Metabolites (Jun 2023)

Liquid Chromatography-Tandem Mass Spectrometry Method for Detection and Quantification of Meloxicam and 5′-Carboxymeloxicam in Oral Fluid Samples

  • Gabriela Moraes Oliveira,
  • Thiago José Dionísio,
  • Viviane Silva Siqueira-Sandrin,
  • Leticia Alves de Lima Ferrari,
  • Bella Luna Colombini-Ishikiriama,
  • Flávio Augusto Cardoso Faria,
  • Carlos Ferreira Santos,
  • Adriana Maria Calvo

DOI
https://doi.org/10.3390/metabo13060755
Journal volume & issue
Vol. 13, no. 6
p. 755

Abstract

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A sensitive, selective and particularly fast method of liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed and validated for the determination of meloxicam and its main metabolite, 5′-carboxymeloxicam, in oral fluid samples. Meloxicam and its major metabolite were separated using a Shim-Pack XR-ODS 75 L × 2.0 column and C18 pre-column at 40 °C using a mixture of methanol and 10 mM ammonium acetate (80:20, v/v) with an injection flow rate of 0.3 mL/min. The total time of the analytical run was 5 min. Sixteen volunteers had oral fluid samples collected sequentially before and after taking a meloxicam tablet (15 mg) for up to 96 h. With the concentrations obtained, the pharmacokinetic parameters were determined using the Phoenix WinNonlin software. The parameters evaluated for meloxicam and 5′-carboxymeloxicam in the oral fluid samples showed linearity, accuracy, precision, medium-quality control (MQC-78.12 ng/mL), high-quality control (HQC-156.25 ng/mL), lower limits of quantification (LLOQ-0.6103 ng/mL), low-quality control (LQC-2.44 ng/mL), stability and dilution. Prostaglandin E2 (PGE2) was also detected and quantified in the oral fluid samples, demonstrating the possibility of a pharmacokinetic/pharmacodynamic (PK/PD) study with this methodology. All the parameters evaluated in the validation of the methodology in the oral fluid samples proved to be stable and within the possible variations in each of the described parameters. Through the data presented, the possibility of a PK/PD study was demonstrated, detecting and quantifying meloxicam, its main metabolite and PGE2 in oral fluid samples using LC-MS/MS.

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