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Development of extraction phase material restricted to microextraction packed sorbent drug in plasma samples and analysis by liquid chromatography coupled to mass spectrometry sequence

Grant number: 13/03808-9
Support Opportunities:Scholarships in Brazil - Doctorate
Effective date (Start): June 01, 2013
Effective date (End): January 31, 2017
Field of knowledge:Physical Sciences and Mathematics - Chemistry - Analytical Chemistry
Principal Investigator:Maria Eugênia Queiroz Nassur
Grantee:Mônia Aparecida Lemos Pinto de Melo
Host Institution: Faculdade de Filosofia, Ciências e Letras de Ribeirão Preto (FFCLRP). Universidade de São Paulo (USP). Ribeirão Preto , SP, Brazil


Schizophrenia is considered the most serious of neuropsychiatric disorders. Besides antipsychotics, most patients with schizophrenia also use other classes of drugs such as antidepressants, anticonvulsants, and anxiolytics, to lessen the symptoms associated with the disease. Therefore, analyzing drugs in plasma samples from schizophrenic patients is important to adjust doses, minimize adverse effects, and check the adherence of the patient the therapy. In recent years, liquid chromatography coupled to mass spectrometry sequential electrospray ionization (ESI) (LC-MS/MS) has become the reference analytical technique to analyze drugs in biological fluids. A sample preparation step is required when developing chromatographic methods, to remove interferences and pre-concentrate the target drugs, which are often present in trace levels in biological samples. Microextraction packed sorbent (MEPS), a receatly developed, consists in a miniaturized sample preparation technique, the system comprised of a solid phase extraction (SPE) standard, that employs reduced volumes of sample and solvent (eluent) from microliters to milliliters. The MEPS integrates the extraction and concentration of the solute in one step and allows one to introduce the extracted of solute into the chromatographic system using the same device employed in the extraction. This procedure avoids loss of solute and shortens the analysis time. The stationary phases of restricted access material (RAM) combine the principles of size exclusion chromatography and reverse phase, because its hydrophilic surface prevents adsorption of macromolecules present in the biological sample onto the stationary phase, while its hydrophobic properties help retain small molecules (drugs). In this project, a microcolumn extraction phase consisting of RAM will be developed for use with the MEPS technique. The method MEPS / LC-MS / MS has been standardized and validated to analyze drugs in the plasma of schizophrenic patients, for therapeutic drug monitoring.Keywords: Schizophrenia, drugs, biological fluids, microextraction packed sorbent (MEPS), restricted access material (RAM), liquid chromatography coupled to mass spectrometry sequence (LC-MS / MS).

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Scientific publications
(References retrieved automatically from Web of Science and SciELO through information on FAPESP grants and their corresponding numbers as mentioned in the publications by the authors)
PINTO, MANIA A. L.; DE SOUZA, ISRAEL D.; MIRANDA, LUIS FELIPPE C.; QUEIROZ, MARIA EUGENIA C.. A New Molecularly Imprinted Polymer for In-Tube SPME/UHPLC-MS/MS of Anandamide in Plasma Samples. Journal of the Brazilian Chemical Society, v. N/A, p. 9-pg., . (13/03808-9, 15/07619-1, 17/02147-0, 20/00126-8, 19/19485-0)
LEMOS PINTO, MONIA AP.; DE SOUZA, ISRAEL D.; QUEIROZ, MARIA EUGENIA C.. Determination of drugs in plasma samples by disposable pipette extraction with C18-BSA phase and liquid chromatography-tandem mass spectrometry. Journal of Pharmaceutical and Biomedical Analysis, v. 139, p. 116-124, . (15/07619-1, 13/03808-9)
Academic Publications
(References retrieved automatically from State of São Paulo Research Institutions)
MELO, Mônia Aparecida Lemos Pinto de. Selective extractive phases for microextraction techniques for determination of drugs and an endocannabinoid in plasma samples by LC-MS/MS. 2017. Doctoral Thesis - Universidade de São Paulo (USP). Faculdade de Ciências Farmacêuticas de Ribeirão Preto (PCARP/BC) Ribeirão Preto.

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