化学
体内分布
药代动力学
色谱法
甲酸
选择性反应监测
质谱法
电喷雾电离
检出限
高效液相色谱法
药理学
液相色谱-质谱法
串联质谱法
分析化学(期刊)
生物化学
体外
医学
作者
Jeferson Ziebarth,Camila Diedrich,Christiane Schineider Machado,Rubiana Mara Mainardes
标识
DOI:10.1016/j.jchromb.2024.124015
摘要
We present an ultra-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for simultaneous detection of insulin degludec (I-Deg) and liraglutide (LIRA) in rat plasma and tissues, characterized by its sensitivity and selectivity. Chromatographic separation was achieved using an Acquity UPLC BEH C18 column, leveraging a mobile phase of acetonitrile and water (both with 0.1 % formic acid) under gradient elution over a run time of 7.5 min. The mass spectrometer operated in positive electrospray ionization multiple reaction monitoring (MRM) mode, tracking transitions of m/z 1221.6 → 641.6 for I-Deg, m/z 938.7 → 1064.1 for LIRA, and m/z 1184.7 → 454.4 for the internal standard. Validation ranged from 5 to 100 ng/mL, exhibiting robust linearity (r2 > 0.99) and limits of detection (LOD) of 1.63–2.02 ng/mL for I-Deg and 0.96–1.62 ng/mL for LIRA. Limits of quantification (LOQ) were 2.38–4.76 ng/mL for I-Deg and 3.22–4.40 ng/mL for LIRA. Notably, no significant matrix effects were detected. Stability was confirmed under various conditions, and precision metrics (intraday RSD 1.68–8.05 % for I-Deg and 1.11–7.69 % for LIRA; interday RSD 1.39–8.61 % for I-Deg and 1.06–8.83 % for LIRA) alongside accuracy (90.5–114.9 % for I-Deg and 92.7–113.7 % for LIRA) were within acceptable ranges. The method was successfully applied to pharmacokinetic and biodistribution studies following simultaneous subcutaneous administration of LIRA and I-Deg in rats.
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