Diquat (I) and paraquat (II) were analyzed by gas chromatography of their perhydrogenated products (III and IV) obtained by their treatment with NaBH
4 and NiCl
2. The system of NaBH
4-NiCl
2 was the most effective to obtain III and IV in the reduction of I and II with NaBH
4-transition metal salt. The reduction products were resolved by a gas chromatograph equipped with a hydrogen flame ionization detector and a 2m×3mm i.d. glass column packed with 5% KOH plus 5% PEG 20 M on Gas-chrom Z at 175°, with N
2 flow rate of 30 ml/min. This procedure is well suited for the assay of 10-90 μg/ml concentration of I and II (internal standard : p-anisidine) and is very useful for routine work because the reduction takes only a short time, without a troublesome apparatus by the use of NaBH
4 and NiCl
2 which are relatively safe to handle. The reduction products of I and II were identified as a mixture of trans-and cis-perhydrodipyrido [1, 2-a : 2', 1'-c] pyrazine (III) and 1, 1'-dimethyl-4, 4'-bipiperidine (IV) by gas chromatography-mass spectrometry and elemental analysis, as in the case of catalytic reduction using Pt
2O.
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