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.

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

Gas-Liquid Chromatographic Determination of Pentachlorophenol in Mason Jar Lids and Home Canned Foods

1980 ◽  
Vol 63 (5) ◽  
pp. 1125-1127
Author(s):  
David L Heikes ◽  
Kenneth R Griffitt
Keyword(s):  
Fruits And Vegetables ◽  
Gel Permeation Chromatography ◽  
Chromatographic Determination ◽  
Electron Capture Detection ◽  
Gas Liquid Chromatography ◽  
Gel Permeation ◽  
Canned Foods ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A method was developed for the determination of pentachlorophenol (PCP) in the seals and enamel of Mason lids. After extraction with acidic CH2Cl2 and methylation, the resulting pentachloroanisole was determined by gas-liquid chromatography (GLC) with electron capture detection (EC). Three of the 9 brands of lids examined contained PCP. Levels were as high as 198 μg/lid. Recoveries from fortified samples ranged from 92 to 103%. Six fruits and vegetables were canned by home canning techniques, using lids shown to contain PCP. PCP in these foods was determined by a procedure specifying extraction with acidic CH2Cl2 and gel permeation chromatography cleanup. Extracts were methylated and determined by GLC-EC. PCP was found in all the canned foods. Levels were as high as 16 μg/qt. Recoveries from foods fortified with PCP ranged from 85 to 94%. The presence of PCP was confirmed by GLC-mass spectrometric determination of the derivative, pentachloroanisole.

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