Electron Capture Gas Chromatographic Determination of Traces of Formaldehyde in Milk as the 2,4-Dinitrophenylhydrazone

1986 ◽  
Vol 69 (4) ◽  
pp. 655-657
Author(s):  
Katherine E Buckley ◽  
Lorne J Fisher ◽  
Vernon G MacKay

Abstract A quantitative method is described for the determination of formaldehyde in milk by packed-column gas chromatography and electron capture detection. Aldehyde derivatization was carried out in situ with 2,4-dinitrophenyIhydrazine followed by extraction and analysis using an external standard. Average recoveries of 96.3 ± 1.6% were characteristic of the chromatographic method with an estimated detection limit of 0.026 mg/kg. The technique was applied to determination of formaldehyde in milk from cows consuming a formalin-treated feedstuff.

1971 ◽  
Vol 54 (3) ◽  
pp. 711-712
Author(s):  
Martha Fuzesi

Abstract A gas chromatographic method is described for the quantitative determination of N-butyl-N-ethyl-α,α,α-trifluoro-2,6-dinitro-p-tolindine and α,α,α-trifluoro-2,6-dinitro-N,N-dipropyI-p-toluidine herbicides in formulations. The sample is extracted with benzene, and equal amounts of sample and reference solution in the same concentration range are analyzed by gas chromatography, using an electron capture detector and an SE-30/Diatoport S column. The method has been applied successfully to laboratory-prepared and commercial samples.


1991 ◽  
Vol 74 (5) ◽  
pp. 830-835 ◽  
Author(s):  
Dalia M Gilvydis ◽  
Stephen M Walters

Abstract An interlaboratory study of the determination of captan, folpet, and captafol in tomatoes, cucumbers, and apples was conducted by 4 laboratories using wide-bore capillary column gas chromatography with electron capture detection. The 3 fungicides were determined using the Luke et al. multlresidue method modified to Include additional solvent elutlon in the optional Florisll column cleanup step used with this method. The crops were fortified with each fungicide at 3 levels per crop. Mean recoveries ranged from 86.2% for a 25.1 ppm level of captan in apples to 115.4% for a 0.288 ppm level of captafol In apples. Interlaboratory coefficients of variation ranged from 3.4% (24.7 ppm folpet) to 9.7% (0.243 ppm captafol) for tomatoes; from 2.8% (2.0 ppm captafol) to 8.2% (24.8 ppm captan) for cucumbers; and from 1.5% (0.234 ppm folpet) to 22.1% (0.266 ppm captafol) for apples.


1992 ◽  
Vol 75 (6) ◽  
pp. 1049-1053 ◽  
Author(s):  
Tord E Möller ◽  
Håkan F Gustavsson

Abstract A quantitative method has been developed for determination of nonmacrocyclic trichothecenes in cereals. The mycotoxins are extracted with acetonitrile- ethyl acetate-water, and the extracts are quickly defatted with hexane and purified on a Sep- Pak Florisil cartridge. The trichothecenes are then silylated with Tri-Sil/TBT and quantitated by capillary gas chromatography with electron capture detection. High recoveries of 13 tested trichothecenes were achieved in experiments on wheat at the 250 μg/kg level. The method was also tested on barley, maize, oats, and rye with good results


1982 ◽  
Vol 28 (10) ◽  
pp. 2100-2102 ◽  
Author(s):  
J F Nash ◽  
R J Bopp ◽  
R H Carmichael ◽  
K Z Farid ◽  
L Lemberger

Abstract This gas-chromatographic method for assay of fluoxetine and norfluoxetine in human plasma involves extraction of the drugs and use of a 63Ni electron-capture detector. The linear range of detection is 25 to 800 micrograms/L for each drug. Overall precision (CV) in the concentration range of 10 to 100 micrograms/L for both drugs was approximately 10%. Accuracy (relative error) in the same concentration range was approximately +10%. None of the commonly prescribed antidepressants or tranquilizers that we tested interfere with the assay.


1986 ◽  
Vol 69 (5) ◽  
pp. 899-901 ◽  
Author(s):  
George M Ware ◽  
Octave J Francis ◽  
Allen S Carman ◽  
Shia S Kuan ◽  
◽  
...  

Abstract Ten laboratories participated in a collaborative study of a method for the determination of deoxynivalenol in wheat by gas chromatography with electron capture detection. Each laboratory analyzed 6 samples in duplicate. Each collaborator received samples spiked at the 100.3, 501.3, and 1002.6 ng/g levels; a control sample; and 2 naturally contaminated samples. The average recovery (outliers excluded) for the spiked samples was 92.2%. The mean repeatability and reproducibility, respectively, were 32.2 and 41.3% for the spiked samples and 30.9 and 47.6% for the naturally contaminated samples. The method was adopted official first action.


2007 ◽  
Vol 90 (2) ◽  
pp. 544-549 ◽  
Author(s):  
Nuria Vela ◽  
Gabriel Prez ◽  
Gins Navarro ◽  
Simn Navarro

Abstract A method for the simultaneous determination of 9 pesticides (dinitroanilines, organophosphorus, triazoles, and pyrimidines) in several products (malt, spent grains, wort, and beer) of the beer industry is reported. Solid samples (malt and spent grains) are extracted by homogenization with a waterhexane mixture, and the pesticides are partitioned with dichloromethane. Liquid samples (wort and beer) are extracted by sonication with a hexanedichloromethane mixture. Determination of pesticide residues was made by capillary gas chromatography with an electron capture detector (ECD). Confirmation of the compounds was performed by gas chromatography/ion trap mass spectrometry in the selected ion monitoring mode. Detection limits for GCECD varied from 0.2 to 5.5 pg for trifluralin and malathion, respectively. Recoveries of the pesticides from spiked samples ranged from 81.2 to 113.7% with a relative standard deviation between 3.47.5%. The method presents good linearity over the studied range (0.0052 g/mL). The proposed method is rapid and reliable and can be useful for routine monitoring during brewing.


1969 ◽  
Vol 52 (4) ◽  
pp. 824-831 ◽  
Author(s):  
M E Getzendaner

Abstract Methods are described for determining residues of Dalapon in four types of substrates: fresh plant tissues, dry plant tissues not containing oil, dry plant tissues containing oil, and body fluids. After aqueous extraction and partition into diethyl ether, Dalapon is determined by gas chromatography using electron capture detection. Recovery from 22 different substrates averaged 90%. An average of 88% of Dalapon added to 11 crops and stored from 1.5 to 7 years was recovered.


1984 ◽  
Vol 67 (4) ◽  
pp. 731-734 ◽  
Author(s):  
George M Ware ◽  
Allen Carman ◽  
Octave Francis ◽  
Shia Kuan

Abstract A method is described for the determination of deoxynivalenol (DON) in wheat. The method involves sample extraction with chloroformethanol (8 + 2), column chromatographic cleanup on silica gel of small particle size, and derivatization with heptafluorobutyric acid anhydride using 4-dimethyIaminopyridine as a catalyst. The derivative DON trisheptafluorobutyrate is determined by gas chromatography using an electron capture detector. Recoveries of DON added to wheat at levels of 118—1184 ng/g averaged 88% with a coefficient of variation of 8.6%.


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