A screening method for polycyclic aromatic hydrocarbons determination in water by headspace SPME with GC-FID (original) (raw)
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Journal of Separation Science, 2012
This article introduces a simple, rapid, and reliable solid-phase microextraction (SPME) method coupled with GC-MS for the quantitative determination of 16 polycyclic aromatic hydrocarbons in water. In this study, the Taguchi experimental design was used to optimize extraction conditions of polycyclic aromatic hydrocarbons using SPME method to obtain highly enriched analytes. Consequently, quantitative determination of polycyclic aromatic hydrocarbons in water was achieved by GC-MS technique. The selected parameters affecting enrichment of polycyclic aromatic hydrocarbons were sample extraction time, stirring speed, temperature, ionic strength, and pH. The study revealed that optimal operating conditions were found to be 90-min extraction time, 1400 rpm stirring speed, and 60ЊC sample temperature. The effect of ionic strength and pH were shown to be insignificant. Optimized conditions were also reevaluated by placing the 16 polycyclic aromatic hydrocarbons into several subgroups based on their molecular weight. The extraction efficiency of polycyclic aromatic hydrocarbons with low molecular weight was shown to be a function of only the extracting temperature. Satisfactory results were obtained for linearity (0.983-0.999), detection limits (2.67-18.02 ng/L), accuracy (71.2-99.3%), and precision (4.3-13.5%). The optimum conditions reported by other design approaches were evaluated and generalized optimum conditions were suggested.
Journal of Chromatography A, 2011
A methacrylate-based monolithic capillary column has been evaluated for the preconcentration of polycyclic aromatic hydrocarbons (PAHs) from environmental water samples. For this purpose, the monolyte was in situ synthesized in a 6 cm × 0.32 mm id fused-silica capillary. The microextraction unit was fitted to a micro-HPLC pump to pass 10 mL of sample. The isolated pollutants were eluted by means of 10 L of methanol, the organic phase being directly collected in a specific interface that can be fitted to the injection port of the gas chromatograph without modification. The interface allows the on-line thermal desorption of the PAHs, avoiding the dilution and providing enough sensitivity to reach the legal limits established for these pollutants in the matrices selected. The limits of detection achieved for 10 mL of water ranged between 2.8 ng/L (indeno(1,2,3-cd)pyrene) and 11.5 ng/L (acenaphthene) with acceptable precision (between 4.5 and 18.2% RSD). The method was applied to the determination of the selected PAHs in tap, river waters and sewage, being fluoranthene and pyrene detected in all of them at concentrations lower than the legal limits established for these compounds in the matrices assayed.
Iranian Journal of Pharmaceutical Research : IJPR, 2016
Polycyclic aromatic hydrocarbons (PAHs) are classified as persistent and carcinogenic organic pollutants. PAHs contamination has been reported in water. Many of relevant regulatory bodies such as EU and EPA have regulated the limit levels for PAHs in drinking water. In this study, 13 priority polycyclic aromatic hydrocarbons (PAHs) were determined in tap water samples of Tehran and water for injection. Dispersive liquid-liquid microextraction procedure combined with gas chromatography-mass spectrometry was used for the extraction and determination of PAHs in the samples. Under the optimized conditions, the range of extraction recoveries and relative standard deviations (RSDs) of PAHs in water using internal standard (anthracene-d10) were in the range of 71-90% and 4-16%, respectively. Limit of detection for different PAHs were between 0.03 and 0.1 ngmL-1. The concentration of PAHs in all tap water as well as water for injection samples were lower than the limit of quantification of ...
Eurasian chemical communications, 2021
In this research the possibility of application of an innovative, simple, economical, selective ability and green (environmentally friendly) method of salting out and Vortex-Assisted dispersive liquid-liquid microextraction based on solidification of floating organic drop by using high performance liquid chromatography with containing UV for pre-concentration, the extraction and determination of polysiclic in water and solid samples followed by HPLC was studied. In this method three integrated and combined approaches have been adopted so as to maximize the advantages of the approach used while minimizing their disadvantages. The effects of experimental variables such as pH, the type and volume of dispersive extracting solvents (μl, pH), the volume of organic drop microextraction (extracting solvent), salt density (concentration), centrifuge condition (time), extraction time and temperature were examined, and the process of optimization was obtained by using a software based on Response Surface Methodology (RSM) and Box-Behnken design [as the experimental model] and Desirability Function (DF). This method has appropriate linear calibration between 0.2 to 800μg/L, and a significant limit of detection coefficient (r 2 > 9991) and low detection range (between 0.05 to 0.09 μg/L). The above method was also applied for the successful determination of polycyclic aromatic hydrocarbons in industrial was water, water and soil samples PAHs) and the percentage of recycling, repeatability and reproducibility, resulting in satisfactory results. Simplicity, being economical, quickness, proper repeatability, less consumption of organic solvent and efficient decomposition are of the principal advantages (merits) of the proposed method for the decomposition and determination of polycyclic aromatic hydrocarbons (PAHs) in water samples.
Chromatographia, 2013
A simple, rapid and environmentally friendly hollow-fibre liquid-phase microextraction (HF-LPME) technique was developed for the quantitative determination of polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. GC-MS was then used as the method of analysis. The HF-LPME technique involves extraction of PAHs from a 20-mL sample containing 20 % acetonitrile as a modifier. The PAHs were extracted into a 5-cm hollow fibre filled with heptane as organic solvent. At a stirring speed and extraction time of 600 rpm and 30 min, respectively, the acceptor solvent was then collected to be analysed. Parameters that affect the extraction efficiency were optimised in order to achieve high enrichment of the analytes. In order to evaluate the practical applicability of the HF-LPME technique, the performance of the method was compared to solid-phase extraction using spiked deionised water and real water samples. The obtained concentration enrichment factors ranged from 48 to 95 for HF-LPME and 81-135 for SPE, depending on the individual PAH. The detection limit ranged from 23 to 95 ng L-1 for HF-LPME and 20-52 ng L-1 for SPE. Water samples from the Johannesburg area, South Africa, were analysed using both extraction methods and the results were in good agreement. The relative standard deviations were less than 12 % for both methods. In this comparison, SPE was found to give high concentration enrichment factors and recovery, whereas faster and cheaper analyses were achieved with HF-LPME. The concentration of PAHs found could be arranged in the following order: phenanthrene [ acenaphthene [ fluoranthene [ naphthalene [ pyrene.
Journal of Chromatography A, 2000
A solid-phase microextraction (SPME) procedure has been developed for the determination of 16 US Environmental Protection Agency promulgated polycyclic aromatic hydrocarbons (PAHs). Five kinds of SPME fibers were used and compared in this study. The extracted sample was analyzed by gas chromatography with flame ionization detection or mass spectrometry. Parameters affecting the sorption of analyte into the fibers, including sampling time, thickness of the fiber coating, and the effect of temperature, have been examined. Moreover, the feasibility of headspace SPME with different working temperatures was evaluated. The method was also applied to real samples. The 85-mm polyacrylate (PA) and 100-mm poly(dimethylsiloxane) (PDMS) fibers were shown to have the highest affinities for the selected PAHs. The PA fiber was more suitable than the PDMS fiber for the determination of low-ring PAHs while high sensitivity of high-ring PAHs was observed when a 100-mm PDMS fiber was used. The method showed good linearity between 0.1 and 100 ng / ml with regression coefficients ranging from 0.94 to 0.999. The reproducibility of the measurements between fibers was found to be very good. The precisions of PA and PDMS fibers were from 3 to 24% and from 3 to 14%, respectively. Headspace SPME is a valid alternative for the determination of two-to five-ring PAHs. A working temperature of 608C provides significant 26 enhancement in sensitivity of two-to five-ring PAHs having low vapor pressures (.10 mmHg at 258C) (1 mmHg5133.3 5 Pa) and low Henry's constants (.10 atm ml / mol) (1 atm51.01?10 Pa).
The determination of polycyclic aromatic hydrocarbons (PAHs) using high-performance liquid chromatography (HPLC) with UV and fluorescence detection has been well established. Although most of the PAHs can be detected by these methods, some environmentally important polyaromatic compounds, such as acenaphthylene, do not show fluorescence and can only be determined by UV detection at higher concentrations. A sensitive and selective determination of acenaphthylene, acenaphthene and the six PAHs listed in the TVO, the German drinking water standard, is also possible by amperometric detection following HPLC separation. The method was applied to the determination of PAHs in different water samples after solid-phase extraction (SPE). The efficiency of the amperometric determination was found to be superior to UV detection (A=300 nm).
Analytica Chimica Acta, 2013
In the present study, facile and competent homogeneous liquid-liquid microextraction via flotation assistance (HLLME-FA) method combined with flow injection flame atomic absorption spectrometry (FI-FAAS) was proposed for simultaneous separation/ preconcentration and determination of trace amounts of cadmium and copper in water samples. The efficient 2-(3,4-dihydroxyphenyl)-1,3-dithiolane (DHPDTO) with thiol groups was used as chelating reagent. The predominant parameters influencing the HLLME-FA, such as solution pH, concentration of DHPDTO, extraction and homogeneous solvent types and volumes, ionic strength, and extraction time were studied. Applying all the optimum conditions in the process, the detection limits of 0.008 and 0.01 μg L −1 , linear ranges of 0.08-40 and 0.1-45 μg L −1 , and the precision (RSD%, n=7) of 3.4 and 3.9 % were obtained, respectively, for cadmium and copper. The proposed procedure showed satisfactory results for analysis of tap water, river water, well water, and seawater.
Iranian Journal of Pharmaceutical Research : IJPR, 2016
Dispersive liquid-liquid microextraction (DLLME) combined with gas chromatography–mass spectrometry (GC–MS) was used for the extraction and determination of 13 polycyclic aromatic hydrocarbons (PAHs) in mineral water samples. In this procedure, the suitable combination of extraction solvent (500 µL chloroform) and disperser solvent (1000 µL acetone) were quickly injected into the water sample (10.00 mL) by Hamilton syringe. After centrifugation, 500 µL of the lower organic phase was dried under a gentle stream of nitrogen, re-dissolved in chloroform and injected into GC-MS. Chloroform and acetone were found to be the best extraction and disperser solvent, respectively. Validation of the method was performed using spiked calibration curves. The enrichment factor ranged from 93 to 129 and the recovery ranged from 71 to 90%. The linear ranges for all the PAHs were 0.10-2.80 ngmL-1. The relative standard deviations (RSDs) of PAHs in water by using anthracene-d10 as internal standard, we...