scholarly journals Cleanup Procedure for Monitoring Chlorinated Compounds in Animal Feed and Crops

1998 ◽  
Vol 81 (3) ◽  
pp. 513-518 ◽  
Author(s):  
Mona Syhre ◽  
Gudrun Hanschmann ◽  
Ralf Heber
Keyword(s):  
Gas Chromatography ◽  
Silica Gel ◽  
Carbon Material ◽  
Animal Feed ◽  
Gel Permeation Chromatography ◽  
Electron Capture Detection ◽  
Chlorinated Pesticides ◽  
Gel Permeation ◽  
Cleanup Procedure

abstract A powerful cleanup procedure for determination of chlorinated pesticides and poly chlorinated biphenyls (PCBs) in difficult agricultural matrixes like feeds or crops was developed to eliminate the interferences in chromatograms obtained by gas chromatography with electron capture detection. The adsorption material used was ENVI-Carb, a graphitized nonporous carbon material. This procedure proved to be more reliable than the established cleanup procedure, which uses gel permeation chromatography and silica gel cartridges. Because ENVI-Carb cleanup delivers clear, colorless eluates with no interferences, chlorinated pesticides and PCBs may be detected at levels as low as 0.0004 mg/kg for monitoring purposes. Accuracy was validated through a series of recovery experiments.

scholarly journals Gel Permeation and Florisil Chromatographic Cleanup and Gas Chromatographic Determination of Organochlorine Pesticides in Eggs

1998 ◽  
Vol 81 (5) ◽  
pp. 1033-1036 ◽  
Author(s):  
Naoto Furusawa ◽  
Kunio Okazaki ◽  
Sachiko Iriguchi ◽  
Hidemasa Yamaguchi ◽  
Minoru Saitoh
Keyword(s):  
Gas Chromatography ◽  
Organochlorine Pesticides ◽  
Mobile Phase ◽  
Gel Permeation Chromatography ◽  
Chromatographic Determination ◽  
Electron Capture Detection ◽  
Coefficients Of Variation ◽  
Gel Permeation ◽  
Whole Egg

Abstract Cleanup of residual organochlorine pesticides (OCPs; α-, β-, γ-, and δ-BHC; aldrin; dieldrin; p,p′-DDE; o,p′-DDT; p,p′-DDD; and p,p′-DUX) in eggs by gel permeation chromatography (GPC) and Florisil minicolumn chromatography is described. Ten OCPs in purified extract are determined by gas chromatography with electron capture detection. The lipids extracted from whole egg are cleaned up first by GPC with an Envirogel column and an ethyl acetate-cychlohexane (1 + 1, v/v) mobile phase and then by Florisil minicolumn chromatography with 15% (v/v) diethyl ether-hexane eluant. Cleanup is highly efficient. Average recoveries of 10 spiked OCPs (0.0025-0.0125 ppm) ranged from 81 to 101%, with coefficients of variation between 1 and 14%. The detection limit was 0.001 ppm for the 10 OCPs

Simple, Low-Cost Method for Determination of Selected Chlorinated Pesticides in Fat Samples

1982 ◽  
Vol 65 (3) ◽  
pp. 677-679 ◽  
Author(s):  
Stefan M Waliszewski ◽  
Grzegorz A Szymczyński
Keyword(s):  
Gas Chromatography ◽  
Petroleum Ether ◽  
Electron Capture ◽  
Silica Gel ◽  
Pesticide Residues ◽  
Low Cost ◽  
Electron Capture Detection ◽  
Chlorinated Pesticides ◽  
Qualitative Determination

Abstract A method is described for the quantitative and qualitative determination of selected chlorinated pesticides in fat samples. Pesticide residues are extracted with petroleum ether and separated from fat with concentrated H2SO4 instead of the commonly used adsorbents Florisil, alumina, or silica gel. Residues were analyzed by gas chromatography with electron capture detection. Recoveries of fortified samples were approximately 100%.

Novel Cleanup Method for Quantitative Gas Chromatographic Determination of Trace Amounts of Di-2-Ethylhexyl Phthalate in Fish Lipid

1981 ◽  
Vol 64 (2) ◽  
pp. 282-286 ◽  
Author(s):  
B Garth Burns ◽  
Charles J Musial ◽  
John F Uthe
Keyword(s):  
Gel Permeation Chromatography ◽  
Chromatographic Determination ◽  
Confirmatory Test ◽  
Fish Lipid ◽  
Gel Permeation ◽  
Fish Lipids ◽  
Cleanup Procedure ◽  
Quantitative Analyses ◽  
Ethylhexyl Phthalate

Abstract A new, simple, and rapid cleanup procedure is described for di-2-ethylhexyl phthalate (DEHP) residues in fish lipids. Extracts are chromatographed on small alumina:sulfuric acid-impregnated alumina (layered) columns after gel permeation chromatography of the fish lipid extracts on BioBeads SX-3. Quantitative analyses were carried out by electron capture gas chromatography using 2 columns. Spiked DEHP recoveries varied from 79.3% in mackerel to 86.1% in herring. DEHP concentrations were determined in plaice, eel, redfish, herring, cod, and mackerel tissues and ranged from trace (<0.001 µ/g) to approximately 10 µ/g (wet wt basis). Ethanolic KOH saponification of the purified DEHP fraction, resulting in the disappearance of the DEHP peak, was used as a confirmatory test. Limited studies with dibutyl, di-n-heptyl, and diethyl phthalates suggest that the method can be made more versatile.

Multiresidue Screen for Organophosphorus Insecticides Using Gel Permeation Chromatography—Silica Gel Cleanup

1991 ◽  
Vol 74 (2) ◽  
pp. 394-399 ◽  
Author(s):  
Dirk M Holstege ◽  
David L Scharberg ◽  
Elizabeth R Richardson ◽  
Gregory Möller
Keyword(s):  
Silica Gel ◽  
Gel Permeation Chromatography ◽  
Bovine Liver ◽  
Rumen Content ◽  
Organophosphorus Insecticides ◽  
Photometric Detection ◽  
Gel Permeation ◽  
Level Method ◽  
Level Analysis

Abstract A multiresidue screen for quantitative determination of 43 organophosphorus insecticides In 5 g of plant and animal tissues Is described. The organophosphorus insecticides are extracted with methanol-dichloromethane (10 + 90, v/v) and cleaned up using automated gel permeation chromatography with hexane-ethyl acetate (60 + 40) eluant and in-line silica gel minicolumns. Concentrated extracts are analyzed by gas chromatography with flame photometric detection. The method recovers 43 organophosphorus insecticides in the range of 72 to 115%. Analysis of fortified bovine liver (n = 5) shows an average 95.9 ± 4.8% recovery at the 0.05 μg/g level and 93 ± 3.8% at the 0.5 μg/g level. Analysis of fortified bovine rumen content (n = 5) shows an average 98 ± 4.2% recovery at the 0.1 μg/g level and 98.7 ± 2.8% at the 1 μg/g level. Method detection limits ranged from 0.01 to 0.05 μg/g for the compounds studied using a nominal 5 gram sample.

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