A preliminary Report on the Derivatization-Gas Chromatographic Determination of Nalidixic Acid and 3, 7 - Dicarboxynalidixic Acid in Urine

衍生化氣相層析法分析尿液中 Nalidixic Acid 及3,7 - Dicarboxynalidixic Acid 之基本研究

吳秀梅(Shou-Men Wu) ； 陳素惠(Su-Hwei Chen) ； 吳信隆(Hsin-Lung Wu)

《The Kaohsiung Journal of Medical Sciences》 5卷11期 (1989/11) Pp. 630-636

https://doi.org/10.6452/KJMS.198911.0630

摘要

以衍生化氣相層析法，針對尿液中添加之尿道抗菌劑 nalidixic acid (NA) 及其代謝物3,7-dicarboxynalidixic acid (CAN) 之分析，進行基本探討。本法利用tetradecyldimethylbenzylammonium chloride為相間轉移催化劑，於鹼性尿液中與解離之NA或CAN形成離子對，而轉移至有機層methyl isobutyl ketone (MIBK)，再與MIBK中所含之衍生試劑pentafluouobenzyl bromide 進行衍生反應，所得有機層之衍生物，經1.5% OV-101氣相層析管分離後，以氫燄離子化型偵探器(flame-ionization detector)進行分析。本報告詳細探討影響衍生之各項因素，包括適當相間轉移催化劑及有機溶煤之選擇，水層之適當酸鹼度，衍生試劑之使用量，反應所需之時間及溫度等。

並列摘要

A preliminary study on the gas chromatographic analysis of urine spiked with nalidixic acid and 3,7-dicarboxynalidixic acid is described. The method is based on the transfer of an ion-pair of NA or CAN with tertradecyldimethylbenzylammonium chloride (benzalkonium chloride) from alkaline aqueous solution into methyl isobutyl ketone (MIBK), the organic phase, where these salts are derivatized with pentafluorobenzyl bromide. The derivatives formed by this process are chromatographed on an analytical column packed with 1.5% OV-101 and detected with a flame-ionization detector. Several parameters affecting the transfer and/or derivatization of NA or CAN were investigated. These parameters include the phase transfer catalyst employed, the organic solvent used, the concentration of the acid and base added, the amount of derivatizing agent required, and reaction time and temperature.

並列關鍵字

nalidixic acid ； 3,7 - dicarboxynalidixic acid ； derivatization-GC