化学
色谱法
甲酸铵
蛋白质沉淀
选择性反应监测
代谢物
电喷雾电离
微透析
质谱法
分析物
电喷雾
液相色谱-质谱法中的离子抑制
串联质谱法
生物化学
细胞外
作者
Duygu Yeniceli,Erol Şener,Orhan Tansel Korkmaz,Dilek Doğrukol-Ak,Neşe Tunçel
出处
期刊:Talanta
[Elsevier]
日期:2011-03-15
卷期号:84 (1): 19-26
被引量:32
标识
DOI:10.1016/j.talanta.2010.11.063
摘要
A specific and highly sensitive liquid chromatography–electrospray mass spectrometry (LC–ESI-MS) method for the direct determination of bupropion (BUP) and its main metabolite hydroxybupropion (HBUP) in rat plasma and brain microdialysate has been developed and validated. The analysis was performed on a Bonus RP C18 (100 mm × 2.1 mm i.d., 3.5 μm particles) column using gradient elution with the mobile phase consisting of acetonitrile and ammonium formate buffer (10 mM, pH 4). Plasma samples were analyzed after a simple, one-step protein precipitation clean-up with trichloroacetic acid (TCA), however clean-up for microdialysis samples was not necessary, enabling direct injection of the samples into the LC–ESI-MS system. Signals of the compounds were monitored under the multiple reaction monitoring (MRM) mode of the LC–ESI-MS (ion trap) for quantification. The precursor to product ion transitions of m/z 240–184 and m/z 256–238 were used to measure BUP and HBUP, respectively. The method was validated in both plasma and microdialysate samples, and the obtained lower limit of quantification (LLOQ) was 1.5 ng mL−1 for BUP and HBUP in both matrices. The intra- and inter-day assay variability was less than 15% for both analytes. This LC–ESI-MS method provided simple sampling, rapid clean-up and short analysis time (<9 min), applicable to the routine therapeutic monitoring and pharmacokinetic studies of BUP and HBUP.
科研通智能强力驱动
Strongly Powered by AbleSci AI