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液质联用法测定犬吸入暴露后血浆中总布地奈德浓度。

Liquid chromatography tandem mass spectrometry determination of total budesonide levels in dog plasma after inhalation exposure.

机构信息

Finnish Food Safety Authority Evira, Chemistry and Toxicology Research Unit, Mustialankatu 3, 00790 Helsinki, Finland.

出版信息

Anal Bioanal Chem. 2012 Jan;402(3):1209-15. doi: 10.1007/s00216-011-5549-3. Epub 2011 Nov 20.

DOI:10.1007/s00216-011-5549-3
PMID:22101462
Abstract

A sensitive and selective method to quantify budesonide in dog plasma samples was developed and fully validated. Liquid-liquid extraction was followed by solid-phase extraction and liquid chromatography-tandem mass spectrometry with electrospray ionization. After reconstitution of the analytes in the mobile phase, samples were analysed by reversed-phase liquid chromatography with isocratic elution. d8-Budesonide was used as an internal standard, and characteristic transitions of d8-budesonide and budesonide were used for quantification. The method was validated with respect to selectivity, specificity, linearity, recovery, repeatability, reproducibility and limits of detection and quantification. The validated method was successfully applied to monitor the plasma levels of budesonide in dogs exposed to clinical doses of inhaled and intravenous drug.

摘要

建立并充分验证了一种灵敏、专属性强的定量分析犬血浆中布地奈德的方法。采用液-液萃取法和固相萃取法,结合液质联用技术(电喷雾离子源)进行样品前处理,以 d8-布地奈德为内标,采用反相高效液相色谱法进行分析,梯度洗脱。方法经过选择性、特异性、线性、回收率、精密度与重复性、检测限与定量限验证,成功应用于吸入和静脉给予临床剂量药物后犬血浆中布地奈德浓度的监测。

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