Gas-Liquid Chromatographic Determination of Technical Chlordane Residues in Food Crops: Interpretation of Analytical Data

1975 ◽  
Vol 58 (5) ◽  
pp. 1051-1061
Author(s):  
William P Cochrane ◽  
James F Lawrence ◽  
Young W Lee ◽  
Ronald B Maybury ◽  
Brian P Wilson
Keyword(s):  
Field Experiments ◽  
Stationary Phases ◽  
Analytical Data ◽  
Chromatographic Determination ◽  
Electron Capture Detection ◽  
Food Crops ◽  
Liquid Chromatographic Determination ◽  
Consistent Method ◽  
Liquid Chromatographic

Abstract An interlaboratory investigation of technical chlordane residues in food crops was carried out to determine the most practical and consistent method of reporting results. Using a technical chlordane reference standard, 8 gas chromatographic stationary phases were studied for their resolution capabilities. The best separations were obtained with SE-30 and its OV-1 equivalent. Using these columns and electron capture detection, potatoes and carrots from supervised field experiments were analyzed in duplicate and quantitated by using 4 methods of calculation. The data were statistically treated to determine the precision and bias for each method. Also, 1 sample was analyzed in duplicate on 2 different occasions by 6 laboratories to substantiate the initial conclusions. Based on the criterion of high precision it is suggested that a comparison of total area under the chromatogram of the sample with total area of a standard technical chlordane be the method of quantitation. Only peaks which are common to both standard and sample have any significance in this type of calculation.

Gas-Liquid Chromatographic Determination of Chloramphenicol in Agricultural Crops

1976 ◽  
Vol 59 (5) ◽  
pp. 1118-1121
Author(s):  
Kumiko Sasaki ◽  
Mitsuharu Takeda ◽  
Mitsuru Uchiyama
Keyword(s):  
Silicic Acid Column ◽  
Stationary Phases ◽  
Chromatographic Determination ◽  
Electron Capture Detection ◽  
Gas Liquid Chromatography ◽  
Agricultural Crops ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Unpolished Rice

Abstract A method is presented for the gas-liquid chromatographic determination of chloramphenicol in agricultural crops. Chloramphenicol is extracted with ethyl acetate, cleaned up by silicic acid column chromatography, acetylated with acetic anhydride and pyridine, and then measured by gas-liquid chromatography with electron capture detection. Two stationary phases, DEGS + phosphoric acid and Reoplex 400, were used. The sensitivity was ca 8 ng (40% full scale deflection). The efficiency of the analytical method was evaluated by analyzing crops fortified with chloramphenicol. The average recovery ranged from 72% in unpolished rice to 86% in Chinese radishes.

Gas-Liquid Chromatographic Determination of Total Inorganic Iodine in Milk

1977 ◽  
Vol 60 (6) ◽  
pp. 1307-1309 ◽  
Author(s):  
Hendrik J Bakker
Keyword(s):  
Liquid Chromatography ◽  
Iodine Content ◽  
Chromatographic Determination ◽  
Electron Capture Detection ◽  
Gas Liquid Chromatography ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Inorganic Iodine ◽  
Liquid Chromatographic

Abstract Total inorganic iodine in milk is determined by conversion to iodobutanone, which is quantitated by gas-liquid chromatography and electron capture detection. As little as 10 μg/L can be determined. The thyroid-active iodine content of milk can be determined rapidly with a relative standard deviation of 1.9%. Average recoveries for added iodide and iodine were 95.5 and 94.6%, respectively.

Gas-Liquid Chromatographic Determination of Diflubenzuron (Dimilin) in Water as Its Trifluoroacetyl Derivative

1977 ◽  
Vol 60 (1) ◽  
pp. 213-217
Author(s):  
Brian L Worobey ◽  
G R Barrie Webster
Keyword(s):  
Organic Matter ◽  
Particulate Organic Matter ◽  
Pond Water ◽  
Chromatographic Determination ◽  
Electron Capture Detection ◽  
Florisil Column ◽  
Freundlich Equation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A new gas-liquid chromatographic (GLC) procedure has been developed for the analysis of diflubenzuron, 1-(4-chlorophenyl)-3-(2,6-difluorobenzoyl) urea, in pond water. The residues from fortified pond water were extracted with ethyl acetate, derivatized, and cleaned up on a mini Florisil column. The diflubenzuron was determined by GLC as its N,N′-di(trifluoroacetyl) derivative, using electron capture detection. A 50% full scale deflection was obtained with 0.03 ng injected. Recoveries from fortified unfiltered pond water were 65.7, 72.8, 82.0, and 90.8% at the 0.020, 0.059, 0.197, and 0.788 mg/L (ppm) levels, respectively. Recoveries from fortified filtered pond water were 94.1 and 89.3% at the 0.020 and 0.060 mg/L levels, respectively. It is postulated that diflubenzuron is immobilized by adsorption, for example, to particulate organic matter in the pond water because recovery data from unfiltered water followed the linear form of the Freundlich equation.

Gas-Liquid Chromatographic Determination of 3-Trifluormethyl-4-nitrophenol Residues in Fish

1974 ◽  
Vol 57 (2) ◽  
pp. 387-388 ◽  
Author(s):  
John L Allen ◽  
Joe B Sills
Keyword(s):  
Aqueous Solution ◽  
Chromatographic Determination ◽  
Electron Capture Detection ◽  
Gas Liquid Chromatography ◽  
Fish Tissues ◽  
Fish Muscles ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Extracting Solvent

Abstract A procedure for the determination of 3-trifluormethyl-4-nitrophenol (TFM) in fish tissues is described. Homogenized tissues are extracted with hexane-ethyl ether; the extract is cleaned up by partitioning the TFM from the extracting solvent into 0.1N NaOH, acidifying the aqueous solution, and partitioning again with hexaneethyl ether. The TFM is methylated with diazomethane and analyzed by gas-liquid chromatography, using electron capture detection. Recoveries ranged from 75 to 100% from fish muscles that were spiked with 0.01—2.00 μg TFM/g.

Simultaneous Gas-Liquid Chromatographic Determination of Four Sulfonamides in Feeds

1971 ◽  
Vol 54 (6) ◽  
pp. 1277-1282 ◽  
Author(s):  
Robert J Daun
Keyword(s):  
Liquid Chromatography ◽  
Electron Capture ◽  
Chromatographic Determination ◽  
Electron Capture Detection ◽  
Gas Liquid Chromatography ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A procedure is described for the gas-liquid chromatographic determination of sulfathiazole, sulfamerazine, sulfamethazine, and sulfaquinoxaline in finished feeds at levels from 0.002 to 0.05%. The procedure utilizes a double derivatization technique to modify the sulfonamides so that they can be determined by gas-liquid chromatography with electron capture detection. The conditions for extraction, derivatization, and gas-liquid chromatography are given, along with recovery data.

Gas-Liquid Chromatographic Determination of α-Cyano-3-phenoxybenzyl α-Isopropyl-4-chlorophenylacetate Residues in Cabbage

1977 ◽  
Vol 60 (4) ◽  
pp. 908-910
Author(s):  
Narayan S Talekar
Keyword(s):  
Chromatographic Determination ◽  
Electron Capture Detection ◽  
Liquid Chromatographic Method ◽  
Steel Column ◽  
Stainless Steel Column ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Ppm Level

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.

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