Gas-Liquid Chromatographic Determination of Fenvalerate Insecticide Residues in Processed Apple Products and By-Products

1982 ◽  
Vol 65 (5) ◽  
pp. 1106-1111
Author(s):  
Terry D Spittler ◽  
Robert J Argauer ◽  
Donald J Lisk ◽  
Ralph O Mumma ◽  
George Winnett ◽  
...  

Abstract Apples from trees treated in the field at 2-week intervals (9 foliar applications) with the synthetic pyrethroid insecticide fenvalerate (cyano(3-phenoxyphenyL)methyl 4-chloro-alpha-(1-methylethyl)- benzeneacetate) were processed into apple sauce, juice, pomace, and peels plus cores. Gas-liquid chromatographic analysis of the commodities for fenvalerate showed the sauce and juice to be essentially residue-free, the whole apples to contain about 0.4 ppm, and the pomace and peels plus cores to contain about 2 and 1.5 ppm, respectively. Agreement among 5 laboratories using modifications of the same basic method was good.

1984 ◽  
Vol 67 (4) ◽  
pp. 824-826
Author(s):  
Terry D Spittler ◽  
Robert J Argauer ◽  
Donald J Lisk ◽  
Ralph O Mumma ◽  
George Winnett ◽  
...  

Abstract The results of a 5-laboratory collaborative determination of residues of the synthetic pyrethroid insecticide fenvalerate in tomato products are presented. Tomatoes from plants treated in the field at 2-4 day intervals (13 foliar applications) were processed into chopped fresh tomatoes, canned quarters, juice, paste, and the by-product skins plus seeds. Gas chromatographic analysis of the commodities for fenvalerate showed the fresh produce to contain 0.26 ppm, and the skins plus seeds contained 1.9 ppm. Residues were barely detectable in canned peeled quarters and juice, but averaged 0.12 ppm for paste, the concentration product of juice. High residues were associated with the skin content of the product. Five laboratories using modifications of the same analytical technique obtained good collaborative agreement.


1999 ◽  
Vol 82 (6) ◽  
pp. 1303-1307 ◽  
Author(s):  
Eva Dudriková ◽  
Sokol Jozef ◽  
Nagy Jozef

Abstract Liquid chromatographic analysis of milk samples from 6 cows treated with tylosin in a veterinary practice indicated that tylosin persisted in milk for more than 3 days after the final treatment. The concentration of tylosin was not below the stated maximum residue limit (0.05 mg/kg). The milk from 3 cows being treated for mastitis catarrhalis chronica contained tylosin residues for 3.5 days after the last withdrawal time (72 h). No residue was detected in the milk of any animal 6 days after cessation of therapy.


1987 ◽  
Vol 70 (4) ◽  
pp. 626-630 ◽  
Author(s):  
Jose E Roybal ◽  
Robert K Munns ◽  
Jeffrey A Hurlbut ◽  
Wilbert Shimoda ◽  
Thomas R Morrison ◽  
...  

Abstract A simple and rapid method is described for the determination of dimetridazole (DMZ) and ipronidazole (IPR) in swine feeds at various levels (0.11-110 ppm). The drugs are released from feed by prewetting with a buffer, followed by extraction with either methanol or methylene chloride, depending on the drug level; if necessary, an acid-base cleanup is used before the liquid chromatographic analysis. The analytes are separated on a C18 column and monitored at 320 nm for detection and quantitation. Recoveries of DMZ from several feed formulations averaged 108% at the 92.8 ppm level with a standard deviation (SD) of 4.00% and a coefficient of variation (CV) of 3.70%, 101% at the 11.2 ppm level with an SD of 11.9% and a CV of 11.8%, and 100% at the 0.112 ppm level with an SD of 9.27% and a CV of 9.25%. Recoveries of IPR averaged 77.1% at the 12.9 ppm level with an SD of 1.75% and a CV of 2.27%; IPR recoveries averaged 35.2% at the 0.129 ppm level with an SD of 3.39% and a CV of 9.63%.


1976 ◽  
Vol 59 (5) ◽  
pp. 1094-1096
Author(s):  
Vincent B Stein ◽  
Kenneth A Pittman

Abstract A new method for the determination of azinphos ethyl (O,O-diethyl-S-(4-oxo-1,2,3-benzotriazin-3(4H)-ylmethyl) phosphorodithioate) in human plasma and in mouse plasma, tissue, and fat has been developed. The method is based on extraction with benzene or hexane and cleanup of fat and tissue samples by a minicolumn containing Florisil and sodium sulfate. Azinphos ethyl is eluted from the column with 10% acetonitrile in benzene and is concentrated to an appropriate volume for gas-liquid chromatographic analysis, using a 63Ni electron capture detector and a glass column containing 3% OV-1 on Gas-Chrom Q. The method is sensitive to 0.005 ppm in human plasma, 0.01 ppm in mouse plasma, 0.08 ppm in mouse liver, 0.05 ppm in mouse brain, and 0.10 ppm in mouse fat. The limit of detection is 2 pg; mean recoveries ranged from 96 to 98%.


1989 ◽  
Vol 72 (3) ◽  
pp. 468-470 ◽  
Author(s):  
Timothy H Begley ◽  
Henry C Hollifield

Abstract A precipitation procedure and liquid chromatography (LC) were used to measure the residual reactants and reaction by-products in polyethylene terephthalate (PET) polymers and food packages. The polymer is dissolved in l,l,l,3,3,3-hexafluoro-2-propanol/methyIene chloride and then precipitated with acetone. The filtered solution is evaporated almost to dryness, and the concentrate is diluted with dimethylacetamide for LC analysis. Recoveries for terephthalic acid (TA), bis(2-hydroxyethyl) terephthalate (BHET), and the PET cyclic trimer averaged 95,104, and 98%, respectively. The residual levels of TA, BHET, monohydroxy ethylene terephthalic acid, and the PET cyclic trimer were measured in commercial resins and food packages.


1972 ◽  
Vol 55 (6) ◽  
pp. 1219-1222
Author(s):  
Victor W Winkler ◽  
John M Yoder

Abstract A method for the quantitative determination of menadione bisulfite addition products in feed premixes is presented. The menadione bisulfite compound is extracted with methanol from the premix and is determined by gas chromatography directly without pretreatment with alkali. The principle of the method is on-column pyrolysis of menadione bisulfite and subsequent gas chromatographic analysis of the pyrolytic product, menadione.


1976 ◽  
Vol 59 (4) ◽  
pp. 859-861
Author(s):  
Barbara Dohman Ammann ◽  
Daniel J Call ◽  
Hans A Draayer

Abstract A method has been developed for the extraction and determination of alachlor (2-chloro-2′,6′-diethyl-N-(methoxymethyl)-acetanilide) residues in green corn and soybeans. Residues are extracted with acetonitrile and cleaned up on a Fiorisil column. The methylene chloride extract is sufficiently clean for electron capture gas-liquid chromatographic analysis and for verification by thin layer chromatography. Average recoveries of spiked samples (0.2 ppm) were 69 and 82% for corn and soybeans, respectively. This procedure could be useful for the detection of the parent compound in these crops soon after field application, but it does not detect metabolites.


1984 ◽  
Vol 67 (3) ◽  
pp. 655-657
Author(s):  
Denis R Lauren

Abstract A simple, direct method is described for determining carbofuran (CF), 2,3-dihydro-2,2-dimethyl-7-benzofuranyl methylcarbamate, in soils. Methanol extraction is followed by hexane–methanol–water (2 + 4 + 1) partition and liquid chromatographic analysis of the aqueous layer with UV detection at 280 nm. The method specifies dilution of the partitioned extract with water to methanol–water (20 + 80), and injection of 1000 μL sample volumes. This technique allowed a 10-fold increase in sensitivity over direct injection from the partition step. Recovery of CF by the method is about 90%, and less than 0.4 μg CF/ g soil can be detected at a medium detector sensitivity of 0.04 AUFS.


1977 ◽  
Vol 60 (4) ◽  
pp. 908-910
Author(s):  
Narayan S Talekar

Abstract A gas-liquid chromatographic method is described for residues of a synthetic pyrethroid, Sumicidin (α-cyano-3-phenoxybenzyl α-isopropyl-4-chlorophenylacetate), on cabbage. The plant material is Soxhlet-extracted with hexaneacetone (1+l) and subsequently cleaned up on Florisil with benzene-ethyl acetate (9+1) eluting solvent. Gas-liquid chromatographic analysis was performed on a 0.5 m × 2 mm stainless steel column containing 3% OV-101 + 3% Apiezon L on 80–100 mesh Gas-Chrom Q, with tritium electron capture detection. Sumicidin recovery was 97% when added at the 0.5 ppm level. Routine Sumicidin residue monitoring data presented.


1980 ◽  
Vol 63 (3) ◽  
pp. 517-522 ◽  
Author(s):  
Julia R Ferreira ◽  
Antonio M S Silva Fernandes

Abstract A method intended for regulatory purposes is described for the determination of organophosphorus insecticide residues in fruits and vegetables. Eighteen organophosphorus insecticides, azinphos-ethyl, chlorpyrifos, diazinon, dichlorvos, dimethoate, ethion, ethoate-methyl, fenitrothion, fenthion, formothion, malathion, methidathion, mevinphos, parathion, phosalone, phosphamidon, thiometon, and trichlorphon, and 7 metabolites, fenitrooxon, fenthion sulfoxide, fenthion sulfone, malaoxon, desethylphosphamidon, thiometon sulfoxide, and thiometon sulfone, were extracted from different crops with acetone and partitioned into hexane or ethyl acetate, according to their polarities. The hexane extract was cleaned up by eluting from a Florisil column with acetone-hexane (4+96). The ethyl acetate extract needs no cleanup. The concentrated extracts were analyzed by gasliquid chromatography using thermionic detectors. Recoveries conducted at fortification levels ranging from 0.1 to 2 mg/kg were in most cases above 80%. The limit of sensitivity is less than 0.1 mg/kg.


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