Effects of Brine Treatment on Pesticide Residues During Recycling of Pickling Brine

1978 ◽  
Vol 61 (6) ◽  
pp. 1441-1444
Author(s):  
Norbert V Fehringer
Keyword(s):  
Liquid Chromatography ◽  
Electron Capture ◽  
Pesticide Residues ◽  
Methylene Chloride ◽  
Gel Permeation Chromatography ◽  
Gas Liquid Chromatography ◽  
Gel Permeation ◽  
Brine Treatment ◽  
Naoh Treatment ◽  
Nitrogen Phosphorus

Abstract The effects of 2 pickle brine recycling treatments on residues of selected insecticides, herbicides, and fungicides are presented. Residues were determined in raw and brined cucumbers, in untreated brine, and in brine following pasteurization or chemical (NaOH) treatment. The samples were extracted with acetone, partitioned into methylene chloride, cleaned up by gel permeation chromatography, and quantitated by gas-liquid chromatography using nitrogen/phosphorus, electron capture, and flame photometric detectors.

Identification of Cholesterol as a Possible Interference in the Analysis of Fish Tissue for Industrial Chemical Residues

1976 ◽  
Vol 59 (5) ◽  
pp. 1187-1188
Author(s):  
Henry C Hollifield
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Electron Capture ◽  
Gel Permeation Chromatography ◽  
Fish Tissue ◽  
Gas Liquid Chromatography ◽  
Tissue Extracts ◽  
Chemical Residues ◽  
Gel Permeation ◽  
Aoac Method

Abstract The presence of cholesterol in cleaned up fish tissue extracts has been established by gas-liquid chromatography and confirmed by mass spectrometry. It was found both in extracts cleaned up by gel permeation chromatography and in those extracts prepared by the AOAC method for nonfatty foods. It is not normally observed in routine residue analyses because selective gas chromatographic detectors such as electron capture are commonly used.

Organochlorine Pesticide Residues in Spanish Meat Products and Meat of Different Species

1994 ◽  
Vol 57 (5) ◽  
pp. 441-444 ◽  
Author(s):  
ANTONIO HERRERA ◽  
AGUSTIN A. ARIÑO ◽  
MARIA P. CONCHELLO ◽  
REGINA LAZARO ◽  
SUSANA BAYARRI ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Organochlorine Pesticides ◽  
Organochlorine Pesticide ◽  
Electron Capture ◽  
Pesticide Residues ◽  
Meat Products ◽  
Gas Liquid Chromatography ◽  
Pork Products ◽  
Organochlorine Pesticide Residues ◽  
Beef Products

The level of organochlorine pesticides in 229 samples of Spanish meat and meat products of different species (lamb, pork, beef and poultry) was investigated. Chlorinated residues were quantitated by gas-liquid chromatography with electron capture detector using packed and capillary columns. Hexachlorobenzene (HCB) and hexachlorocyclohexane (HCH) were detected in all samples. In general, lamb appeared to be more heavily contaminated by HCB and HCH, which reached maximums of 178 ppb (μg/kg on a fat basis) and 505 ppb, respectively. The level of HCB averaged 49 ppb in lamb; varied between 8–18 ppb in pork and beef products; and amounted to 26 ppb in fresh poultry sausages. Of the three isomers of HCH determined, the γ-HCH (lindane) was most frequently detected; 100% in lamb and pork (both meat, cured sausage and pork bologna), and 64 to 94% in fresh sausages of poultry and beef. The level of the HCH group averaged 112 ppb in lamb, 85 ppb in poultry, nearly half that much in pork and pork products, and around 20–40 ppb in beef products. Dieldrin was the only chlorocyclodiene detected: 8 to 15% in pork products, and 28% in fresh poultry sausage. The DDTs in lamb showed 83% of detection, especially in the pp' form of DDE and DDT. The overall contamination with DDT and its metabolites was found to be very moderate averaging 25 ppb, with a maximum of 91 ppb. No residues of aldrin, endrin, heptachlor, heptachlor epoxide, chlordane, methoxychlor, endosulfan or trans-nonachlor were detected.

Extraction and Cleanup of Fish, Sediment, and Water for Determination of Triaryl Phosphates by Gas-Liquid Chromatography

1981 ◽  
Vol 64 (1) ◽  
pp. 79-84
Author(s):  
Derek C G Muir ◽  
Norbert P Grift ◽  
John Solomon
Keyword(s):  
Liquid Chromatography ◽  
Soxhlet Extraction ◽  
Gel Permeation Chromatography ◽  
Gas Liquid Chromatography ◽  
Fish Samples ◽  
Alumina Treatment ◽  
Diphenyl Phosphate ◽  
Nitrogen Phosphorus ◽  
Acetone Hexane

Abstract Several techniques were evaluated for extracting triphenyl phosphate (TPP), 14C-labeled TPP, cresyl diphenyl phosphate, and tricresyl phosphate isomers (o-TCP, m-TCP, and p-TCP) from fish and sediment samples. Extracts of fish samples were cleaned up by gel permeation chromatography/alumina column chromatography; sediment extracts received alumina treatment only. Compounds were determined by gas-liquid chromatography (GLC) with nitrogenphosphorus detection. Methanol/Polytron and hexane/ball mill extraction of fish samples fortified at 0.01, 0.1, and 1.0 μg/g levels gave overall recoveries of the 5 compounds of 89 and 97%, respectively. Methanol recovered more radioactivity (97%) from fish exposed to 14C-TPP in aquaria for 24 h than did hexane from fish exposed for 16 h (79%). Refluxing fortified sediment (0.05 and 0.5 μg/g) with methanol-water (9+1) gave significantly higher recoveries (88%) of the 5 triaryl phosphates than did dichloromethane-methanol (1+1) reflux or acetone-hexane (1+1) Soxhlet extraction. Recoveries of TPP and o-, m- and p-TCP from fortified river water (0.5, 5.0, and 50 μg/L) by shaking with dichloromethane ranged from 91 to 118%. Some problems were encountered with interfering GLC peaks at low (μg/g) levels in fish and sediment extracts despite the use of nitrogen-phosphorus specific detectors.

Determination of iV-Methylcarbamate Pesticides in Liver by Liquid Chromatography

1989 ◽  
Vol 72 (4) ◽  
pp. 586-592 ◽  
Author(s):  
Sher M Ali
Keyword(s):  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Fluorescence Detection ◽  
Methylene Chloride ◽  
Gel Permeation Chromatography ◽  
Purification Technique ◽  
Coefficients Of Variation ◽  
Gel Permeation ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method using a 2-step purification technique for the simultaneous determination of 10 carbamates in bovine, swine, and duck livers has been developed. Carbamates are extracted from liver samples with methylene chloride. After evaporation, the residues from the extract are dissolved in methylene chloride- cyclohexane (1 + 1) and cleaned up by gel permeation chromatography. The eluate containing carbamate residues is evaporated to dryness, reconstituted in methylene chloride, further purified by passing it through an aminopropyl Bond Elut extraction cartridge, and analyzed by liquid chromatography using post-column derivatization with orthophthalaldehyde and fluorescence detection. Excitation and emission are set at 340 and 418 nm, respectively. Liver samples for beef, pork, and duck were fortified with 5, 10, and 20 ppb of mixed carbamate standards. The average of 10 recoveries of 10 carbamates at all 3 levels of fortification was greater than 80% with coefficients of variation less than 17%.

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 Nitrogen- and Phosphorus-Containing Pesticide Residues in Vegetables by Gas Chromatography with Nitrogen–Phosphorus and Flame Photometric Detection after Gel Permeation Chromatography and a Two-Step Minicolumn Cleanup

2003 ◽  
Vol 86 (6) ◽  
pp. 1241-1251 ◽  
Author(s):  
Eiji Ueno ◽  
Harumi Oshima ◽  
Isao Saito ◽  
Hiroshi Matsumoto
Keyword(s):  
Gas Chromatography ◽  
Pesticide Residues ◽  
Gel Permeation Chromatography ◽  
Good Resolution ◽  
Photometric Detection ◽  
Relative Standard ◽  
Phosphorus Containing ◽  
Gel Permeation ◽  
Flame Photometric Detection ◽  
Nitrogen Phosphorus

Abstract An efficient and reliable multiresidue method for determining pesticide residues in a large number of vegetable samples was studied. First, the important target compounds for monitoring, 52 nitrogen-and/or phosphorus-containing pesticides, were selected. The sample was extracted with acetonitrile, and the separated acetonitrile layer was cleaned up by a salting-out step. The acetonitrile extract was purified by gel permeation chromatography that divided the pesticide eluate into 2 fractions; the pesticide fractions were respectively purified by a 2-step minicolumn cleanup in which the second pesticide fraction was loaded on a silica-gel minicolumn. After a Florisil minicolumn was inserted on the silicagel minicolumn, the first pesticide fraction was loaded on the tandem minicolumn, which was eluted with acetone–petroleum ether (3 + 7). The combined eluate was subjected to dual-column gas chromatography (GC) with nitrogen–phosphorus and flame photometric detection. By application of the optimum cleanup conditions to the 52 pesticides selected, good resolution and low breakdown levels of the pesticides during GC were maintained. Recoveries of the 52 pesticides from fortified cabbage, lettuce, spring onion, and spinach ranged from 72 to 108% with relative standard deviations of 2–17%, except for the recoveries of methamidophos and chlorothalonil. The detection limits of the pesticides were satisfactory (0.001–0.009 mg/kg) for monitoring pesticide residues in vegetables.

Collaborative Study of an Extension of the Mills et al. Method for the Determination of Pesticide Residues in Foods

1976 ◽  
Vol 59 (1) ◽  
pp. 169-171
Author(s):  
Charles E Finsterwalder
Keyword(s):  
Liquid Chromatography ◽  
Potassium Chloride ◽  
Electron Capture ◽  
Pesticide Residues ◽  
Collaborative Study ◽  
Heptachlor Epoxide ◽  
Gas Liquid Chromatography ◽  
Standard Deviations

Abstract Fifteen laboratories collaboratively determined parathion, o,p′-DDT, p,p′-DDT, and p,p′-DDE in kale, and lindane, dieldrin, heptachlor epoxide, and p,p′-DDE in eggs, using electron capture gas-liquid chromatography (potassium chloride thermionic detector for parathion). Pesticide levels ranged from 0.033 ppm heptachlor epoxide to 3.32 ppm p,p′-DDT. Mean recoveries (± standard deviations) were: parathion 91±15%, o,p′-DDT 99±8%, p,p′-DDT 97±8%, lindane 94±4%, dieldrin 106±8%, heptachlor epoxide 106±5%, p,p′-DDE 94±8% in eggs and 101±9% in kale. The methods have been adopted as official first action.

Collaborative Study of the Determination of Endosulfan, Endosulfan Sulfate, Tetrasul, and Tetradifon Residues in Fresh Fruits and Vegetables

1976 ◽  
Vol 59 (1) ◽  
pp. 209-212
Author(s):  
Lawrence R Mitchell
Keyword(s):  
Liquid Chromatography ◽  
Petroleum Ether ◽  
Electron Capture ◽  
Fruits And Vegetables ◽  
Methylene Chloride ◽  
Collaborative Study ◽  
Gas Liquid Chromatography ◽  
Endosulfan Sulfate ◽  
Florisil Column

Abstract A method for the determination of endosulfan I, endosulfan II, endosulfan sulfate, tetrasul, and tetradifon residues in fresh fruits and vegetables was studied collaboratively. The method consists of extraction of the product with acetonitrile, extract cleanup by partition with petroleum ether and elution from a Florisil column with mixtures of hexane, methylene chloride, and acetonitrile, and determination of the residues by electron capture gas-liquid chromatography. This method was studied by 8 collaborators, using apples and cucumbers as the samples. Each sample was spiked with 2 levels of each pesticide. The average per cent recoveries for apples and cucumbers, respectively, were as follows: endosulfan I, 103.6 and 101.5; endosulfan II, 102.9 and 100.0; endosulfan sulfate, 100.9 and 92.9; tetrasul, 98.8 and 102.2; and tetradifon, 106.4 and 101.9. The method has been adopted as official first action.

Sensitive and Specific Gas-Liquid Chromatographic-Spectrophotometric Screening Procedure for Trace Levels of Five Sulfonamides in Liver, Kidney, and Muscle Tissue

1978 ◽  
Vol 61 (5) ◽  
pp. 1050-1053
Author(s):  
Donald P Goodspeed ◽  
Randy M Simpson ◽  
Raymond B Ashworth ◽  
Jerry W Shafer ◽  
Henry R Cook
Keyword(s):  
Liquid Chromatography ◽  
Electron Capture ◽  
Muscle Tissue ◽  
Ethyl Ether ◽  
Methylene Chloride ◽  
Animal Tissue ◽  
Gas Liquid Chromatography ◽  
Separatory Funnel ◽  
Liquid Chromatographic ◽  
Ppm Level

Abstract Free and conjugated sulfonamides are extracted from edible animal tissue with acetone. Carbohydrate "is precipitated and removed, and the acetone is evaporated. The residue is transferred to a separatory funnel with ethyl ether and 17V HC1. The acid layer is drawn off and a portion of the 17V HC1 is screened, using the Bratton-Marshall reaction. If this portion is positive, the remaining portion is buffered to pH 6.5 and extracted with methylene chloride. The residue is methylated with diazomethane and then acylated with pentafluoropropionic anhydride. The resulting derivatives are detected by gas-liquid chromatography, using electron capture (63Ni) detection and a column packed with 3% OV-17 on Gas-Chrom Q. This method has been validated by recovering sulfathiazole, sulfachloropyrazine, sulfamethazine, sulfadimethoxine, and sulfabromomethazine from liver, kidney, and muscle at levels of 0.1, 0.5, and 1.0 ppm. The 5 sulfonamides were recovered in excess of 60%, with an average mean recovery of 81.5% at the 0.1 ppm level, 79.1% at the 0.5 ppm level, and 76.0% at the 1.0 ppm level.

Validation Study of a Method for Pesticide Residues in Foods and Animal Feeds

1967 ◽  
Vol 50 (6) ◽  
pp. 1205-1215
Author(s):  
Clyde E Wells
Keyword(s):  
Liquid Chromatography ◽  
Petroleum Ether ◽  
Electron Capture ◽  
Pesticide Residue ◽  
Drug Administration ◽  
Validation Study ◽  
Pesticide Residues ◽  
Animal Feed ◽  
Gas Liquid Chromatography ◽  
Florisil Column

Abstract Eighteen laboratories of the Food and Drug Administration tested a multi-pesticide residue method using 65 pesticides and 80 food and animal feed products. Recoveries of 32 pesticides averaged between 80 and 110%; 20 additional pesticides were recovered with some degree of success; and 13 of the pesticides tested were not recovered. The method tested is based on the AOAC procedure which involves extraction of the pesticides with acetonitrile, partition into petroleum ether, cleanup on a Florisil column, and gas-liquid chromatography. Recoveries were essentially independent of the type of product. Of the products tested, only carrots, parsnips, onions, and lettuce exhibited serious interference when the electron capture detector was used

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