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芳香族α-酮酸的O-三甲基甲硅烷基喹喔啉醇衍生物。质谱和定量气相色谱法。

O-trimethylsilylquinoxalinol derivatives of aromatic alpha-keto acids. Mass spectra and quantitative gas chromatography.

作者信息

Langenbeck U, Mench-Hoinowski A, Dieckmann K P, Möhring H U, Petersen M

出版信息

J Chromatogr. 1978 Mar 1;145(2):185-93.

PMID:649713
Abstract

As an extension of earlier work on aliphatic alpha-keto acids, a method is described for the quantitative gas chromatographic determination of urinary aromatic alpha-keto acids. The keto acids are derivatized with o-phenylenediamine to yield the quinoxalinols. These compounds are chromatographed after trimethylsilylation. The aromatic keto acids are stabilized by sodium dithionite (4 mg/ml urine) and storage below 0 degrees. The final derivatives are stable for weeks at room temperature. Low resolution mass spectra are reported. The fragmentation mechanisms are elucidated by analysis of O-trimethylsilyl-(TMS)-quinoxalinois, O-(TMS-d9)-quinoxalinois and O-TMS-6(7)-chloroquinoxalinois.

摘要

作为早期关于脂肪族α-酮酸研究工作的拓展,本文描述了一种用于定量气相色谱测定尿中芳香族α-酮酸的方法。酮酸用邻苯二胺衍生化以生成喹喔啉醇。这些化合物在三甲基硅烷化后进行色谱分析。芳香族酮酸通过连二亚硫酸钠(4毫克/毫升尿液)稳定化,并在0摄氏度以下储存。最终衍生物在室温下可稳定数周。报道了低分辨率质谱。通过对O-三甲基硅基-(TMS)-喹喔啉醇、O-(TMS-d9)-喹喔啉醇和O-TMS-6(7)-氯喹喔啉醇的分析阐明了裂解机制。

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