Quantitation Of Polycyclic Aromatic Hydrocarbons Research Articles

Rapid screening and quantitation of PAHs in water and complex sample matrices by solid-phase microextraction coupled to capillary atmospheric pressure photoionization-mass spectrometry.

A capillary atmospheric pressure photoionization (cAPPI) source was used to analyze polycyclic aromatic hydrocarbons (PAHs) in complex matrices like grilled meat extract and urban dust reference material, as well as screening for PAHs in aqueous samples such as tap and lake water. A high-throughput workflow was developed that allowed rapid screening of unknown samples by direct solid-phase microextraction (SPME) coupled with cAPPI-MS, with confirmatory gas chromatography performed only for samples containing trace amounts of PAHs. Extraction times were as low as 15 s, with a total analysis time of 2 min per sample for screening. Limits of detections were in the low pg/ml range and in the subpg/ml range for the direct and chromatographic approach, respectively, with a linear dynamic range between two and three orders of magnitude, as determined for 15 model PAHs. This rapid approach represents an attractive way to screen samples containing nonpolar compounds using an ambient ionization source.

Quantitation of Polycyclic Aromatic Hydrocarbons and Organochlorine Pesticides in Surface Waters

We develop an assay for the total content of xenobiotics from the polyaromatic hydrocarbon (PAH) and organochlorine pesticide (OCP) groups in samples of surface water containing suspended matter. It is found that the suspended matter isolated from water by filtration during sample preparation according to standard method ISO 5667:2006 may contain PAH and OCP xenobiotics. The xenobiotics containing in the filtrate and suspended matter isolated from water samples are extracted with n-hexane. After the extracts are concentrated by a factor of 250–1000, their qualitative and quantitative composition is determined by high-performance liquid phase chromatography with fluorescence detection and by gas chromatography mass spectrometry. For water samples, the limit of quantitation (LOQ) for OCP and PAH xenobiotics is found to be 0.1 and 0.005 μg/L, respectively, and in case of the suspended matter samples the LOQs are 0.1 and 0.005 ng/g. The determination error is expressed as the relative standard (mean-square) deviation Sr (%), and the completeness of xenobiotic extraction is expressed in per cents (r, %). The method is tested on samples of surface waters containing suspended matter in the range of 90 ± 10 to 2800 ± 50 mg/L. The developed method enables us to detect trace amounts of xenobiotics in water and in suspended matter in it. The method can be useful in studies of surface waters and in forecasting the level of contamination of aquatic environments with PAHs and OCPs released as a result of degradation of suspended matter that binds the xenobiotics.

Magnetic fiber headspace solid-phase microextraction coupled to GC-MS for the extraction and quantitation of polycyclic aromatic hydrocarbons.

A technique was developed for magnetic fiber headspace-solid phase microextraction (MF-HS-SPME) of polycyclic aromatic hydrocarbons (PAHs). The efficiency of the extraction of a steel SPME fiber coated with an aminoethyl-functionalized SBA-15 (Santa Barbara Amorphous 15; a nanoporous sorbent) is substantially improved after its magnetization during HS-SPME. The effects of magnetic field strength, extraction temperature, extraction time, moisture content of the sample, desorption time and desorption temperature were optimized using a simplex method. The application of a moderately strong magnetic field to the fiber results in up to 135% increase in the extraction efficiency and wider linear dynamic ranges. The PAHs (specifically naphthalene, acenaphthene, fluorene, anthracene, phenanthrene, fluoranthene and pyrene) were then quantified by GC-MS analysis. Comparison of an electromagnet and a permanent magnet indicated the superior effect of the permanent magnet for the target analytes due to the Ohmic heating of the magnetic coil and its negative effect on the extraction of some of the PAHs. The limits of detections of the PAHs are between 0.17 to 0.57ngg-1 by using the electromagnet, and between 0.10 and 0.32ngg-1 for the permanent magnet. Relative standard deviations of 2.9 to 7.6% were obtained for six replicated analyses of the analytes. The method was applied to some polluted soil samples, and satisfactory results were obtained. Graphical abstract Schematic representation of the designed magnetic fiber headspace solid-phase microextraction (MF-HS-SPME) system using (a) an electromagnet, (b) a pair of permanent disc magnets.

Feasibility of Multidimensional Fluorescence at Low Temperature in Shpol'skii Matrices Combined with PARAFAC for the Quantitation of Polycyclic Aromatic Hydrocarbons

Feasibility of Multidimensional Fluorescence at Low Temperature in Shpol'skii Matrices Combined with PARAFAC for the Quantitation of Polycyclic Aromatic Hydrocarbons

Evaluation of the impact of peak description on the quantitative capabilities of comprehensive two-dimensional liquid chromatography

Comprehensive, two-dimensional liquid chromatography (LC×LC) is a powerful technique for the separation of complex mixtures. Most studies using LC×LC are focused on qualitative efforts, such as increasing peak capacity. The present study examined the use of LC×LC–UV/vis for the separation and quantitation of polycyclic aromatic hydrocarbons (PAHs). More specifically, this study evaluated the impact of different peak integration approaches on the quantitative performance of the LC×LC method. For well-resolved three-dimensional peaks, parameters such as baseline definition, peak base shape, and peak width determination did not have a significant impact on accuracy and precision. For less-resolved peaks, a dropped baseline and the summation of all slices in the peak improved the accuracy and precision of the integration methods. The computational approaches to three-dimensional peak integration are provided, including fully descriptive, select slice, and summed heights integration methods, each with its own strengths and weaknesses. Overall, the integration methods presented quantify each of the PAHs within acceptable precision and accuracy ranges and have comparable performance to that of single dimension liquid chromatography.

Four-way modeling of 4.2 K time-resolved excitation emission fluorescence data for the quantitation of polycyclic aromatic hydrocarbons in soil samples

A screening method for the soil analysis of 15 Environmental Protection Agency-polycyclic aromatic hydrocarbons (EPA-PAHs) is reported. The new method is based on the collection of 4.2K fluorescence time-resolved excitation–emission cubes (TREECs) via laser-excited time-resolved Shpol'skii spectroscopy. 4.2K fluorescence TREECs result from the superposition of fluorescence time-resolved excitation emission matrices recorded at different time windows from the laser excitation pulse. Potential interference from unknown sample concomitants is handled by processing the four-way 4.2K fluorescence TREEC data arrays with either parallel factor analysis (PARAFAC) or unfolded partial least-squares/residual-trilinearization(U-PLS/RTL). The sensitivity of the two approaches makes possible to determine PAHs at the ngg−1 to pgg−1 concentration level with no need for sample pre-concentration. Its selectivity eliminates sample clean-up steps and chromatographic separation. These features reduce PAH loss, analysis time and cost. The method is environmentally friendly as the complete screening of the 15 EPA-PAHs takes only 250μL of organic solvent per sample.

Picogram quantitation of polycyclic aromatic hydrocarbons adsorbed on aerosol particles by two-step laser mass spectrometry.

Polycyclic aromatic hydrocarbons (PAHs) are emitted into the atmosphere mostly by anthropogenic combustion sources. Because of their carcinogenic and mutagenic properties, PAHs are often analyzed in air quality measurements. Atmospheric concentrations of PAHs, typically in the nanograms-per-cubic-meter range, require significant effort for sample collection and processing when conventional methods such as gas chromatography/mass spectrometry (GC/MS) or liquid chromatography/mass spectrometry are used. In contrast, two-step laser mass spectrometry (L2MS) is highly sensitive and selective for PAHs and requires almost no sample preparation. Here, we present for the first time a method based on L2MS to quantify PAHs adsorbed on aerosol particles collected on a filter. Linear ranges for quantitation were determined for five different PAHs in the mass range of 178-276 Da (i.e., phenanthrene, pyrene, chrysene, benzo[e]pyrene, benzo[ghi]perylene) covering more than 2 orders of magnitude with detection limits between 50 and 300 pg of a single PAH on a whole filter sample. A quantitative comparison with GC/MS was performed using model aerosols consisting of benzo[e]pyrene adsorbed on inorganic salt aerosol particles. On average, 25% less benzo[e]pyrene was determined with GC/MS than with L2MS, with a variability between the two methods of +/-68%. The general lower amount measured with GC/MS is attributed to losses during the sample preparation for the GC/MS measurements.

Comparison of microprobe two-step laser desorption/laser ionization mass spectrometry and gas chromatography/ mass spectrometry studies of polycyclic aromatic hydrocarbons in ancient terrestrial rocks

Microprobe two-step laser desorption/laser ionization mass spectrometry (μL 2MS) and gas chromatography/mass spectrometry (GC/MS) were used to analyze polycyclic aromatic hydrocarbons (PAHs) in ancient terrestrial rocks. μL 2MS provides an in situ analysis of very small samples, records the PAHs with no isomer information, and gives quantitative data on the degree of alkylation of a given PAH series over the complete mass range. GC/MS provides isomer separation and quantitation of PAHs in bitumen but not kerogen, and is limited by sample size. Combination of these techniques allows analysis of very small samples by μL 2MS with GC/MS confirmation of isomer distributions of the solvent extractable components (bitumen). It was found that the concentration of bitumen within the rock samples affects the PAH alkylation signal for μL 2MS. At low bitumen concentrations μL 2MS can produce pyrolysis products from kerogen that is present; however, as bitumen concentrations increase, the PAH distribution from bitumen dominates the signal.

SFE-plus-C(18) lipid cleanup and selective extraction method for GC/MS quantitation of polycyclic aromatic hydrocarbons in smoked meat.

In biological matrixes lipid material often poses an interference problem for determinations of nonpolar compounds, e.g., polycyclic aromatic hydrocarbons (PAHs). A newly developed supercritical fluid extraction plus adsorbent method, "SFE-plus-C(18)", offers selective extraction of PAHs in lipid-rich biological matrixes without the need for supplementary cleanup. This method eliminates the use of large volumes of toxic solvent and lengthy lipid removal procedures. This study reports the first application of the SFE-plus-C(18) method to the analysis of a genuine food product, i.e., smoked meat (beef). The procedure employs the addition of C(18) adsorbent beads to the initial sample slurry of pureed smoked meat prior to supercritical CO(2) extraction and GC/MS quantitation. During SF extraction, indigenous lipids are preferentially retained on the beads, and PAHs are selectively extracted with supercritical CO(2). In a comparison of determinations of PAHs by SFE-plus-C(18) vs the conventional SFE method, only 11-17% of the indigenous lipids observed by the conventional SFE method were co-extracted using the SFE-plus-C(18) method. The PAHs in smoked meat could thus be determined efficiently in the presence of a reduced background of co-extracted lipids. Out of 10 targeted PAHs, seven were detected with a range of 10.0-26.0 ng/g in the smoked meat sample. The other three PAHs were not present above the detection limit of the instrument (2.5-4.1 pg). The recoveries of PAHs obtained using the conventional SFE method were 63-94% lower than those achieved by SFE-plus-C(18).

Highly sensitive automatic analysis of polycyclic aromatic hydrocarbons in indoor and outdoor air

A method for the quantitation of polycyclic aromatic hydrocarbons (PAHs) in indoor and outdoor air by high-performance liquid chromatography (HPLC) with a spectrofluorometric detection and programmed excitation and emission wavelength pairs is proposed. The mobile phase is a linear gradient of methanol-water. The relative standard deviations ( n = 5) are in the range 0.38–1.7% at concentration levels of 0.69–11.40 ng ml −1. The determination limits ( S N = 10 ) are 0.5–15.9 pg. The proposed method was successfully applied to quantitate 12 PAHs in gas phase and particulates in indoor and outdoor air. The recoveries of PAHs from gas phase and particulates were 95.7–117.5 and 94.8–112.4%, respectively. This highly sensitive automatic HPLC analysis for PAHs both in gas phase and particulates can be applied to indoor and outdoor survey.

Optimization of automated solid-phase extraction for quantitation of polycyclic aromatic hydrocarbons in aqueous media by high-performance liquid chromatography-UV detection

A solid-phase extraction method for the quantitation of 16 regulated polycyclic aromatic hydrocarbons (PAHs) was developed and conditions were optimized to meet the recoveries stated in US Environmental Protection Agency Method 550.1. The best elution procedure soaked the extraction cartridge with acetonitrile followed by elution with methylene chloride. Rinsing the sample bottle with acetonitrile and combining the rinse with the sample extract was necessary to achieve the desired recoveries. The average recovery for a mixture of the sixteen regulated PAHs was 83%.

Polycyclic aromatic hydrocarbons in waste derived pyrolytic oils

Waste material in the form of wood waste, municipal solid waste and rice husks was pyrolysed in a gas-purged static batch reactor and a fluidised bed reactor. The condensed pyrolytic oils were analysed for their content of polycyclic aromatic hydrocarbons (PAH). The oils were fractionated into chemical classes using mini-column liquid chromatography followed by analysis using GC/FID and GC/MS for identification and quantitation of PAH. The waste derived oils were found to contain substantial concentrations of PAH, which were formed via secondary Diels—Alder and deoxygenation reactions. The concentrations of PAH were influenced by reactor temperature and residence time. The PAH consisted mainly of naphthalene, fluorene and phenanthrene and their alkylated homologues, but also included some PAH which were of known carcinogenic or mutagenic activity.

Selective Fluorescence Detection of Polycyclic Aromatic Hydrocarbons in Environmental Tobacco Smoke and Other Airborne Particles

Abstract An analytical method is described for the simultaneous quantitation of polycyclic aromatic hydrocarbons [PAHs] and alkyl-derivatives [alkyl-PAHs] in “real world” samples using microbore reversed-phase high performance liquid chromatography in conjunction with two programmable fluorescence detectors. Sensitivity and selectivity were enhanced by analyzing PAHs under their optimum fluorescence wavelengths. The accuracy of the analytical method was evaluated by determination of PAHs in 5 mg of standard reference material SRM 1649. The method was also successfully employed to analyze major parent PAHs and some alkyl-PAHs from environmental tobacco smoke [ETS] with a sample size of 2 mg using class-selective fluorescence wavelengths. Some alkyl-PAHs were tentatively identified even in the absence of standard compounds. Coeluting pairs were identified and analyzed by careful selection of excitation and emission wavelengths for each compound. Identities of the signals were confirmed by comparing both the...

A new selective technique for characterization of polycyclic aromatic hydrocarbons in complex samples: UV resonance Raman spectrometry of coal liquids.

Evidence is given showing that UV resonance Raman spectroscopy (UVRRS) is a powerful technique for the identification and quantitation of polycyclic aromatic hydrocarbons (PAH's) in a coal liquid. Results suggest that this technique will be of general utility for the study of systems containing chromaphoric species absorbing in the UV spectral region. In this paper it is demonstrated that (1) the resonance Raman spectra of PAH derivatives can be selectively observed in solutions of coal liquids and (2) different UV excitation wavelengths result in the selective Raman enhancement of different polycyclic aromatic hydrocarbon ring systems.

Quantitation of polycyclic aromatic hydrocarbons in diesel exhaust particulate matter by high-performance liquid chromatography fractionation and high-resolution gas chromatography.

ADVERTISEMENT RETURN TO ISSUEPREVArticleNEXTQuantitation of polycyclic aromatic hydrocarbons in diesel exhaust particulate matter by high-performance liquid chromatography fractionation and high-resolution gas chromatographyH. Y. Tong and F. W. KarasekCite this: Anal. Chem. 1984, 56, 12, 2129–2134Publication Date (Print):October 1, 1984Publication History Published online1 May 2002Published inissue 1 October 1984https://doi.org/10.1021/ac00276a034RIGHTS & PERMISSIONSArticle Views403Altmetric-Citations67LEARN ABOUT THESE METRICSArticle Views are the COUNTER-compliant sum of full text article downloads since November 2008 (both PDF and HTML) across all institutions and individuals. These metrics are regularly updated to reflect usage leading up to the last few days.Citations are the number of other articles citing this article, calculated by Crossref and updated daily. Find more information about Crossref citation counts.The Altmetric Attention Score is a quantitative measure of the attention that a research article has received online. Clicking on the donut icon will load a page at altmetric.com with additional details about the score and the social media presence for the given article. Find more information on the Altmetric Attention Score and how the score is calculated. Share Add toView InAdd Full Text with ReferenceAdd Description ExportRISCitationCitation and abstractCitation and referencesMore Options Share onFacebookTwitterWechatLinked InReddit PDF (771 KB) Get e-Alerts Get e-Alerts

Gas chromatographic method for the analysis of major polynuclear aromatics in particulate matter

A chromatographic method has been developed and applied to the determination of polycyclic aromatic hydrocarbons (PAHs) present in sediments in the Rhondda Fawr Valley. The procedure involves Soxhlet extraction followed by a purification process including both column and thin-layer chromatography. Identification was achieved by fluorescence analysis coupled with gas-liquid or gas-solid chromatography. The quantitation of PAHs was made employing gas chromatography. The method enables the routine analysis of at least nine PAHs present in the environment. Good cross checkes were obtained with gas chromatography-mass spectrometry.