3, 4-DCA (3, 4-dichloroaniline), an intermediate of carbamate- and amide-herbicides such as swep and propanil, is a substance which is hard to decompose thermally. That has been detected in metabolites or decomposed products of selective herbicides in plants and soil. These herbicides or 3, 4-DCA, once ingested into the human body, are excreted mainly in urine.
This study was one which attempted to establish the method of quantitative analysis of 3, 4- DCA in urine by using gas chromatograph with an electron capture detector.
1) The determination procedure : One to two ml of concentrated hydrochloric acid was added to 50 ml of urine for adjusting the sample to pH 1. After being hydrolysed at 60°C for 20 min, the sample was adjusted to pH 8 by addition of ammonium hydroxide. And then, 10 ml of benzene was added to it and the mixture was shaken well for 5 min and centrifuged at 3, 000rpm for 5 min. After separation of solvent, an aliquot portion of the benzene phase was directly injected for the determination of 3, 4-DCA into a Shimadzu GC-4 BPE gas chromatograph. The packings of the columns (1.0 m×3 mm i.d.) were 2% OV-17, 5% DC-11 and 20% Apiezon L treated with 10% potassium hydroxide on Chromosorb W, AW, DMCS.
2) When the concentration of 3, 4-DCA in urine was 5 μg/ml, the average recovery rate was 91% with the coefficient of variation of 1.7%. The detection limit of the method was 0.1 μg 3, 4-DCA per 1 ml of urine
3) The gas chromatographic method (GC-method) for 3, 4-DCA determination from urine was compared with the ultraviolet absorption spectroscopic method (UV-method). The analytical results of the GC-method were nearly the same as that of the UV-method.
The method is simple and accurate, since the concentration and clean up of the sample were not necessary in this method. It was supposed that the UV-method is to be used for routine work in a factory laboratory and the GC-method for cross check of analytical results and investigation of metabolism of 3, 4-DCA.
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