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用埃特拉路特(Extrelut)萃取后,通过气相色谱法和气相色谱-质谱联用仪同时测定尿液中的奥布卡因及其五种代谢物。

Oxybuprocaine and five metabolites simultaneously determined in urine by gas chromatography and gas chromatography-mass spectrometry after extraction with Extrelut.

作者信息

Kasuya F, Igarashi K, Fukui M

出版信息

Clin Chem. 1987 May;33(5):697-700.

PMID:3568356
Abstract

We describe a gas-liquid chromatographic (GC) method for determination of oxybuprocaine, and a gas chromatographic-mass spectrometric (GC-MS) method for simultaneous determination of four of its nine metabolites in urine. We used an Extrelut column to simply and rapidly extract oxybuprocaine and its metabolites from urine. For the GC-MS analyses, we monitored the characteristic fragment ions at m/z 353, 395, 369, 411, and 235 for 3-butoxy-4-aminobenzoic acid (metabolite 2, M-2), 3-butoxy-4-acetylaminobenzoic acid (M-3), 3-hydroxy-4-aminobenzoic acid (M-4), 3-hydroxy-4-acetylaminobenzoic acid (M-5), and methaqualone (internal standard), respectively. We quantified the glucuronide of M-2 after enzymic treatment. The assay's selectivity and reproducibility (within-day and between-day CVs less than 8% for all metabolites) make it applicable to determine oxybuprocaine and its metabolites in human urine. Mean 9-h urinary excretion of oxybuprocaine and its five metabolites from four healthy volunteers was 89.2% after a 100-mg oral dose.

摘要

我们描述了一种用于测定奥布卡因的气-液色谱(GC)方法,以及一种用于同时测定尿液中其九种代谢物中四种的气相色谱-质谱(GC-MS)方法。我们使用埃克斯特鲁特柱从尿液中简单快速地提取奥布卡因及其代谢物。对于GC-MS分析,我们分别监测了3-丁氧基-4-氨基苯甲酸(代谢物2,M-2)、3-丁氧基-4-乙酰氨基苯甲酸(M-3)、3-羟基-4-氨基苯甲酸(M-4)、3-羟基-4-乙酰氨基苯甲酸(M-5)和甲喹酮(内标)在m/z 353、395、369、411和235处的特征碎片离子。我们在酶处理后对M-2的葡萄糖醛酸苷进行了定量。该分析方法的选择性和重现性(所有代谢物的日内和日间变异系数均小于8%)使其适用于测定人尿液中的奥布卡因及其代谢物。四名健康志愿者口服100毫克剂量后,奥布卡因及其五种代谢物的平均9小时尿排泄率为89.2%。

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