Data were acquired in Multiple Reaction Monitoring (MRM) mode with optimized conditions (ion optics and collision energy). Peak detection, integration and quantitative analysis were done using Mass Hunter Quantitative analysis software (Agilent Technologies) based on calibration lines built with commercially available eicosanoids standards (Cayman Chemicals). Calibration curves were calculated by the IS method using the area ratio between the analyte and the internal standard. Linear regression with a weight factor of 1/X was applied for each compound and the linearity and the accuracy of the detection were determined. Finally, the limit of detection (LOD) and the limit of quantification (LOQ) were defined for the compounds of interest.
"],"repository":["MetaboLights"],"study_status":["Public"],"ptm_modification":[""],"instrument_platform":["Liquid Chromatography MS - positive - HILIC"],"chromatography_protocol":["High performance liquid chromatography was performed using an Agilent 1290 Infinity equipped with an autosampler, a binary pump and a column oven. The analytical column was a ZorBAX SB-C18 column (2.1 mm, 50 mm, 1.8 μm) (Agilent Technologies) maintained at 40 °C. The mobile phases consisted of water, ACN and FA (75:25:0.1;v/v/v) (A) and ACN, FA (100:0.1, v/v) (B). The linear gradient was as follows: 0% B at 0 min, 85% B at 8.5 min, 100% B at 9.5 min, 100% B at 10.5 min and 0% B at 12 min. The flow rate was 0.35 mL/min. The autosampler was set at 5 °C and the injection volume was 5 μL.lease update this protocol description
"],"publication":["Adjunctive ibuprofen in pre-extensively drug-resistant and extensively drug-resistant tuberculosis: a Phase IIA open-label pilot clinical trial."],"submitter_name":["Emilie Layre","Cristina Vilaplana","Lilibeth Arias"],"submitter_affiliation":["CNRS","Institut Germans Trias i Pujol","Fundació Institut d'Investigació en Ciències de la Salut Germans Trias i Pujol"],"organism_part":["plasma","calibrant"],"technology_type":["mass spectrometry assay"],"extraction_protocol":["260 µL of cold methanol and 40 µL of internal standard (Deuterium labeled compounds) were added to 250 µL of samples. After centrifugation at 2000 g for 15 min at 4°C, supernatants were transferred into 2 mL 96-well deep plates and diluted in H2O to 2 mL. Samples were then submitted to solid phase extraction (SPE) using OASIS HLB 96-well plate (30 mg/well, Waters) pretreated with MeOH (1 mL) and equilibrated with 10% MeOH (1 mL). After sample application, extraction plate was washed with 10% MeOH (1 mL). After drying under aspiration, lipids mediators were eluted with 1 mL of MeOH. Prior to LC-MS/MS analysis, samples were evaporated under nitrogen gas and reconstituted in 10 µL on MeOH.
"],"disease":[""],"organism":["Homo sapiens"],"full_dataset_link":["https://www.ebi.ac.uk/metabolights/MTBLS13376"],"author":["Iza Jikia. National Center for Tuberculosis and Lung Diseases.","Ketevan Barbakadze.","Emilie Layre. Institut de Pharmacologie et de Biologie Structurale. emilie.layre@ipbs.fr.","Chiara Sopegno.","Kaori Fonseca. Fundació Institut d'Investigació en Ciències de la Salut Germans Trias i Pujol. kaorifonseca@gmail.com.","Zaza Avaliani.","Juan Garcia-Illarramendi.","Neil Martinson.","Judith Farres. Fundació Institut d'Investigació en Ciències de la Salut Germans Trias i Pujol. j.farres.marisch@gmail.com.","Nadiia Buhiichyk.","Jerome Nigou.","Malkhaz Tsotskhalashvili.","Nestani Tukvadze.","Lilibeth Arias. Fundació Institut d'Investigació en Ciències de la Salut Germans Trias i Pujol. larias@igtp.cat.","Sergo Vashakidze.","Kennedy Otwombe.","Cristina Vilaplana. Fundació Institut d'Investigació en Ciències de la Salut Germans Trias i Pujol. Crtra. de Can Ruti, Camà de les Escoles, s/n 08916, Badalona, Barcelona, Spain. cvilaplana@igtp.cat. 34930330527.","Albert Despuig.","Tamta Korinteli."],"data_transformation_protocol":["There was no transformation of the raw data
"],"study_factor":["Sample type","Etiology"],"sample_collection_protocol":["Samples were retrieved from the NSAIDS-XDRTB clinical trial (ClinicalTrials.gov NCT02781909), a phase IIA prospective, interventional, randomized (1:1), controlled, open-label, pilot trial to estimate the potential efficacy and safety of using adjunctive ibuprofen for the treatment of pre-XDR and XDR-TB . Peripheral whole blood samples were collected at baseline, and at months 2 and 6 of treatment. Plasma was isolated from whole blood collected in sodium citrate CPT tubes (BD Vacutainer® CPTTM). Samples were stored at -80 Celsius degrees until analysis.
"],"submitter_email":["larias@igtp.cat","cvilaplana@igtp.cat","emilie.layre@ipbs.fr"],"omics_type":["Metabolomics"],"study_design":["ESI-triple quadruple G6460 mass spectrometer (Agilent Technologies)","Extensively Drug Resistance Process","Tuberculosis","Clinical Trial","untargeted analysis","Ibuprofen","Patient","Homo sapiens","Agilent 1290 Infinity System","plasma","calibrant","experimental sample"],"curator_keywords":["ESI-triple quadruple G6460 mass spectrometer (Agilent Technologies)","Extensively Drug Resistance Process","Tuberculosis","Clinical Trial","untargeted analysis","Ibuprofen","Homo sapiens","Patient","Agilent 1290 Infinity System","plasma","calibrant","experimental sample"],"mass_spectrometry_protocol":["The samples were analyzed at the MetaToul lipidomic platform (I2MC, INSERM 1048, Toulouse, France). LC-MS/MS analyses of eicosanoids were performed as described (Cf ref). Briefly, lipid mediators were separated on a ZorBAX SB-C18 column (2.1 mm, 50 mm, 1.8 µm) (Agilent Technologies) using Agilent 1290 Infinity HPLC system (Technologies) coupled to an ESI-triple quadruple G6460 mass spectrometer (Agilent Technologies). Data were acquired in Multiple Reaction Monitoring (MRM) mode with optimized conditions (ion optics and collision energy).
Ref : LC-MS/MS method for rapid and concomitant quantification of pro-inflammatory and pro-resolving polyunsaturated fatty acid metabolites. Le Faouder P et al, J Chrom B, 2013, vol 932 p123-133
"],"additional_accession":[]},"is_claimable":false,"name":"Adjunctive ibuprofen in pre-extensively drug-resistant and extensively drug-resistant tuberculosis: a Phase IIA open-label pilot clinical trial","description":"Drug-resistant tuberculosis (TB) remains a major global health challenge. Host-directed therapies (HDTs) aim to limit tissue damage, shorten treatment, and improve outcomes by modulating immune responses. We evaluated the safety and potential efficacy of adjunctive ibuprofen an inexpensive, well-tolerated non-steroidal anti-inflammatory drug in pre-extensively drug-resistant (pre-XDR) and extensively drug-resistant (XDR)TB. In this prospective, open-label, randomized pilot study (NCT02781909) in Georgia, 28 adults with bacteriologically confirmed pulmonary pre-XDR or XDR-TB were randomized 1:1 to receive standard-of-care (SoC) alone (n=14) or SoC plus ibuprofen 400 mg daily for 2 months (n=14), with 6 months of follow-up. Primary endpoints were sputum culture conversion and radiological improvement. Secondary endpoints included WHO-defined outcomes, safety, health-related quality of life, and inflammatory markers. By month 2, culture negativity was achieved in 27% of controls and 9% of ibuprofen recipients, with median conversion time of 4 months in both groups. Radiological improvement was observed in 64% vs 54% at month 2, and in 90% of both groups by month 6. Final outcomes were comparable (71% cured), and adverse events did not differ. Ibuprofen was associated with reductions in inflammatory markers, including monocyte-to-lymphocyte ratio and interferon gamma. Adjunctive ibuprofen did not improve primary endpoints but showed immune-modulating activity with a favourable safety profile, supporting further investigation in larger studies.
","dates":{"publication":"2026-05-28","submission":"2025-11-24"},"accession":"MTBLS13376","cross_references":{}}