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.

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.

A Rapid Multiresidue Screen for Organophosphorus, Organochlorine, and N-Methyl Carbamate Insecticides in Plant and Animal Tissues

1994 ◽  
Vol 77 (5) ◽  
pp. 1263-1274 ◽  
Author(s):  
Dirk M Holstege ◽  
David L Scharberg ◽  
Elizabeth R Tor ◽  
Laura C Hart ◽  
Francis D Galey
Keyword(s):  
Ethyl Acetate ◽  
Solid Phase ◽  
Gel Permeation Chromatography ◽  
Bovine Liver ◽  
Animal Tissues ◽  
Average Recovery ◽  
Carbamate Insecticides ◽  
High Lipid ◽  
Level Method

Abstract A multiresidue screen for the quantitative determination of 43 organ op hosphorus, 17 orga no-chlorine, and 11 N-methyl carbamate insecticides in 10 g of plant or animal tissues is described. The insecticides are extracted with 5% ethanol in ethyl acetate (v/v). Samples with high lipid content are cleaned up by automated gel permeation chromatography with a 30% ethyl acetate in hexane (v/v) eluant and in-line silica gel minicolumns. Highly pigmented samples are cleaned up with class-specific solid-phase extraction columns. The concentrated extracts are analyzed by selective detection with gas chromatography or liquid chromatography. Recovery of 71 insecticides ranged from 77 to 113%. Analysis of fortified bovine liver (n = 5) resulted in an average recovery of 96 ± 4% at the 0.5 to 0.05 μg/g level. Analysis of fortified alfalfa hay (n = 5) resulted in a mean recovery of 94 ± 4% at the 0.06 to 0.5 μg/g level, and analysis of fortified fresh tomatoes (n = 5) resulted in an average recovery of 97 ± 3% at the 0.06 to 0.5 μg/g level. Method detection limits ranged from 0.02 to 0.5 μg/g for the compounds studied with a nominal 10 g sample.

Multiresidue Method for Determination of Organophosphorus Insecticide Residues in Fatty Processed Foods by Gel Permeation Chromatography

1995 ◽  
Vol 78 (6) ◽  
pp. 1502-1512 ◽  
Author(s):  
Anna Sannino ◽  
Paola Mambriani ◽  
Mirella Bandini ◽  
Luciana Bolzoni
Keyword(s):  
Methylene Chloride ◽  
Organophosphorus Compounds ◽  
Gel Permeation Chromatography ◽  
Gas Chromatography Mass Spectrometry ◽  
Gas Liquid Chromatography ◽  
Processed Foods ◽  
Multiresidue Method ◽  
Photometric Detection ◽  
Gel Permeation

Abstract A multiresidue method for quantitative determination of 39 organophosphorus compounds (parent pesticides and their major metabolites) in 7 fatty processed foods is described. Samples are extracted with methylene chloride and cleaned up by automated gel permeation chromatography with a Biobeads SX3 column and a methylene–chloridecyclohexane (15 + 85) eluant. Organophosphorus compounds are quantitated by capillary gas-liquid chromatography with flame photometric detection using OV-1701 and DB-5 columns. Average recoveries from samples fortified at 0.025–1 mg/kg ranged from 50.6% for dichlorvos to 185% for malaoxon. Determination limits were between 0.005 and 0.040 μg/mL. Results were confirmed by gas chromatography/mass spectrometry with selected-ion monitoring.

scholarly journals Determination of Organotins in Aquatic Food by Gas Chromatography with Pulsed Flame Photometric Detection

2008 ◽  
Vol 91 (3) ◽  
pp. 653-659 ◽  
Author(s):  
Zhao Yun-Feng ◽  
Zhao Kong-Xiang ◽  
Wu Yong-Ning
Keyword(s):  
Gas Chromatography ◽  
Standard Deviation ◽  
Gel Permeation Chromatography ◽  
Photometric Detection ◽  
Relative Standard ◽  
Gel Permeation ◽  
Flame Photometric Detection ◽  
Aquatic Food ◽  
Derivative Products

Abstract A method based on gas chromatography (GC)-pulsed flame photometric detection (PFPD) was developed to determine the levels of organotins in aquatic food. After being purified by gel-permeation chromatography in ethyl actatetetrahydrofuran, the organotin compounds were derivatized by pentylmagnesium bromide. The derivative products were injected into the GC system and detected by PFPD (sulfur mode). The method was validated by analysis of the certified reference material and spiked samples. Recoveries of organotins ranged from 84.1 to 116.6 with relative standard deviation between 1.3 and 16.0 when spiked at levels of 2, 10, and 40 g/kg. The limits of detection varied from 0.1 to 1.2 g/kg for shellfish and 0.1 to 0.5 g/kg for fish. The proposed method was suitable for determining organotins in aquatic foods.

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