Determination of antibacterial agent tilmicosin in pig plasma by LC/MS/MS and its application to pharmacokinetics

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• 作者：Bing Li ; Shi-Yue Gong ; Xu-Zheng Zhou ; Ya-Jun Yang ; Jian-Yong Li ; Xiao-Juan Wei ; Fu-Sheng Cheng ; Jian-Rong Niu ; Xi-Wang Liu and Ji-Yu Zhang
• 刊名：Biomedical Chromatography
• 出版年：2017
• 出版时间：March 2017
• 年：2017
• 卷：31
• 期：3
• 全文大小：1084K
• ISSN：1099-0801

文摘

A rapid and sensitive high-performance liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed and validated to quantify tilmicosin in pig plasma. Plasma samples were prepared by liquid–liquid extraction. Chromatographic separation was achieved on a C₁₈ column (2.1 × 30 mm, 3.5 μm) using acetonitrile–water (90:10, v/v; water included 0.1% formic acid) as the mobile phase. Mass detection was carried out using positive electrospray ionization in multiple reaction monitoring mode. The calibration curve was linear from 0.5 to 2000 ng/mL (r² = 0.9998). The intra- and inter-day accuracy and precision were within the acceptable limits of ±10% for all tilmicosin concentrations. The recoveries ranged from 95 to 99% for the three tested concentrations. The LC–MS/MS method described herein was simple, fast and less laborious than other methods, achieved high sensitivity using a small sample volume, and was successfully applied to pharmacokinetic studies of tilmicosin enteric granules after oral delivery to pigs. In comparison with tilmicosin premix, tilmicosin enteric granules slowed the elimination rate of tilmicosin, prolonged its period of action and significantly improved its bioavailability.