Gas Chromatographic Determination of N-Butyl-N-ethyl-α,α,α-trifluoro-2,6-dinitro-p-toluidine and α,α,α-Trifluoro-2,6-dinitro-N,N-dipropyl-p-toluidine in Formulations

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.

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.


1996 ◽  
Vol 79 (2) ◽  
pp. 587-588 ◽  
Author(s):  
Lan Zhao ◽  
De-Fang Fan

Abstract A gas chromatographic method is described for determination of chlorothalonil residues in leaves and roots of Scrophularia and in soil. Samples were extracted with acetone and cleaned up on a Florisil column. Chlorothalonil residues are chromatographed directly on a glass column of 1.5% OV-17 and 2% QF-1 coated on 80-100 mesh Chromosorb W (HP) support and measured with a 63Ni electron capture detector. Detection limits are 0.001 ppm for leaf, 0.005 ppm for root, and 0.001 ppm for soil.


1987 ◽  
Vol 70 (4) ◽  
pp. 745-748
Author(s):  
Uaz Ahmad

Abstract A capillary column gas chromatographic method is described for determining parts-per-trillion (ppt) levels of chlorsulfuron in agricultural runoff water. The water sample is acidified with acetic acid and extracted with methylene chloride. The chlorsulfuron in the extract is derivatized to its monomethyl derivative. After Florisil column cleanup, the methylated chlorsulfuron is determined by electron-capture gas chromatography. Recovery of chlorsulfuron from fortified water samples is greater than 80%. Detection limit of the method is 25 ng chlorsulfuron/L water (25 ppt). There are 2 reaction sites on the chlorsulfuron molecule, both of which are susceptible to methylation leading to monomethyl chlorsulfuron and dimethyl chlorsulfuron. A procedure is described to methylate selectively the sulfonamide nitrogen of chlorsulfuron.


1974 ◽  
Vol 20 (2) ◽  
pp. 249-254 ◽  
Author(s):  
M A Evenson ◽  
G L Lensmeyer

Abstract A rapid, simple, accurate, and precise isothermal gas-chromatographic method is introduced for determination of methaqualone (2-methyl-3-o-tolyl-4(3H)-quinazolinone) in serum. A single extraction of 2 ml of serum, without derivative formation, will give adequate sensitivity for quantitation of therapeutic serum concentrations of the drug within 15 min. The method is free of interferences from biological substances, as well as from commonly used drugs. A non-drug internal standard compensates for variables in extraction, injection, and instrumental changes during analysis. The coefficient of variation, day-to-day, is 5.6%. Mean recovery of added methaqualone was 80%. To compensate for the nonquantitative yield and ensure accurate results, we prepared all analytical methaqualone standards in serum.


1970 ◽  
Vol 53 (3) ◽  
pp. 566-568
Author(s):  
J E Paterson

Abstract A gas chromatographic method is described for the quantitative determination of dioxathion and chlorfenvinphos in emulsifiable concentrates and livestock dips. A convenient quantity of the emulsifiable formulation is dissolved in xylene and the aqueous dip is extracted with xylene for gas chromatographic analysis, using a mixed silicone oil stationary phase and a flame ionization detector. The coefficients of variation for the dioxathion and chlorfenvinphos determinations in the emulsifiable concentrate are 2.4 and 1.0%, respectively. Recoveries of the former from a fouled dip ranged from 97 to 103% and recoveries of the latter ranged from 92 to 97%.


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.


1975 ◽  
Vol 30 (11-12) ◽  
pp. 726-729 ◽  
Author(s):  
L Van Broekhoven ◽  
A Van Der Kerk ◽  
-Van Hoof ◽  
C Salemink

Abstract Using an electron capture detector, a sensitive gas chromatographic method has been developed for the determination of the juvenile hormone methyl(2E, 6E)-10, 11-epoxy-3,7,11-trimethyl-2,6-dodecadienoate (JH III) in insect material. The sensitivity in electron capture detection of the bisheptafluorobutyrate was determined. The work-up procedure was checked by adding known amounts of JH III to insect material. The method seems equally applicable to all three juvenile hormones.


1993 ◽  
Vol 76 (3) ◽  
pp. 650-656 ◽  
Author(s):  
Teodoro Crisippi ◽  
Guido Zini ◽  
Riccardo Fabbrini

Abstract A gas chromatographic method is described that is suitable for the determination of benalaxyl residues ranging from 10 to 0.1 μg/kg in several crops, must, wine, and water. The compound is extracted with acetone and purified either by partitioning between water and n-hexane or by passing the extract through an Extrelut column with n-hexane. Further purification is achieved by column chromatography on alumina. The active ingredient is finally determined by gas chromatography with nitrogenphosphorus detection. Mean recoveries were ≥95% in the various crops tested and in the 0.01-1.05 mg/kg fortification range. Standard deviations for each crop were ≤6.5%.


1974 ◽  
Vol 57 (1) ◽  
pp. 189-191
Author(s):  
James B Leary

Abstract A gas chromatographic method is described for determining acephate (O,S-dimethyl acetylphosphoramidothioate) and a metabolite, Ortho 9006 (O,S-dimethyl phosphoramidothioate), in a variety of crops. After extraction of the sample with ethyl acetate, the solvent is evaporated, and an ether solution of the residue is passed through a silica gel column to remove interferences. Acephate and Ortho 9006 are eluted from the column with 10% methanol in ether and measured simultaneously by programmed temperature gas chromatography, using an alkali flame ionization detector.


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