Determination of Type A and B Trichothecenes in Cereals by Gas Chromatography with Electron Capture Detection

1992 ◽  
Vol 75 (6) ◽  
pp. 1049-1053 ◽  
Author(s):  
Tord E Möller ◽  
Håkan F Gustavsson
Keyword(s):  
Gas Chromatography ◽  
Ethyl Acetate ◽  
Electron Capture ◽  
Capillary Gas Chromatography ◽  
Quantitative Method ◽  
Type A ◽  
Electron Capture Detection

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

Surrogate-Assisted Determination of 2,3,7,8-Tetrachlorodibenzo-p-Dioxin in Fish by Electron Capture Capillary Gas Chromatography

1986 ◽  
Vol 69 (6) ◽  
pp. 976-980
Author(s):  
Richard A Niemann
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Capillary Gas Chromatography ◽  
Capillary Column ◽  
Electron Capture Detection ◽  
Matrix Interference ◽  
Relative Standard ◽  
Tetrachlorodibenzo P Dioxin ◽  
Liquid Chromatographic

Abstract Surrogate spiking the sample with 1000 parts per trillion (pptr) 1,3,7,8-tetrachlorodibenzo-p-dioxin (1378-TCDD) has doubled analytical throughput in determining toxic 2378-TCDD (analyte) at the low partper- trillion level in fish, using multicolumn high resolution liquid chromatographic cleanup before quantitation by capillary gas chromatography with electron capture detection. The 1378- and 2378-TCDD were recovered equally and were well separated by the capillary column so that the earlier-eluting surrogate did not interfere with the quantitation of levels of analyte many-fold lower. Matrix interference contributed <1 % bias in surrogate quantitation. Using surrogate recovery to correct for analyte losses during analysis, accuracy averaged (n = 7) 105% in determining 18 or 45 pptr 2378-TCDD added to fish without detectable bioincurred analyte. Analyses of selected fish with bioincurred 2378-TCDD gave results comparable to earlier work where recovery correction required a second analysis of sample fortified with analyte. With surrogate fortification, repeatability of determination (n = 3 or 4) improved markedly to <5% relative standard deviation at 37-46 pptr.

scholarly journals Determination of Fluvalinate Residues in Beeswax by Gas Chromatography with Electron-Capture Detection

2000 ◽  
Vol 83 (5) ◽  
pp. 1225-1228 ◽  
Author(s):  
Angeliki Tsigouri ◽  
Urania Menkissoglu-Spiroudi ◽  
Andreas T Thrasyvoulou ◽  
Grigorios C Diamantidis
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Diethyl Ether ◽  
Capillary Gas Chromatography ◽  
Diatomaceous Earth ◽  
Accurate Method ◽  
Electron Capture Detection ◽  
Limit Of Determination ◽  
Coefficients Of Variation

Abstract A simple, rapid, and accurate method is described for the determination of residual fluvalinate in beeswax. The procedure consists of partitioning on a disposable column of diatomaceous earth (Extrelut®), followed by chromatographic cleanup on a Florisil cartridge. The final extract is analyzed by capillary gas chromatography with electron-capture detection (GC–ECD). Briefly, wax samples were dissolved in n-hexane, and the solutions were sonicated and transferred to Extrelut columns. The fluvalinate was extracted with acetonitrile, and a portion of the extract was cleaned up on a Florisil cartridge. The fluvalinate was eluted with diethyl ether–n-hexane (1 + 1) and directly determined by GC–ECD. Recoveries from wax samples spiked at 5 fortification levels (100–1500 μg/kg) ranged from 77.4 to 87.3%, with coefficients of variation of 5.12–8.31%. The overall recovery of the method was 81.4 ± 3.2%, and the limit of determination was 100 μg/kg.

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
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Quantitative Method ◽  
Chromatographic Method ◽  
Packed Column ◽  
Chromatographic Determination ◽  
Electron Capture Detection ◽  
External Standard

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.

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