scholarly journals Determination of Pentachlorophenol Residue in Meat and Fish by Gas Chromatography–Electron Capture Detection and Gas Chromatography–Mass Spectrometry with Accelerated Solvent Extraction

2013 ◽  
Vol 52 (5) ◽  
pp. 429-435 ◽  
Author(s):  
Dongmei Zhao
2001 ◽  
Vol 84 (4) ◽  
pp. 1194-1201 ◽  
Author(s):  
Luise Wennrich ◽  
Peter Popp ◽  
Gábor Köller ◽  
Jürgen Breuste

Abstract An analytical scheme for the determination of several organochlorine pesticides like hexachlorocyclohexanes (HCHs) and DDX compounds (p,p′-DDE, p,p′-DDD, and p,p′-DDT) as well as chlorobenzenes in strawberries has been developed. The procedure is based on aqueous accelerated solvent extraction (ASE) followed by solidphase microextraction (SPME) or stir bar sorptive extraction (SBSE) and subsequent thermodesorption–gas chromatography/mass spectrometry analysis. A 65 μm polydimethylsiloxane/divinylbenzene fiber was chosen for the SPME experiments. Significant SPME and ASE parameters were optimized using spiked water and strawberry samples. For the ASE of the organochlorine compounds, a water–acetone mixture (90 + 10, v/v) as the extraction solvent, an extraction temperature of 120°C, and 2 cycles of 10 min extraction proved optimal. The developed method was evaluated with respect to precision and limits of detection (LOD). The relative standard deviations of replicate ASE–SPME determinations (n = 5) were in the range of 4–24%. LOD values between 1 and 10 μ g/kg were achieved with the exception of DDT and DDE (40 μg/kg). Using SBSE, the LOD of these compounds could be improved (2 and 5 μg/kg). The main advantages of this method are the avoidance of cleanup and concentration procedures as well as the significant reduction of the required volume of organic solvents. The described method was applied to the determination of the pollutants in strawberry samples collected from different allotment gardens in a potentially polluted area, the Bitterfeld-Wolfen region (Germany).


Author(s):  
Cuicui Kang ◽  
Haijian Ma ◽  
Yuan Li ◽  
Chizhong Zhang ◽  
Yueqin Hong ◽  
...  

AbstractThe aim of the experiment is to establish a method for the determination of acrylamide in food by automatic accelerated solvent extraction-gas chromatography-mass spectrometry. D3-acrylamide was used as isotope internal standard, crushed samples were extracted and purified by automatic accelerated solvent, acrylamide was derivatized into 2,3-dibromopropanamide by potassium bromide and potassium bromate under acidic conditions, and then the derivative was extracted by ethyl acetate and detected by gas chromatography-mass spectrometry. The method had a good linear relationship in the concentration range of 10–2000 ng/mL, and the coefficient of determination (R2) was 0.9997. The detection limit of the method was 3 μg/kg. The quantification limit of the method was 10 μg/kg. The standard addition recovery of acrylamide was between 105 and 120%, and the relative standard deviation of the recovery of acrylamide was less than 3.0%. The experimental result showed that the method was simple, sensitive, efficient and accurate, and could be used for the determination of acrylamide in food.


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