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

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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Determination of PAHs in River Water Using Bamboo Charcoal as a Solid-Phase Extraction Adsorbent by Synchronous Fluorescence Spectrometry

Advanced Materials Research ◽

10.4028/www.scientific.net/amr.518-523.1501 ◽

2012 ◽

Vol 518-523 ◽

pp. 1501-1505

Author(s):

Li Fang He ◽

Xia Hong Zhang ◽

Ru Ping Zhang

Keyword(s):

Polycyclic Aromatic Hydrocarbons ◽

Solid Phase Extraction ◽

Aromatic Hydrocarbons ◽

Solid Phase ◽

Synchronous Fluorescence ◽

Phase Extraction ◽

Bamboo Charcoal ◽

Relative Standard ◽

Polycyclic Aromatic

A solid-phase extraction (SPE) using bamboo charcoal as absorbent coupled with constant wavelength synchronous fluorescence (CWSL) analytical method was developed for the determination of 16 polycyclic aromatic hydrocarbons (PAHs) in environmental water samples. A new method for simultaneous determination for sixteen kinds of polycyclic aromatic hydrocarbons (PAHs) in water was developed by constant wavelength synchronous fluorescence (CWSL) with bamboo charcoal solid phase extraction. The four main factors influencing on extraction efficiency, that is, type and volume of the elution solvent, sampling speed and volume were investigated. A solid-phase extraction with bamboo charcoal cartridges was carried out and the elution was performed with 15 mL of n-hexane. Sampling speed was 5 mL/min. Sampling volume was 500 mL. The linear response of this method was in the range of 0~1000ng/mL (r ≥ 0.9988), the relative standard deviations (RSDs) were in the range of 0.017%~4.12% (n = 6). The detection limits were in the range of 0.052~12.37ng /mL. .By using this method, real samples were determined directly and good results were obtained with the recoveries of 78.87%-107.9%in water from the Longjin river estuary of the provincial control section. The results showed the method was cheap, simple, and could used as an excellent alternative for the routine analysis in environmental field.

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