薬物の裁判化学的研究(第3報)除草剤DiquatならびにParaquatの水素化ホウ素ナトリウム・遷移金属塩(塩化ニッケル)系還元成績体のガスクロマトグラフィー

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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.
公益社団法人日本薬学会の論文
1977-02-28