Determination of organochlorine pesticides and polychlorinated biphenyls in post-mortem human lung by matrix solid-phase dispersion with the aid of response surface methodology and desirability function

2012 ◽  
Vol 1227 ◽  
pp. 1-9 ◽  
Author(s):  
Georgios N. Rallis ◽  
Vasilios A. Sakkas ◽  
Vassiliki A. Boumba ◽  
Theodore Vougiouklakis ◽  
Triantafyllos A. Albanis
Keyword(s):  
Response Surface Methodology ◽  
Polychlorinated Biphenyls ◽  
Organochlorine Pesticides ◽  
Human Lung ◽  
Solid Phase ◽  
Desirability Function ◽  
Post Mortem ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion

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.

scholarly journals Sample Preparation Based on Matrix Solid-Phase Dispersion and Solid-Phase Extraction Cleanup for the Determination of Organochlorine Pesticides in Fish

2010 ◽  
Vol 93 (3) ◽  
pp. 992-998 ◽  
Author(s):  
Mercedes Barriada-Pereira ◽  
María José Gonzlez-Castro ◽  
Soledad Muniategui-Lorenzo ◽  
Purificíon López-Maha ◽  
Daro Prada-Rodrguez
Keyword(s):  
Organochlorine Pesticides ◽  
Solid Phase ◽  
Electron Capture Detection ◽  
Fish Liver ◽  
Fish Tissues ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Dispersing Agent ◽  
Assisted Extraction

Abstract A method based on matrix solid-phase dispersion (MSPD) and SPE to determine 20 organochlorine pesticides (OCPs) in fish tissues (muscle and liver) was optimized in terms of the sorbents and elution solvents used for the analysis. The following analytical components were evaluated: ENVI-Carb and ENVI-18 as dispersing agents, Florisil and Florisil over alumina as cleanup adsorbents, and hexane and hexaneethyl acetate (80 + 20) as elution solvents. The pesticides were determined by GC with electron capture detection. The best results were obtained with ENVI-Carb as a dispersing agent and an ENVI-Florisil co-column using 40 mL hexaneethyl acetate (80 + 20) as the elution solvent. Analytical recoveries ranged between 75 and 130 except for -HCH in fish liver, and the RSD values were <15 for most of the pesticides studied. Furthermore, sensitivity was sufficient (LOD of <300 g/kg) for all OCPs under study, in compliance with the tolerance limits of the U.S. Food and Drug Administration for OCPs in fish. The results were compared with those obtained by microwave-assisted extraction (MAE) and pressurized liquid extraction (PLE) in order to evaluate the performance of the MSPD procedure. The MPSD methodology was shown to be easy to use and fast, with a clear advantage relative to cost, because it does not need the expensive equipment required for MAE and PLE.

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