Multicolumn Solid-Phase Extraction Cleanup of Organophosphorus and Organochlorine Pesticide Residues in Vegetable Oils and Butterfat

1995 ◽  
Vol 78 (2) ◽  
pp. 431-436 ◽  
Author(s):  
Allesia M Gillespie ◽  
Sean L Daly ◽  
Dalia M Gilvydis ◽  
Felix Schneider ◽  
Stephen M Walters
Keyword(s):  
Solid Phase Extraction ◽  
Vegetable Oils ◽  
Pesticide Residues ◽  
Diatomaceous Earth ◽  
Solid Phase ◽  
Electron Capture Detection ◽  
Phase Extraction ◽  
Lipid Matrix ◽  
Photometric Detection

Abstract Diatomaceous earth columns used with reversed and normal solid phase extraction (SPE) cartridges were evaluated for the quantitative determination of a number of organophosphorus (OP) and organochlorine (OC) pesticide residues in edible vegetable oils and butterfat. An oil or fat sample (about 2 g) in hexane was passed through a diatomaceous earth (Extrelut QE) column and a Cis bonded silica (ODS) SPE cartridge, resulting in the separation of the pesticides from about 98% of the lipids. The eluate was split in half, with the first portion concentrated into acetone for the determination of OP pesticides by gas chromatography with flame photometric detection (GC–FPD). The other half was passed through an Alumina-N SPE cartridge for additional cleanup of lipid matrix to determine OC pesticides by GC with electron-capture detection (GC–ECD). Average recoveries from fortified samples were greater than 89% for the pesticides studied.

scholarly journals Determination of Organochlorine Pesticide and Polychlorinated Biphenyl Residues in Fatty Fish by Tandem Solid-Phase Extraction Cleanup

1996 ◽  
Vol 79 (5) ◽  
pp. 1209-1214 ◽  
Author(s):  
Frank J Schenck ◽  
Lori Calderon ◽  
Lynda V Podhorniak
Keyword(s):  
Solid Phase Extraction ◽  
Organochlorine Pesticide ◽  
Pesticide Residues ◽  
Polychlorinated Biphenyl ◽  
Solid Phase ◽  
Electron Capture Detection ◽  
Phase Extraction ◽  
Fatty Fish ◽  
Organochlorine Pesticide Residues

Abstract A rapid, multiresidue solid-phase extraction (SPE) technique for determination of organochlorine pesticide and polychlorinated biphenyl (PCB) residues in nonfatty fish was modified for use with fatty fish. In the modified procedures, samples are extracted with acetonitrile, and the extract is cleaned up with both C18 and Florisil SPE columns. Residues are determined by gas chromatography with electron capture detection. The original method was modified for use with fatty fish by reducing the amount of tissue extracted and by using an improved Florisil SPE cleanup. Recovery data are presented for 24 fortified organochlorine pesticide residues (0.12 ppm) and 3 fortified PCB residues (0.80 ppm) from flounder, bluefish, and shad samples, which contained 0.8,5.4, and 22.6% fat, respectively. For the 3 types of fish, recoveries of 23 of 24 fortified organochlorine pesticide residues ranged from 55 to 129%, and recoveries of 3 fortified PCB residues ranged from 55 to 104%. There were no significant differences in recovery based on fish species and/or fat content for the majority of residues studied. This SPE method and the official AOAC method yielded comparable results for fish containing incurred organochlorine residues.

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