A preliminary report on the derivatization-gas chromatographic determination of nalidixic acid and 3,7-dicarboxynalidixic acid in urine.
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 CNA with tetradecyldimethylbenzylammonium 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 CNA 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.
Wu
S M
SM
Chen
S H
SH
Wu
H L
HL
D055598:Chemical Phenomena; D002621:Chemistry; D002849:Chromatography, Gas / Q000379:methods; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D009268:Nalidixic Acid / Q000031:analogs & derivatives* / Q000652:urine*; D012015:Reference Standards
C025188:7-carboxynalidixic acid; D009268:Nalidixic Acid