Critical Assessment of Clean-Up Techniques Employed in Simultaneous Analysis of Persistent Organic Pollutants and Polycyclic Aromatic Hydrocarbons in Fatty Samples

Interference of residual lipids is a very common problem in ultratrace analysis of contaminants in fatty matrices. Therefore, quick and effective clean-up techniques applicable to multiple groups of analytes are much needed. Cartridge and dispersive solid-phase extraction (SPE and dSPE) are often used for this purpose. In this context, we evaluated the lipid clean-up efficiency and performance of four commonly used sorbents—silica, C18, Z-Sep, and EMR-lipid—for the determination of organic pollutants in fatty fish samples (10%) extracted using ethyl acetate or the QuEChERS method. Namely, 17 polychlorinated biphenyls (PCBs), 22 organochlorine pesticides (OCPs), 13 brominated flame retardants (BFRs), 19 per- and polyfluoroalkyl substances (PFAS), and 16 polycyclic aromatic hydrocarbons (PAHs) were determined in this study. The clean-up efficiency was evaluated by direct analysis in real time coupled with time-of-flight mass spectrometry (DART-HRMS). The triacylglycerols (TAGs) content in the purified extracts were significantly reduced. The EMR-lipid sorbent was the most efficient of the dSPE sorbents used for the determination of POPs and PAHs in this study. The recoveries of the POPs and PAHs obtained by the validated QuEChERS method followed by the dSPE EMR-lipid sorbent ranged between 59 and 120%, with repeatabilities ranging between 2 and 23% and LOQs ranging between 0.02 and 1.50 µg·kg−1.

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QuEChERS Method Followed by Solid Phase Extraction Method for Gas Chromatographic-Mass Spectrometric Determination of Polycyclic Aromatic Hydrocarbons in Fish

International Journal of Analytical Chemistry ◽

10.1155/2015/352610 ◽

2015 ◽

Vol 2015 ◽

pp. 1-7 ◽

Cited By ~ 6

Author(s):

Mona Khorshid ◽

Eglal R. Souaya ◽

Ahmed H. Hamzawy ◽

Moustapha N. Mohammed

Keyword(s):

Polycyclic Aromatic Hydrocarbons ◽

Solid Phase Extraction ◽

Aromatic Hydrocarbons ◽

Solid Phase ◽

Phase Extraction ◽

Quechers Method ◽

Relative Standard ◽

Fish Samples ◽

Polycyclic Aromatic

A gas chromatography equipped with mass spectrometer (GCMS) method was developed and validated for determination of 16 polycyclic aromatic hydrocarbons (PAHs) in fish using modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method for extraction and solid phase extraction for sample cleanup to remove most of the coextract combined with GCMS for determination of low concentration of selected group of PAHs in homogenized fish samples. PAHs were separated on a GCMS with HP-5ms Ultra Inert GC Column (30 m, 0.25 mm, and 0.25 µm). Mean recovery ranged from 56 to 115%. The extraction efficiency was consistent over the entire range where indeno(1,2,3-cd)pyrene and benzo(g,h,i)perylene showed recovery (65, 69%), respectively, at 2 µg/kg. No significant dispersion of results was observed for the other remaining PAHs and recovery did not differ substantially, and at the lowest and the highest concentrations mean recovery and RSD% showed that most of PAHs were between 70% and 120% with RSD less than 10%. The measurement uncertainty is expressed as expanded uncertainty and in terms of relative standard deviation (at 95% confidence level) is±12%. This method is suitable for laboratories engaged daily in routine analysis of a large number of samples.

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A traceless clean-up method coupled with gas chromatography and mass spectrometry for analyzing polycyclic aromatic hydrocarbons in complex plant leaf matrices

The Analyst ◽

10.1039/d0an00128g ◽

2020 ◽

Vol 145 (9) ◽

pp. 3266-3273

Author(s):

Xiangzi Jin ◽

Han Yeong Kaw ◽

Huijie Li ◽

Zhao Wang ◽

Jinhua Zhao ◽

...

Keyword(s):

Mass Spectrometry ◽

Gas Chromatography ◽

Polycyclic Aromatic Hydrocarbons ◽

Aromatic Hydrocarbons ◽

Solid Phase ◽

Phase Extraction ◽

Plant Leaves ◽

Gas Purge ◽

Polycyclic Aromatic

This study developed a traceless clean-up method by combining solid phase extraction (SPE) with gas purge–microsyringe extraction (GP–MSE) to purify sample extracts for the determination of polycyclic aromatic hydrocarbons (PAHs) in plant leaves.

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Identification and quantification of organic pollutants in the air of the city of Astana using solid phase microextraction

Chemical Bulletin of Kazakh National University ◽

10.15328/cb826 ◽

2017 ◽

pp. 14-17

Author(s):

Dina Orazbayeva ◽

Ulzhalgas Karatayeva ◽

Kulzhan Beysembayeva ◽

Kulyash Meyramkulova

Keyword(s):

Polycyclic Aromatic Hydrocarbons ◽

Aromatic Hydrocarbons ◽

Solid Phase Microextraction ◽

Solid Phase ◽

Ambient Air ◽

Average Concentration ◽

Polycyclic Aromatic ◽

Benzene Toluene ◽

The City

Solid-phase microextraction in combination with gas chromatography and mass-spectrometry (GC-MS) was used for determination of benzene, toluene, ethylbenzene and o-xylene (BTEX), polycyclic aromatic hydrocarbons (PAH), and for identification of volatile organic compounds (VOCs) in ambient air of the city of Astana, Kazakhstan. The screening of the samples showed the presence of mono- and polycyclic aromatic hydrocarbons, alkanes, alkenes, phenols, and benzaldehydes. The concentrations of naphthalene were 5-7 times higher than the permissible value, it was detected in all studied air samples. Average concentration of naphthalene was 18.4 μg/m3, acenaphthylene – 0.54 μg/m3, acenaphthene – 1.63 μg/m3, fluorene – 0.79 μg/m3, anthracene – 3.27 μg/m3, phenanthrene – 0.22 μg/m3, fluorantene – 0.74 μg/m3, pyrene – 0.73 μg/m3. Average concentrations of BTEX in the studied samples were 31.1, 84.9, 10.8 and 11.6 μg/m3, respectively. Based on the statistical analysis of the concentrations of BTEX and PAH, the main source of city air pollution with them was assumed to be vehicle emissions.

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