Determination of Nicarbazin by Gas Liquid_Chromatography

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Abstract
Nicarbazin (NCZ) is an equimolar complex of 4, 4-dinitrocarbanilide (DNC) and 2-hydroxy-4, 6-dimethylpyrimidine. Gas chromatographic determination with an electron capture detector (ECD) was carried out for p-nitroaniline (NA) obtained by acid hydrolysis of NCZ in a liquid paraffin bath at 150°C for 15 minutes. NA, a reaction product, was extracted with ethyl acetate in the presence of supersaturated sodium chloride in alkaline solution and the NA was determined by gas liquid chromatography. Gas chromatography: A Shimadzu GC 4CMPFE gas chromatograph with an ECD was used for NA. The column consisted of a glass tube (1mm×3mm ID) packed with 5% Thermon 3000 on Chromosorb W (AW DMCS, 80-100 mesh) and conditioned at 190°C. The temperature of the bath detector and injector was 230°C and the flow rate of nitrogen carrier gas was 20ml/min. A sample was extracted with methanol in an electric blender. The extract was cleaned up by ion exchange column chromatography on Amberlite CG-400 (OH form). The eluent was a mixture of hydrochloric acid and methanol (2:98). The recoveries of NCZ added to chicken tissues and eggs were in the range of 85-97%. The minimum detectable concentration was 0.02ppm as NCZ.

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