中国临床药理学与治疗学2017，Vol.22Issue(3)：272-280,9.
LC-MS/MS法测定对氨基水杨酸浓度及在大鼠组织分布研究中的应用
Development and validation of a sensitive LC-MS/MS method for the determination of para-aminosalicylic acid in different tissues in rats
摘要
Abstract
AIM:To develop a novel HPLC-ESI-MS/MS method to determine P-aminosalicylic acid (PAS) in different rat tissues to overcome the weaknesses of the conventional complicated pretreatment process and its low sensitivity.METHODS:The assay was performed with a one-step pre-column process of protein precipitation for extraction and the use of a Phenomenex Synergi 4u Polar-RP 80A (150 mm × 4.6 mm;4 μm) column with gradient elution for separation.Chlorzoxazone was selected as an internal standard (IS).LC-MS/MS (API4000) was applied for determination.PAS and IS were detected by tandem mass spectrometer using multiple reaction monitoring mode (MRM) with negative electrospray ionization.The ion transitions recorded in multiple reaction monitoring mode were m/z 152.0→108.1 for PAS and m/z 167.9→ 131.9 for the internal standard.RESULTS:The total analytical run time was short of 6.5 min.Calibration curve was linear over the range of 0.05-50 μg/mL and the lower limit of quantification (LLOQ) was low up to 0.05 μg/ mL.All validation criteria were fulfilled in compliance with the guidelines of the United States Food and Drug Administration (FDA).CONCLUSION:This HPLC-MS/MS method is accurate and reliable.The described assay method has been successfully applied for the measurement of PAS in preclinical distribution study.关键词
结核病/对氨基水杨酸/HPLC-ESI-MS/MS/组织分布Key words
tuberculosis/PAS/HPLC-ESI-MS/MS/tissue distribution分类
医药卫生引用本文复制引用
袁雅文,李岩,杨劲..LC-MS/MS法测定对氨基水杨酸浓度及在大鼠组织分布研究中的应用[J].中国临床药理学与治疗学,2017,22(3):272-280,9.基金项目
国家自然科学基金资助项目(81460570) （81460570）
