which was about twice as high as that of the monolithic chip prepared without GO. By comparing the SPE results with that of GO free monolithic chip, good enrichment effects were demonstrated on the pAS–COOH–GO incorporated monolithic chip.

Etched Stainless Steel Powder as Novel Sorbent Material for Solid-Phase Extraction Coupled with High-Performance Liquid Chromatography for Determination of Polycyclic Aromatic Hydrocarbons in Water

The etched stainless steel powder was prepared and explored as sorbent material for solid-phase extraction coupled with high-performance liquid chromatography (HPLC) for determination of trace polycyclic aromatic hydrocarbons (PAHs) in environmental matrices. The etched stainless steel powder was shown to be promising for solid-phase extraction of PAHs in environmental samples with subsequent HPLC separation and UV detection. This paper explored different factors that affected the adsorption efficiency of etched stainless steel powder, including the etched time of stainless steel powder, the mass of sorbent, and the volume of water sample, and so on. In the optimum conditions, nine kinds of PAHs, including trace naphthalene, acenaphthylene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzanthracene and benzopyrene, were extracted by etched stainless powder and the extraction efficiency is satisfactory.

Ultrasonic assisted extraction combined with titanium-plate based solid phase extraction for the analysis of PAHs in soil samples by HPLC-FLD

In this work, ultrasonic assisted extraction combined with solid phase extraction (SPE) was applied in the analysis of polycyclic aromatic hydrocarbons (PAHs) in environment samples. A titania nanotubes/titanium plate was modified with n-octadecanethiol monolayer-protected Ag nanoparticles, and developed as the adsorbent in SPE of PAHs. Six different PAHs in soil samples were analyzed with high performance liquid chromatography-fluorescence detection. The experiment conditions including the deposition time of Ag nanoparticles, extraction solvent properties, the amount of extraction solvent, the amount of organic modifier, extraction time, and desorption solvent properties were optimized. Under the optimized conditions, good linearity and low limits of detection of 0.0015–0.4ngg−1 were obtained. The analysis of PAHs in real soil samples gave satisfactory recoveries ranging from 70.32% to 115.51% with 3.14%–13.56% intra-day relative standard deviations (RSD) and 4.92%–14.87% inter-day RSD.

Porous metal membranes for solid-phase extraction of polycyclic aromatic hydrocarbons

Solid-phase extraction (SPE) is one of the most important techniques for sample preparation, purification, concentration and cleanup. Membranes made from synthetic organic polymers, cellulose, or glass fibers are used for sample pretreatment. In this work, we report that a porous metal membrane, the metal filter in HPLC, was used as a novel kind of solid-phase extraction adsorbent material. To evaluate the performance of the porous metal membrane for the SPE, naphthalene, fluorene, anthracene, phenanthrene, fluoranthene, pyrene, chrysene, perylene and benzo(a)pyrene were selected as analytes. Several parameters that affected the extraction efficiency such as the extraction time, the concentration of NaCl, the extraction temperature and the agitation speed were optimized. The experimental result indicates that the porous metal membrane possesses high adsorption ability to the tested polycyclic aromatic hydrocarbons (PAHs). Under the optimum conditions, the detection limits of the developed method were in the range of 0.03-0.082 μg L(-1) (S/N = 5), and excellent linear correlations between peak area and concentration of PAHs were found over the range of 0.1-60 μg L(-1). The precisions (RSD) for five replicate extractions of the PAHs from sample solutions were in the range of 2.6-5.0%. The recoveries of the PAHs from tap water and river water samples spiked with 9 PAHs (20 μg L(-1) of each individual PAH) ranged from 83.0% to 112.5%. The porous metal membrane is durable, simple, inexpensive, reproducible and has a high adsorption ability for use in SPE of PAHs.

Influence of natural organic matter on the solid-phase extraction of organic micropollutants: Application to the water-extract from highly contaminated river sediment

In freshwater systems, organic micropollutants are bound to natural organic matter (NOM), which is responsible for a decrease in their recoveries by solid-phase extraction (SPE). This “negative effect” has been investigated for the SPE of polycyclic aromatic hydrocarbons (PAHs), oxygenated PAHs, nitrated PAHs and n-alkanes from salt water using Aldrich humic acid as a model of NOM. The effect has been partially obviated by the addition of isopropanol as a surfactant. The SPE protocol, developed with isopropanol, has been applied to the water-extract of a highly contaminated sediment. The water-extract has been size fractionated by cross-flow ultrafiltration into particulate (PM), colloidal (CM) and truly dissolved matter (tDM). Organic extracts from SPE experiments have been analyzed by gas chromatography–mass spectrometry. The major classes of molecules are heteroaromatic PAHs and PAHs. Those molecules are mainly bound to the tDM, which highlights: (1) the competition between organic micropollutants and natural organic molecules for available sorption sites and (2) the toxicological hazard linked to the mobilization of sediments highly contaminated by both industrial and urban activities.