Masami Matsui

Gas chromatographic determination of methylguanidine, guanidine and agmatine as their hexafluoroacetylacetonates

Abstract Seven derivatives each of methylguanidine, guanidine and agmatine have been prepared, and the specificity and volatility of their gas chromatographic detection have been studied. The hexafluoroacetylacetonates have been found to be the most specific for the three guanidines, and are highly sensitive to alkali flame ionization and electron-capture detections. These derivatives are also fairly resistant to hydrolysis occurring in the derivatization process.

Gas chromatographic separation of hydroxylated N-nitrosamines.

Derivatives of six hydroxylated N-nitrosamines were prepared by acylation, trifluoroacylation, trimethylsilylation and methylation, and the volatilities and sensitivities of these derivatives on gas chromatographic detection were compared. All six nitrosamines were successfully derivatized by either acylation or trimethylsilylation. The acylated derivatives were easy to prepare; in addition, acylation was more specific than trimethylsilylation for the reaction with hydroxyl groups in the molecule.

Study on Analysis of N-Nitroso compunds in The Environment. A Sample Preparation Method for Analysis of N-Nitrosodiethanolamine.

環境中のN-ニトロソ化合物は動物実験において発癌性があることが報告され, それらの化合物が環境中での存在する可能性について関心がもたれている。N-ニトロソジエタノールアミン (NDELA) はエタノールアミン類と亜硝酸との反応により生成され, 切削油, タバコ, および化粧品などの生活環境中ですでに見出されている。今回, 難揮発性NDELAの分析において, N-ニトロソアミンの蒸留/濃縮装置を用いて試料に対してNDELA5ppbレベルの分析可能な精製濃縮法について検討したので報告する。試料 (化粧品) 10gに0.5gのスルファミン酸アンモニウムを加えたものを減圧蒸留装置で, アセトン蒸留を100℃においてNDELAを試料中の他の化合物と分離し, 蒸留を1時間 (留出液約100ml) 行い, その留出液をとり, 濃縮ののち, GC-TEA分析のためにBSTFAでシリル化した。この方法は従来法よ迅速性や検出感度に優れているばかりでなく, 他の揮発性N-ニトロソ化合物の分析にも適用できる。