Development of solid-phase extraction method for the determination of aromatic sensitisers in paper mill effluent

In this paper, a procedure for the determination of 11 aromatic hydrocarbon-type sensitisers and their related compounds from water samples, used in the manufacture of thermal paper, is presented. The compounds were extracted using a solid-phase extraction (SPE) cartridge with an octadecyl (C18) or a phenyl-bonded silica (PH) sorbent and then determined by gas chromatography–mass spectrometry (GC–MS). Factors affecting the performance of the extraction steps were thoroughly evaluated, and their effects on the yield of the sample preparation were discussed. Under optimised experimental conditions, SPE cartridges were conditioned with 10?mL hexane followed subsequently by 10?mL methanol, loaded with water sample at 2?mL?min^?1, and eluted with 10?mL hexane at 1.5?mL?min^?1. The limits of detection and quantification, calculated for signal-to-noise ratios of 3 and 10, were in the range of 1–5?µg?L^–1 and 2.5–10?µg?L^–1, respectively. Recovery yields of the present method using river water were in the range of 88%–112% with a C18 sorbent and 86%–116% with a PH sorbent. The repeatability, expressed as a relative standard deviation, was in the range of 2.8%–11% with a C18 sorbent and 0.7%–9.7% with a PH sorbent (n?=?4). Analysis of paper mill effluents revealed the presence of aromatic hydrocarbon-type sensitisers with maximum concentrations of up to 5.2?µg?L^?1.     

A Nanospherical Metal–Organic Framework UiO-66 for Solid-Phase Microextraction of Polycyclic Aromatic Hydrocarbons

Polycyclic aromatic hydrocarbons are a low content, but highly toxic organic pollutant in the environment. Because of their great threat to the health and survival of humans and other creatures, it is necessary to have a very simple and convenient as well as highly sensitive method to detect them. Based on previous studies, a nanospherical metal–organic framework UiO-66 was re-applied as the solid-phase microextraction coating and the extraction performance of polycyclic aromatic hydrocarbons was investigated. Scanning electron microscope and X-ray diffraction were used to characterize the extraction material. The extraction conditions were optimized factor by factor, and the analytical method was established with broad linear ranges (0.03–50 and 0.10–50 µg L^?1), excellent correlation coefficients (0.9955–0.9993) and low limits of detection (0.01–0.03 µg L^?1). The analytical method was applied to detect polycyclic aromatic hydrocarbons in rainwater and lake water, and satisfactory results were obtained. Compared with previous reports, this method had wider linear range, lower limit of detection and longer service life.     

Chemically modified silica gel for selective solid-phase extraction and preconcentration of heavy metal ions

This paper describes our research on the synthesis of the sorbent with chemically bonded ketoimine groups, and, furthermore, using this sorbent in the SPE technique to extract and preconcentrate trace amounts of metal ions in water samples. Surface characteristics of the sorbent were determined by elemental analysis, NMR spectra for the solid phases (²⁹Si CP MAS NMR), and analysis of pore size distribution of the sorbent and nitrogen adsorption-desorption. The newly proposed sorbent with ketoimine groups was applied for the extraction and preconcentration of trace amounts of Cu (II), Cr (III) and Zn (II) ions from the water from a lake, post-industrial water and purified water unburdened back to the lake. The determination of the transition-metal ions was performed on an emission spectroscope with inductively coupled plasma ICP-OES. For the batch method, the optimum pH range for Cu (II) and Cr (III) extraction was equal to 5, and Zn(II)–to 8. All the metal ions can be desorbed from SPE columns with 10?mL of 0.5?mol?HNO₃. The detection limits of the method were found to be 0.7?µg?L^?1 for Cu (II), 0.08?µg?L^?1 for Cr (III), and 0.2?µg?L^?1 for Zn (II), respectively.     

Boron nitride nanotubes as novel sorbent for solid-phase microextraction of polycyclic aromatic hydrocarbons in environmental water samples

Boron nitride nanotube (BNNT) is a novel material that shows potential ability in capturing organic pollutants. In this study, BNNTs fixed on a stainless steel fiber by a sol–gel technique were used as sorbent for solid-phase microextraction. Five polycyclic aromatic hydrocarbons with different numbers of aromatic rings were selected as target analysts. Gas chromatography coupled with tandem mass spectrometry was used for detection and quantitative determination. Under optimized conditions, the experimental results show a wide range of linearity (1 to 1,000 ng L^?1), less than 10.1 % repeatability of relative standard deviation, and low detection limits (0.08 to 0.39 ng L^?1). In addition, the fabricated fiber offered good thermal and chemical stability. The proposed method was successfully applied for the analysis of real water samples, and satisfactory results were obtained with relative recoveries ranging from 80.2 to 116.8 %. The results demonstrated that BNNTs could be used as sorbent for the analysis of environmental pollutants at trace levels.     

Analysis of organic pollutants in water at trace levels using fully automated solid-phase extraction coupled to high-performance liquid chromatography

Summary A method has been developed for the determination of trace levels of 32 pesticides, 19 explosives and 16 polycyclic aromatic hydrocarbons (PAH) in water in three individual steps. Solid-phase enrichment (SPE) is coupled to high-performance liquid chromatography (HPLC) with a fully automated system. The organic pollutants are enriched on reusable cartridges packed with adsorbent materials: pesticides and explosives on a mixed bed of divinylbenzene-ethylvinylbenzene copolymers (LiChrolut EN^?) and perfluorinated polyethylene (PolyF^?), and polycyclic aromatic hydrocarbons on C₁₈-modified silica (Zorbax^? ODS1). Thermally assisted desorption (TAD) has been shown to increase the recovery of analytes significantly. As all enriched analytes are transferred to the detector, only fifty millilitres of sample is needed for each single on-line analysis, compared with at least a litre for conventional methods. The separation of the enriched organic analytes is performed on specialized HPLC columns based on reversed-phase materials. The limits of detection of the system employed were found to be below 100 ng L⁻¹. Use of fluorescence detection for the polycyclic aromatic hydrocarbons resulted in limits of detection in the upper pg L⁻¹ range. Thek values, number of theoretical plates, the recovery rates and the limits of detection of this method for fast screening of organic pollutants from three fifty-millilitre aqueous samples are described. Presented at the 21^st ISC held in Stuttgart, Germany, 15^th–20^th September, 1996     

Magnetic metal–organic framework MIL‐100(Fe) microspheres for the magnetic solid‐phase extraction of trace polycyclic aromatic hydrocarbons from water samples

In this work, a magnetic metal–organic framework designated as MIL‐100(Fe) was prepared and applied as a magnetic solid‐phase extraction sorbent for the determination of trace polycyclic aromatic hydrocarbons in environmental water samples by coupling with high‐performance liquid chromatography and fluorescence detection. The magnetic microspheres exhibited large surface areas and high extraction ability, making them excellent candidates as sorbents for enrichment of trace polycyclic aromatic hydrocarbons. Under the optimized experimental conditions, good sensitivity levels were achieved with low detection limits ranging from 32 to 2110 pg/mL and good linearities with correlation coefficients higher than 0.9990 for the investigated 13 polycyclic aromatic hydrocarbons. The proposed method has been validated in the analysis of real water samples with mean recoveries in the range of 81.4–126.9% at four spiked levels and the relative standard deviations in the range of 1.3–17.0%. The magnetic MIL‐100(Fe) microspheres were stable enough for 150 extractions without a significant loss of extraction performance.     

Development of an analytical method for eight fluoroquinolones using solid-phase extraction and liquid chromatography with fluorescence detection

In this study, a practicable and effective analytical method based on solid-phase-extraction and reversed-phase liquid chromatography with fluorescence detection (SPE-LC-FLD) was developed and partially validated for routine analysis of eight FQs in wastewater at the trace level. Different SPE materials, pH conditions and eluents were modified to find an economic and effective SPE conditions. In our work, it is the first time that well-known commercially available SPE sorbent are compared to ‘generic’ cheap SPE sorbent. Aqueous samples (pH 2–3) were extracted using Anpel? MEP cartridges where they were subsequently eluted by 6?mL of 2% formic acid in MeOH. The aqueous extracts were analysed by gradient elution LC-FLD, whose initial mobile phase was composed of ACN and 10?mmol?L^?1 tetrabutyl ammonium bromide (4/96, v/v, pH 3). The LODs and LOQs of the wastewater were as low as 0.32–2.12?ng?L^?1 and 1.07–7.07?ng?L^?1, respectively. The precisions of the overall method (RSD, n?=?3) using wastewater were below 10%. The method was used to quantify FQs in influents and effluents of several typical sewage treatment plants (STPs) in Shanghai. The extraction recoveries of 100?mL influent, 500?mL effluent and 500?mL of river water samples were between 88.6 and 102.6%, 79.2 and 109.2%, 80.0 and 105.5% and 87.4 and 99.4%, respectively. FQs of interest except sarafloxacin were identified in the influents, effluents and river waters with concentrations varying from 0.012–1.163?µg?L^?1, 0.003–0.291?µg?L^?1, and 0.002–0.040?µg?L^?1, respectively. The method can serve as a tool to obtain detailed information on occurrence, behaviour and fate of FQs in the aquatic environment. Occurrence of FQs detected in summer is higher than in spring at STPs, and those detected in the suburban area are less than those in the urban area. Complete removal of FQs is not achieved from the STPs, indicating domestic wastewater and STP discharge is the source of FQs in the surface water.     

Polyaniline-coated magnetite nanoparticles incorporated in alginate beads for the extraction and enrichment of polycyclic aromatic hydrocarbons in water samples

A magnetic solid-phase extraction sorbent consisting of polyaniline-coated magnetite nanoparticles entrapped in alginate beads (PANI/alginate/Fe₃O₄) was successfully synthesised and applied for the extraction and preconcentration of polycyclic aromatic hydrocarbons (PAHs) in water samples. The magnetite nanoparticles helped to provide an easy and rapid isolation of the sorbent from the sample solution using an external magnet. The alginate beads helped to increase the surface area for polyaniline coating. The polyaniline-coated alginate/magnetite composite helped to increase the extraction efficiency due to the π–π interactions between the polyaniline and the PAHs. Various parameters that affected the extraction efficiencies were optimised including the polymerisation time, the amount of sorbent, sample pH, extraction time, ionic strength, and desorption conditions. Under the optimal conditions, a linear response was achieved in the concentration range of 0.040–50.0 µg L^?1, and the limit of detection was 0.010 µg L^?1. This simple, convenient, cost-effective, and environmentally friendly method was successfully applied for the extraction and enrichment of PAHs in water samples. The recoveries ranged from 86.0% to 97.8% with a relative standard deviation <10 %.     

A highly thermal-resistant electrospun-based polyetherimide nanofibers coating for solid-phase microextraction

A high-temperature-resistant solid-phase microextraction (SPME) fiber was prepared based on polyetherimide (PEI) by the electrospinning method. The PEI polymeric solution was converted to nanofibers using high voltages and directly coated on a stainless steel SPME needle. The scanning electron microscopy images of PEI coating showed fibers with diameter range of 500–650 nm with a homogeneous and smooth surface morphology. The SPME nanofibers coating was optimized for PEI percentage, electrospinning voltage, and time. The extraction efficiency of the coating was investigated for headspace SPME of some environmentally important polycyclic aromatic hydrocarbons from aqueous samples followed by gas chromatography–mass spectrometry measurement. In addition, the important extraction parameters including extraction temperature, extraction time, ionic strength, as well as desorption temperature and time were investigated and optimized. The detection limits of the method under optimized conditions ranged from 1 to 5 ng L^?1 using time-scheduled selected ion monitoring mode. The relative standard deviations of the method were between 1.1 and 7.1 %, at a concentration level of 500 ng L^?1. The calibration curves of polycyclic aromatic hydrocarbons showed linearity in the range of 5–1000 ng L^?1. The developed method was successfully applied to real water samples and the relative recovery percentages obtained from the spiked water samples were from 84 to 98 % for all the selected analytes except for acenaphthene which was from 75 to 106 %.     

Extraction and preconcentration of ultra trace amounts of beryllium from aqueous samples by nanometer mesoporous silica functionalized by 2,4-dihydroxybenzaldehyde prior to ICP OES determination

A new functionalized nanometer mesoporous silica (MCM-41) using 2,4-dihydroxybenzaldehyde (4-OHsal) was applied as an effective sorbent for solid phase extraction (SPE) of beryllium ions from aqueous solution followed by inductively coupled plasma optical emission spectrometric detection (ICP OES). The influences of some analytical parameters on the quantitative recoveries of the analyte ion were investigated in batch method. In order to perform the batch mode of SPE, known amount of sorbent was added to a test tube containing sample solution buffered at pH 7.2. After manual shaking and centrifugation the aqueous phase was decanted and beryllium was desorbed by adding 1.0 mL of 1.0 mol L^?1 HNO₃ to the sedimented sorbent. The sorbent was separated by centrifugation and the concentration of beryllium in the supernatant was determined by ICP OES. The maximum sorption capacity of the modified MCM-41 was found to be 34 mg g^?1. The sorbent exhibited good stability, reusability and fast rate of equilibrium for sorption/desorption of beryllium ions. The present method was used for preconcentration and determination of beryllium for water samples. Under optimal conditions, the limit of detection (LOD) obtained was 0.3 ng L^?1. The accuracy of the procedure was evaluated by analysis of the certified reference material (NIST 1640).     

Development and validation of a SPE-GC-MS method for the determination of pesticides in surface water

A method for analysis of 20 commonly used pesticides in surface water based on solid-phase extraction and gas chromatography-mass spectrometry was proposed. During method development the key parameters that can affect SPE extraction and determination such as selection of efficient SPE sorbent, pH of water sample, type and volume of elution solvent, breakthrough volume and matrix effects were investigated. The method was validated using spring water spiked with appropriate concentration of pesticides. The obtained correlation coefficients were in range 0.9972–1.000, limits of detection (LOD) were 0.001–0.5?µg?L^?1 and the limits of quantification (LOQ) were 0.005–1?µg?L^?1 depending on a pesticide. Much higher LOD (20?µg?L^?1) and LOQ (50?µg?L^?1) values were obtained for bentazone. The influence of matrix was assessed using real water samples spiked with appropriate concentration of pesticide standards solution. Both signal enhancement and suppression were observed, depending on a pesticide, therefore standard addition method was used for pesticides determination. The developed method was applied on real water samples taken in close vicinity of agricultural fields. Many of the targeted pesticides were found in the samples and the results are presented in this article.     

Exploiting a combined computational/experimental sorbent-injection vortex-assisted dispersive microsolid-phase extraction for chromatographic determination of priority phenolic pollutants in water samples

An amine-functionalized metal–organic framework based on aluminum (NH₂-MIL-53(Al)) was synthesized and employed as a sorbent for the extraction of phenolic pollutants. A new designed sorbent-injection vortex-assisted dispersive microsolid-phase extraction was proposed in which the sorbent suspension was simply injected into the sample solution. Herein the experimental parameters that affected the extraction efficiency for the target analytes were optimized, including volume of sorbent suspension, vortex agitation time, eluent type and its volume, and sample volume. Good linearity was obtained in the concentration range of 0.1–10.0 mg L^?1 with the correlation coefficients in the range of 0.9970–0.9981. The LODs and LOQs were in the ranges of 0.030–0.055 and 0.090–0.150 mg L^?1, respectively. The results of the intra- and inter-day experiments showed good precision of peak area with the relative standard deviation (RSD) values of better than 5.82 and 7.85%, respectively. The developed method has been successfully applied to determine phenolic residues in water samples. The satisfactory recoveries were obtained in the range of 83.0–122.4% with the RSDs of less than 12.9%. In addition, molecular docking was performed to predict the adsorption ability of NH₂-MIL-53(Al) sorbent toward the target analytes. The computational results were in good agreement with data obtained experimentally.     

Magnetic solid phase extraction of N- and S-containing polycyclic aromatic hydrocarbons at ppb levels by using a zerovalent iron nanoscale material modified with a metal organic framework of type Fe@MOF-5, and their determination by HPLC

Metal organic frameworks of type MOF-5 exhibit good adsorption capacity for many organic compounds. The authors have used nanoscale silica-coated zerovalent iron and MOF-5 to prepare, by co-precipitation, a novel magnetic nanomaterial of type Fe@MOF-5. Its morphology and structure were characterized by transmission electron microscopy and X-ray diffraction. The nanomaterial is shown to be well suited for magnetic solid phase extraction for five kinds of N- and S-containing polycyclic aromatic hydrocarbons prior to quantitation by HPLC. The limits of detection are in the 25 to 33 ng?L^?1 concentration range. Four real water samples were used to validate the method, and the recoveries of spiked samples with concentrations of 5 and 10 ppb were found to be in the range between 92.6 and 97.3% (n = 3). The Fe@MOF-5 sorbent obviously has excellent adsorption capability for such compounds, can be fairly easily synthesized, displays sensitivity, simplicity, ease of operation, and can be prepared at low costs. In our perception, it has a large potential in terms of monitoring such environmental pollutants.

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Graphical abstract A metal organic framework of type Fe@MOF-5 is found to exhibit good adsorption capacity for N- and S-containing polycyclic aromatic hydrocarbons. A sensitive magnetic solid phase extraction method with Fe@MOF-5 was developed for the determination of N- and S-containing polycyclic aromatic hydrocarbons from the water samples.

     

Hollow-Fibre Liquid-Phase Microextraction for the Determination of Polycyclic Aromatic Hydrocarbons in Johannesburg Jukskei River, South Africa

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.     

Preconcentration of beryllium via octadecyl silica gel microparticles doped with aluminon, and its determination by flame atomic absorption spectrometry

A simple and sensitive method is presented for solid phase extraction (SPE) and preconcentration of trace quantities of beryllium using octadecyl silica gel modifed with aurin tricarboxylic acid (aluminon). Beryllium is then determined by flame atomic absorption spectroscopy. Parameters affecting SPE such as pH, sample solution and eluent flow rate, type, concentration and volume of eluent, interfering ions and breakthrough volume, were investigated. Under optimal conditions, the beryllium ions were retained on the sorbent at pH 6–6.7, while 3.0 mL of 0.05 mol L^?1 HNO₃ is sufficient to elute the ions. The limit of detection (LOD) based on 3σ was 0.8 µg L^?1 for 250 mL sample solution and 5 mL 0.05 mol L^?1 HNO₃ as eluent. The LOD can reach 0.1 µg L^?1 for 1 L sample solution and 3 mL of 0.05 mol L^?1 HNO₃. The accuracy and precision (RSD %) of the method is >90% and <10%, respectively. The method was applied to the determination of beryllium in aqueous samples.     

Determination of monohydroxylated metabolites of polycyclic aromatic hydrocarbons (OH-PAHs) from wastewater-treatment plants

A high-performance liquid chromatography separation coupled with mass spectrometry via an electrospray interface is proposed for the determination of the hydroxylated derivatives of polycyclic aromatic hydrocarbons (OH-PAHs) in treated and untreated wastewaters and suspended solids from sewage treatment plants (STPs). The developed SPE procedure was applied to spiked wastewater samples, with recovery yields (1000?mL; 100?ng?L^?1 spiking level) in the 65–87% (RSD: 6–12%) range for the selected OH-PAHs. The limits of detections ranged between 0.3 and 3.2?ng?L^?1, depending on the selected compound and on the investigated matrix. The proposed method was applied to the determination of the selected analytes in real samples from a sewage-treatment plant (STP). The investigated OH-PAHs were detected mainly in the particulate fraction. The exhibited mean concentrations of positive samples (as the sum of dissolved and particulate matter) in the STP final effluent ranged from 15 to 68?ng?L^?1.     

Hydroxyundecanethiol-Modified Steel Fibers for the Selective Solid-Phase Microextraction of Polycyclic Aromatic Hydrocarbons from River and Wastewater

A novel organic–inorganic composite-coated fiber was developed for selective solid-phase microextraction (SPME) by direct electrodeposition of zinc oxide microparticles on a pretreated stainless steel wire followed by self-assembly of hydroxyundecanethiol with zinc–sulfur bonds. The performance of the hydroxyundecyl-modified zinc oxide-coated steel fiber was then assessed for SPME of polar aromatic compounds coupled to high-performance liquid chromatography with ultraviolet detection. Excellent extraction and selectivity were obtained for polycyclic aromatic hydrocarbons. The extraction and desorption times, temperature, stirring rate, and ionic strength were optimized. The limits of detection were from 0.034 to 0.132?µg?L^?1. The relative standard deviations were from 3.4 to 4.9% for a single fiber and from 5.1 to 6.4% for multiple fibers. The recovery of polycyclic aromatic hydrocarbons in environmental water fortified at 5.0 and 50?µg?L^?1 was from 83.1 to 103% with relative standard deviations below 8.4%. This fiber was shown to withstand at least 200 extraction and desorption cycles. The method was used for the preconcentration and determination of polycyclic aromatic hydrocarbons in environmental water.     

Sensitive Stripping Determination of Cadmium(II) and Lead(II) on Disposable Graphene Modified Screen‐Printed Electrode

In the present work, a sensitive, facile and disposable sensing platform for trace analysis of heavy metal ions was developed at the Bi modified graphene‐poly(sodium 4‐styrenesulfonate) composite film screen printed electrode (GR/PSS/Bi/SPE). The GR/PSS/Bi/SPE improved sensitivity and linearity due to the functionalization of graphene with negatively charged PSS providing more absorbing sites. The detection limit of the GR/PSS/Bi/SPE is found to be 0.042 µg L^?1 for Cd²⁺ and 0.089 µg L^?1 for Pb²⁺ with linear responses of Cd²⁺ and Pb²⁺ in the range of 0.5–120 µg L^?1. Finally, the practical application was confirmed in real water with satisfactory results.     

Selective Sensing of Fe3+ and Al3+ Ions and Detection of 2,4,6‐Trinitrophenol by a Water‐Stable Terbium‐Based Metal–Organic Framework

A water‐stable luminescent terbium‐based metal–organic framework (MOF), {[Tb(L₁)_1.5(H₂O)] ? 3 H₂O}_n (Tb‐MOF), with rod‐shaped secondary building units (SBUs) and honeycomb‐type tubular channels has been synthesized and structurally characterized by single‐crystal X‐ray diffraction. The high green emission intensity and the microporous nature of the Tb‐MOF indicate that it can potentially be used as a luminescent sensor. In this work, we show that Tb‐MOF can selectively sense Fe³⁺ and Al³⁺ ions from mixed metal ions in water through different detection mechanisms. In addition, it also exhibits high sensitivity for 2,4,6‐trinitrophenol (TNP) in the presence of other nitro aromatic compounds in aqueous solution by luminescence quenching experiments.     

Analysis of PAHs in Water and Fruit Juice Samples by DLLME Combined with LC-Fluorescence Detection

A simple, rapid and efficient method termed dispersive liquid–liquid microextraction combined with liquid chromatography-fluorescence detection, has been developed for the extraction and determination of polycyclic aromatic hydrocarbons (PAHs) in water and fruit juice samples. Parameters such as the kind and volume of extraction solvent and dispersive solvent, extraction time and salt effect were optimized. Under optimum conditions, the enrichment factors ranged from 296 to 462. The linear range was 0.01–100 μg L^?1 and limits of detection were 0.001–0.01 μg L^?1. The relative standard deviations (RSDs, for 5 μg L^?1 of PAHs) varied from 1.0 to 11.5% (n = 3). The relative recoveries of PAHs from tap, river, well and sea water samples at spiking level of 5 μg L^?1 were 82.6–117.1, 74.9–113.9, 77.0–122.4 and 86.1–119.3%, respectively. The relative recoveries of PAHs from grape and apple juice samples at spiking levels of 2.5 and 5 μg L^?1 were 80.8–114.7 and 88.9–123.0%, respectively. It is concluded that the proposed method can be successfully applied for determination of PAHs in water and fruit juice samples.