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使用氘代内标物通过气相色谱 - 质谱联用仪测定小鼠尿液中的1 - 氨基环丙烷羧酸

Gas chromatographic-mass spectrometric determination of urinary 1-aminocyclopropanecarboxylic acid in mice using a deuterated internal standard.

作者信息

Howell S E, Miller S R, McCallister J D, Cherkofsky S C, Patrick K S

机构信息

Department of Pharmaceutical Sciences, Medical University of South Carolina, Charleston 29425-2303, USA.

出版信息

J Chromatogr B Biomed Appl. 1995 Jan 6;663(1):148-52. doi: 10.1016/0378-4347(94)00416-3.

Abstract

A gas chromatographic-mass spectrometric method is described for the determination of 1-aminocyclopropanecarboxylic acid in mouse urine using the 2,2,3,3-[2H4] isotopolog as an internal standard. Samples (0.1 ml) were extracted using an exchange resin, then derivatized with pentafluoropropanol and pentafluoropropionic anhydride at 100 degrees C for 25 min. Gas chromatography was performed on a (5% phenyl)methylpolysiloxane column and detection was by selected-ion monitoring of M-CO2CH2CF2CF3 fragment ions. The method provided high response linearity (mean r = 0.999) and precision (< 5% coefficient of variation). After orally dosing mice with 1-aminocyclopropanecarboxylic acid (300 mg/kg), 46 and 10% of the dose was excreted unchanged in the 0-24 h and 24-48 h urines, respectively.

摘要

描述了一种气相色谱 - 质谱法,以2,2,3,3 - [2H4]同位素异构体为内标物测定小鼠尿液中的1 - 氨基环丙烷羧酸。取0.1 ml样品,用离子交换树脂萃取,然后在100℃下用五氟丙醇和五氟丙酸酐衍生化25分钟。在(5%苯基)甲基聚硅氧烷柱上进行气相色谱分析,通过对M - CO2CH2CF2CF3碎片离子的选择离子监测进行检测。该方法具有高响应线性(平均r = 0.999)和精密度(变异系数<5%)。给小鼠口服1 - 氨基环丙烷羧酸(300 mg/kg)后,分别有46%和10%的剂量在0 - 24小时和24 - 48小时的尿液中以原形排出。

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