engleski

Gas chromatographic determination of triazine herbicides in human urine

A method was developed for quantitative analysis of triazine herbicides atrazine, simazine, prometryn, and ametryn, and atrazine metabolites deisopropylatrazine, deethylatrazine and deethyldeisopropylatrazine in human urine. Following a modification of the procedure described by Bradway and Moseman (1) triazine compounds were extracted with diethyl ether from 5-mL urine samples saturated with NaCl. The saturation of urine with NaCl efficiently retarded emulsion created during extraction. The ethereal extracts were evaporated under a stream of nitrogen to dryness and the dry residue was redissolved in n-hexane. The samples were analysed by capillary gas chromatography using either a BPX 35 [Phenyl(35%-diphenyl-65%-dimethylsiloxane)] or SPB-50 [Poly(50%-diphenyl-50%-dimethylsiloxane)] capillary column and a thermionic sensitive detector. In the investigated concentration range (41-1664 ng/mL), the extraction recoveries of triazine compounds did not depend on the initial concentration in urine. The recoveries of atrazine and simazine were almost quantitative while those of prometryn and ametryn were about 30% lower. There was a considerable difference in atrazine metabolites extraction recoveries: deethylatrazine and deethyldeisopropylatrazine were recovered twice as efficiently as deisopropylatrazine. Additional extraction of urine with ethyl acetate did not increase the extraction recoveries of polar metabolites. With regard to the differences in the extraction recovery, the sensitivity of the method ranged from 30 ng/mL for deethyldeisopropylatrazine to 10 ng/mL for the most efficiently recovered atrazine and simazine. The influence of the urine pH value on the extraction recoveries was checked for atrazine. Atrazine was extracted most efficiently from urine of natural pH value (5.53-6.97). 1. D. E. Bradway, R. F. Moseman, J. Agric. Food Chem., 30 (1982) 224

atrazine; simazine; prometryn; ametryn; atrazine metabolites; extraction from urine

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