scholarly journals Determination of Polycyclic Aromatic Hydrocarbons in Agricultural Products

2021 ◽  
Vol 16 (3) ◽  
pp. 127-136
Author(s):  
К.К. Tsymbaliuk ◽  
O.V. Snurnikova ◽  
K.V. Melnyk ◽  
E.M. Fadeev ◽  
V.P. Antonovich
Keyword(s):  
Polycyclic Aromatic Hydrocarbons ◽  
Aromatic Hydrocarbons ◽  
Matrix Effects ◽  
Soxhlet Extraction ◽  
Agricultural Products ◽  
Gas Chromatography Mass Spectrometry ◽  
Polycyclic Aromatic ◽  
Optimized Conditions ◽  
Gas Chromatographic Separation

The procedure for the determination of polycyclic aromatic hydrocarbons (PAH) in agricultural products on the example of five crops (rapeseed, sunflower, flax, corn, soybeans) by gas chromatography mass spectrometry (GC-MS) was developed. It was showed the advantage of using binary mixtures of organic solvents "hexanedichloromethane" for PAH extraction. The time of Soxhlet extraction is from 6 to 8 hours at optimized conditions. The fractionation and purification of extracts by column chromatography on deactivated alumina was optimized. The article presents the optimization of sample injection in the programmed temperature vaporization (PTV) mode, parameters of gas chromatographic separation and mass spectrometric detection in determining 16 priority PAH in agricultural products. The recoveries, correctness and accuracy of the proposed method were checked by “spikes” with concentrations 0.5, 1.0, 2.5, 5.0 μg kg-1. The linearity of the method was determined by calibration curves obtained for three measurements of calibration solutions with concentrations of 0.5-100 ng mL-1. The effectiveness of the proposed combination of sample preparation and analysis by PTV-GC-MS was studied for linearity, accuracy, matrix effects and reproducibility. The method was validated by linearity, accuracy, matrix effect and reproducibility.

scholarly journals Determination of the Levels of Polycyclic Aromatic Hydrocarbons in Toasted Bread Using Gas Chromatography Mass Spectrometry

2010 ◽  
Vol 2010 ◽  
pp. 1-8 ◽  
Author(s):  
Amal Al-Rashdan ◽  
Murad I. H. Helaleh ◽  
A. Nisar ◽  
A. Ibtisam ◽  
Zainab Al-Ballam
Keyword(s):  
Polycyclic Aromatic Hydrocarbons ◽  
Wheat Flour ◽  
Aromatic Hydrocarbons ◽  
Soxhlet Extraction ◽  
Gas Chromatography Mass Spectrometry ◽  
White Wheat ◽  
Relative Standard ◽  
Polycyclic Aromatic ◽  
Repeatability And Reproducibility

Concentration of 16 polycyclic aromatic hydrocarbons (PAHs) in eighteen baked bread samples using gas oven toasting were evaluated in this study. Samples were classified into the following categories: (1) bread baked from white wheat flour, (2) bread baked from brown wheat flour, and (3) sandwich bread baked from white wheat flour. Analysis was performed by GC-MS after Soxhlet extraction of the sample and clean up of the extract. The levels of B[a]P was not detected in ten of eighteen samples. In the rest of the samples, B[a]P are varied from 2.83 to 16.54 g/kg. B[a]A, CHR, B[b]FA, B[k] FA, IP, DB[a,h]A, and B[ghi]P concentrations were found to be less than 10.0 g/kg. However, B[a]P are not detected in original white and brown wheat flour. The total PAHs were varied in the range 1.06–44.24 g/kg and 3.08–278.66 g/kg for H-PAH and L-PAH, respectively. Reproducibility and repeatability of the proposed method was calculated and presented in terms of recovery and relative standard deviations (RSD, %). Recoveries were varied from 72.46% to 99.06% with RSD ± 0.28–15.01% and from 82.39% to 95.01% with RSD ±1.91–13.01% for repeatability and reproducibility, respectively. Different commercialized samples of toasted bread were collected and analyzed.

Investigation of a QuEChERS Based Method for Determination of Polycyclic Aromatic Hydrocarbons in Rat Plasma by GC/MS

2021 ◽  
Author(s):  
Noha F El Azab ◽  
Said F Hotar ◽  
Yossra A Trabik
Keyword(s):  
Polycyclic Aromatic Hydrocarbons ◽  
Aromatic Hydrocarbons ◽  
Matrix Effects ◽  
Rat Plasma ◽  
Gas Chromatography Mass Spectrometry ◽  
Plasma Samples ◽  
Material Optimization ◽  
Limit Of Quantitation ◽  
Polycyclic Aromatic

Abstract Owing to their toxic effects on humans and the environment, sensitive biomonitoring of polycyclic aromatic hydrocarbons (PAHs) is essential and significant. In this work, a sensitive, simple and rapid bioanalytical method was established for the simultaneous determination of thirteen (PAHs) in rat plasma depending on QuEChERS as a preliminary step and gas chromatography/mass spectrometry (GC/MS) for identification. QuEChERS procedure was optimized where acetonitrile was employed for plasma samples extraction which was further cleaned using primary secondary amine as the sorbent material. Optimization of GC/MS conditions was performed to produce optimum selectivity of the proposed method. The method was fully validated for rat plasma samples where recoveries, matrix effects, limit of quantitation, linearity, and precision were evaluated. Linearity range was 5.0–100.0 ng/mL for most of the thirteen analytes. Average recoveries of the thirteen PAHs ranged between 85.57 % to 109.64 % in fortified rat plasma with standard deviations (SDs) less than 8.91 except for anthracene which showed 19.24. The limits of detection (LODs) and quantitation (LOQs) for the thirteen compounds ranged from 0.045 to 0.372 ppb and from 0.137 to 1.128 ppb respectively. The established method was successfully implemented to perform a minor toxicokinetic study in intraperitoneally dosed rats (0.25 and 2 mg/kg in vegetable oil). The thirteen PAHs were tracked in rat plasma samples for 6 h after administration, and most of the target compounds were recognized in plasma samples only at the higher dose.

scholarly journals UNSUITABILITY OF THE ZEK/AFPS TEST METHOD FOR THE DETERMINATION OF POLYCYCLIC AROMATIC HYDROCARBONS IN CARBON BLACK

2018 ◽  
Vol 91 (1) ◽  
pp. 225-250
Author(s):  
Stephan Hamm ◽  
Kai Hölscher ◽  
Thomas M. Gruenberger ◽  
Gilles Moninot ◽  
Wolfgang Örtel ◽  
...  
Keyword(s):  
Polycyclic Aromatic Hydrocarbons ◽  
Carbon Black ◽  
Aromatic Hydrocarbons ◽  
Soxhlet Extraction ◽  
Test Method ◽  
Gas Chromatography Mass Spectrometry ◽  
Specific Method ◽  
Relative Distribution ◽  
Polycyclic Aromatic

ABSTRACT The Zentraler Erfahrungsaustauschkreis/Ausschuss für Produktsicherheit (ZEK/AfPS) analytical method established within the Geprüfte Sicherheit (GS) quality label for the determination of 18 polycyclic aromatic hydrocarbons (PAHs) in consumer articles made out of rubber or plastic was demonstrated as unsuitable for carbon black (CB). High molecular weight PAHs are not efficiently extracted from CB through the ZEK/AfPS method when compared with the CB-specific method consisting of 48 h Soxhlet extraction. The low extraction efficiency correlates with the low recovery or loss of the deuterated isotopologues added prior to the 1 h ZEK/AfPS ultrasound extraction of the native PAHs. These phenomena are dependent on the type and concentration level of the various PAHs and are attributed to the relative distribution and adsorption of the native and deuterated PAHs between the CB surface and the toluene phase. These findings are based on comparative extractions of various carbon black grades, use of a larger set of deuterated isotopologues for gas chromatography/mass spectrometry (GC/MS) quantification of native PAHs, and monitoring of the recoveries of the deuterated PAHs added prior to or after the ZEK/AfPS extractions.

scholarly journals Optimization of a Low Volume Extraction Method to Determine Polycyclic Aromatic Hydrocarbons in Aerosol Samples

2021 ◽  
Vol 9 ◽  
Author(s):  
Caroline Scaramboni ◽  
Jordan Brizi Neris ◽  
Rita de Kássia Silva do Nascimento ◽  
Natasha Leandra Chiaranda da Rosa ◽  
Jonatas Schadeck Carvalho ◽  
...  
Keyword(s):  
Polycyclic Aromatic Hydrocarbons ◽  
Aromatic Hydrocarbons ◽  
Extraction Method ◽  
Reference Method ◽  
Atmospheric Particulate Matter ◽  
Component Mixture ◽  
Polycyclic Aromatic ◽  
Low Volume ◽  
Optimized Conditions

This work describes the optimization of an extraction method for the determination of polycyclic aromatic hydrocarbons (PAHs) and their nitro- and oxy-PAH derivatives in atmospheric particulate matter (PM) samples, and demonstrates that this method is also effective for the determination of levoglucosan. The optimization of the extraction solvents was performed using a three-component mixture design with the solvents dichloromethane, methanol, and acetonitrile. The number of extractions, volume of solvent, and duration of extraction in an ultrasonic bath were optimized using a full factorial design followed by a central composite design. The analyses were performed by gas chromatography coupled with mass spectrometry. The optimized conditions of the method were three extractions using 4.0 ml of acetonitrile, with ultrasonication for 34 min. The proposed method presented good linearity (r > 0.990) and acceptable precision for low (100 ng ml−1, RSD: 1–16%), medium (300 ng ml−1, RSD: 1–19%), and high (500 ng ml−1, RSD: 2–16%) concentrations of PAHs. The limits of quantification for different PAHs ranged from 10 to 50 ng ml−1, which were suitable for atmospheric PM. Assessment of the method using sample matrix spiking/recovery assays, as well as use of a reference method, showed good recoveries for levoglucosan and for most of the PAHs and their derivatives, except for the most volatile compounds, which were lost during the evaporation of the solvent. The results for PM samples extracted by the optimized method and the reference method were in good agreement. The proposed method required 97% less solvent than the reference method, shortened the analysis time by 85%, and proved to be accurate and precise for the determination of at least 27 PAHs and their derivatives present in PM samples collected with a low-volume sampler.

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