Bioanalytical Department, Jubilant Generics Limited, Noida, India.
Eur J Mass Spectrom (Chichester). 2023 Aug;29(4):240-247. doi: 10.1177/14690667231194812. Epub 2023 Aug 15.
The aim of this paper was to develop, validate, and utilize a sensitive liquid chromatography-tandem mass spectrometry bioanalytical method for bioequivalence/clinical trial studies conducted in human plasma. To accomplish the target, a stable labeled internal standard, that is, dexamethasone D was used as an internal standard to track and compensate the parent compound during processing, and extraction from plasma. The method involves a rapid liquid-liquid phase extraction from plasma, followed by reverse phase chromatography, and mass spectrometry detection, with a total run time of 3.5 min. The method was developed and validated from 2 to 600 ng/ml for dexamethasone. The mean recovery for dexamethasone was found to be 81.0%. The validated method enabled the analysis of dexamethasone in samples from clinical pharmacokinetic studies. The peak concentration of dexamethasone ranged between 253 to 281 ng/ml and 319 to 343 ng/ml, respectively, in fasted and fed conditions. The terminal half-life values for dexamethasone ranged between 3.5 to 8.2 h and 3.0 to 7.5 h, respectively.
本文旨在开发、验证和应用一种灵敏的液相色谱-串联质谱生物分析方法，用于在人血浆中进行生物等效性/临床试验研究。为了实现这一目标，使用了一种稳定标记的内标物，即地塞米松 D，作为内标物来跟踪和补偿处理过程中以及从血浆中提取时的母体化合物。该方法涉及从血浆中进行快速液-液萃取，随后进行反相色谱和质谱检测，总运行时间为 3.5 分钟。该方法是从 2 至 600ng/ml 的地塞米松进行开发和验证的。地塞米松的平均回收率为 81.0%。验证后的方法可用于分析临床药代动力学研究中的地塞米松样品。地塞米松的峰浓度分别在禁食和进食条件下在 253 至 281ng/ml 和 319 至 343ng/ml 之间变化。地塞米松的半衰期值分别在 3.5 至 8.2 小时和 3.0 至 7.5 小时之间变化。
