Hignite C E, Tschanz C, Huffman D H, Azarnoff D L
Drug Metab Dispos. 1978 May-Jun;6(3):288-95.
An improved method for quantitating N-demethylantipyrine (N-DEM-AP) in urine by gas chromatography or gas chromatography-mass spectrometry has been developed. Recovery of greater than 90% of N-DEM-AP was achieved by extraction of the sample at pH 1 after addition of 3-amino-1-phenyl-2-pyrazolin-5-one. The coefficient of variation of replicate analyses was 8%. N-DEM-AP was excreted in the urine as a glucuronic acid conjugate. This conjugate was isolated from the urine of an individual receiving antipyrine and purified. The NMR and mass-spectral data are consistent with the conjugate being an O-glucuronide of N-DEM-AP in its enol form.
已开发出一种通过气相色谱法或气相色谱-质谱法对尿液中N-去甲基安替比林（N-DEM-AP）进行定量的改进方法。在加入3-氨基-1-苯基-2-吡唑啉-5-酮后，通过在pH 1下萃取样品，N-DEM-AP的回收率大于90%。重复分析的变异系数为8%。N-DEM-AP以葡萄糖醛酸共轭物的形式经尿液排出。该共轭物从接受安替比林的个体尿液中分离出来并进行了纯化。核磁共振和质谱数据与该共轭物为烯醇形式的N-DEM-AP的O-葡萄糖醛酸苷一致。
