Liquid Chromatography-Tandem Mass Spectrometry Method for Detection and Quantification of Meloxicam and 5′-Carboxymeloxicam in Oral Fluid Samples
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...
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| Format: | Article |
| Language: | English |
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MDPI AG
2023-06-01
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| Series: | Metabolites |
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| Online Access: | https://www.mdpi.com/2218-1989/13/6/755 |
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| author | 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 |
| author_facet | 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 |
| author_sort | Gabriela Moraes Oliveira |
| collection | DOAJ |
| description | 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, <i>v</i>/<i>v</i>) 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 E<sub>2</sub> (PGE<sub>2</sub>) 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 PGE<sub>2</sub> in oral fluid samples using LC-MS/MS. |
| first_indexed | 2024-03-11T02:10:45Z |
| format | Article |
| id | doaj.art-c064c77f7e944cd08ec92cf5b79e1ac3 |
| institution | Directory Open Access Journal |
| issn | 2218-1989 |
| language | English |
| last_indexed | 2024-03-11T02:10:45Z |
| publishDate | 2023-06-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Metabolites |
| spelling | doaj.art-c064c77f7e944cd08ec92cf5b79e1ac32023-11-18T11:35:14ZengMDPI AGMetabolites2218-19892023-06-0113675510.3390/metabo13060755Liquid Chromatography-Tandem Mass Spectrometry Method for Detection and Quantification of Meloxicam and 5′-Carboxymeloxicam in Oral Fluid SamplesGabriela Moraes Oliveira0Thiago José Dionísio1Viviane Silva Siqueira-Sandrin2Leticia Alves de Lima Ferrari3Bella Luna Colombini-Ishikiriama4Flávio Augusto Cardoso Faria5Carlos Ferreira Santos6Adriana Maria Calvo7Hospital for Rehabilitation of Craniofacial Anomalies, University of São Paulo (HRAC/USP), Bauru 17012-900, SP, BrazilDepartment of Biological Sciences, Bauru School of Dentistry, University of São Paulo, Bauru 17012-901, SP, BrazilDepartment of Biological Sciences, Bauru School of Dentistry, University of São Paulo, Bauru 17012-901, SP, BrazilDepartment of Biological Sciences, Bauru School of Dentistry, University of São Paulo, Bauru 17012-901, SP, BrazilDepartment of Biological Sciences, Bauru School of Dentistry, University of São Paulo, Bauru 17012-901, SP, BrazilDepartment of Biological Sciences, Bauru School of Dentistry, University of São Paulo, Bauru 17012-901, SP, BrazilHospital for Rehabilitation of Craniofacial Anomalies, University of São Paulo (HRAC/USP), Bauru 17012-900, SP, BrazilDepartment of Biological Sciences, Bauru School of Dentistry, University of São Paulo, Bauru 17012-901, SP, BrazilA 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, <i>v</i>/<i>v</i>) 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 E<sub>2</sub> (PGE<sub>2</sub>) 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 PGE<sub>2</sub> in oral fluid samples using LC-MS/MS.https://www.mdpi.com/2218-1989/13/6/755meloxicam5′-carboxymeloxicammass spectrometryoral fluid |
| spellingShingle | 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 Liquid Chromatography-Tandem Mass Spectrometry Method for Detection and Quantification of Meloxicam and 5′-Carboxymeloxicam in Oral Fluid Samples Metabolites meloxicam 5′-carboxymeloxicam mass spectrometry oral fluid |
| title | Liquid Chromatography-Tandem Mass Spectrometry Method for Detection and Quantification of Meloxicam and 5′-Carboxymeloxicam in Oral Fluid Samples |
| title_full | Liquid Chromatography-Tandem Mass Spectrometry Method for Detection and Quantification of Meloxicam and 5′-Carboxymeloxicam in Oral Fluid Samples |
| title_fullStr | Liquid Chromatography-Tandem Mass Spectrometry Method for Detection and Quantification of Meloxicam and 5′-Carboxymeloxicam in Oral Fluid Samples |
| title_full_unstemmed | Liquid Chromatography-Tandem Mass Spectrometry Method for Detection and Quantification of Meloxicam and 5′-Carboxymeloxicam in Oral Fluid Samples |
| title_short | Liquid Chromatography-Tandem Mass Spectrometry Method for Detection and Quantification of Meloxicam and 5′-Carboxymeloxicam in Oral Fluid Samples |
| title_sort | liquid chromatography tandem mass spectrometry method for detection and quantification of meloxicam and 5 carboxymeloxicam in oral fluid samples |
| topic | meloxicam 5′-carboxymeloxicam mass spectrometry oral fluid |
| url | https://www.mdpi.com/2218-1989/13/6/755 |
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