Development and validation of a sensitive LC-MS/MS method for the determination of para-aminosalicylic acid in different tissues in rats

Abstract

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 0.05μg/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.

Key words: tuberculosis, PAS, HPLC-ESI-MS/MS, tissue distribution

CLC Number:

R965.2

YUAN Yawen, LI Yan, YANG Jin. Development and validation of a sensitive LC-MS/MS method for the determination of para-aminosalicylic acid in different tissues in rats[J]. Chinese Journal of Clinical Pharmacology and Therapeutics, 2017, 22(3): 272-280.

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