ガスクロマトグラフィーによる製剤中のDiisopropylamine Dichloroacetateの定量

概要

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Fundamental conditions were examined for the gas chromatographic determination of diisopropylamine dichloroacetate (DADA) by the method of nitrosation-extraction. To 10 ml. of the sample solution containing 1〜10 mg. of DADA, 2.5 ml. of glacial acetic acid and 5 ml. of 50% sodium nitrite solution are added, and the mixture is allowed to react for 5 minutes at 60°. When cooled, the solution is made alkaline with 7 ml. of 50% potassium hydroxide solution, and extracted with 10 ml. of cyclohexane containing 5 mg. of p-dibromo-benzene as an internal standard. The extracted solution is centrifuged, concentrated in a vacuum to 0.5〜1 ml., and injected at column temperature of 160° into the gas chromatograph with polyethylene glycol succinate (5%) on Celite 545 column. When N-nitrosodiisobutylamine is used as an internal standard, 10 ml. of 0.5% diisobutylamine hydrochloride solution is added to the sample solution, nitrosated, and extracted with 10 ml. of cyclohexane. The proposed method is reproducible and may be used for samples containing many other substances, such as biological fluids.
公益社団法人日本薬学会の論文
1966-09-25