Rapid screening of polychlorinated biphenyls in sediments using non-equilibrium solid-phase microextraction and fast gas chromatography with electron-capture detection

2006 ◽  
Vol 1124 (1-2) ◽  
pp. 43-50 ◽  
Author(s):  
R. Montes ◽  
M. Ramil ◽  
I. Rodríguez ◽  
E. Rubí ◽  
R. Cela
Keyword(s):  
Gas Chromatography ◽  
Polychlorinated Biphenyls ◽  
Electron Capture ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Rapid Screening ◽  
Electron Capture Detection ◽  
Fast Gas Chromatography ◽  
Equilibrium Solid Phase ◽  
Non Equilibrium

scholarly journals Multiresidue Determination of Organochlorine Pesticides and Polychlorinated Biphenyls in Milk by Gas Chromatography with Electron-Capture Detection after Extraction by Matrix Solid-Phase Dispersion

2001 ◽  
Vol 84 (5) ◽  
pp. 1561-1568 ◽  
Author(s):  
Cristina Yagüe ◽  
Susana Bayarri ◽  
Regina Lázaro ◽  
Pilar Conchello ◽  
Agustín Ariño ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Polychlorinated Biphenyls ◽  
Organochlorine Pesticides ◽  
Electron Capture ◽  
Analytical Method ◽  
Solid Phase ◽  
Electron Capture Detection ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Repeatability And Reproducibility

Abstract A multiresidue analytical method based on matrix solid-phase dispersion was developed to analyze liquid milk for 22 organochlorine pesticides (OCPs) and 6 polychlorinated biphenyls (PCBs). Initial extraction is performed by loading 3 mL milk onto a 2.0 g octadecyl (C18)-bonded silica cartridge with n-hexane as the eluant. Neutral alumina column chromatography with sodium sulfate as the drying agent is used for further cleanup. The eluate is concentrated to 0.5 mL, and target analytes are determined by capillary gas chromatography with electron-capture detection. The optimized method was validated by determining accuracy (recovery percentages), precision (repeatability and reproducibility), and sensitivity (detection and quantitation limits) from analyses of milk samples fortified at 10 and 1 μg/L levels. Average recoveries were between 74 and 106% for all residues except β-HCH, β-endosulfan, and endosulfan sulfate. Both repeatability and reproducibility relative standard deviation values were < 22% for all residues. Detection limits ranged from 0.02 to 0.12 μg/L and quantitation limits were between 0.02 and 0.62 μg/L. The proposed analytical method may be used as a fast and simple procedure in routine determinations of OCPs and PCBs in milk.

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