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Development of a monolithic phase with amino groups and addition of nanoparticles for the determination of carbidopa, levodopa, Benserazide, dopamine and 3-O-methyldopa in plasma samples of patients with Parkinson's Disease by MEPS/HILIC-MS/MS

Grant number: 17/03726-3
Support Opportunities:Scholarships in Brazil - Master
Effective date (Start): June 01, 2017
Effective date (End): May 31, 2019
Field of knowledge:Physical Sciences and Mathematics - Chemistry - Analytical Chemistry
Acordo de Cooperação: Coordination of Improvement of Higher Education Personnel (CAPES)
Principal Investigator:Maria Eugênia Queiroz Nassur
Grantee:Caroline Fernandes Grecco
Host Institution: Faculdade de Filosofia, Ciências e Letras de Ribeirão Preto (FFCLRP). Universidade de São Paulo (USP). Ribeirão Preto , SP, Brazil


Parkinson's disease (PD) is an idiopathic neurodegenerative disease that affects approximately 3% of the population over 65 years old in Brazil. It can also reach individuals under 40 years old (Premature Parkinsonism). PD is caused by deficiency of the neurotransmitter, dopamine, in the nigrostriatal and cortical pathway, interfering in the motor system. Levodopa is a prodrug (decarboxylated by the aromatic amino acid decarboxylase in dopamine) which is the most effective in controlling the symptoms of PD. Levodopa (LD) has been associated with the peripheral dopa- decarboxylase inhibitor, such as carbidopa or benserazide, as it increases the availability of LD in the central nervous system and decreases the adverse effects of dopamine formed in the peripheral system. Prolonged use of LD leads to fluctuations in motor performance and dyskinesias, decreasing the efficacy of LD. Liquid chromatography coupled to tandem mass spectrometry (LC-MS / MS) has been considered the reference analytical technique to determine drugs in biological samples. Hydrophilic interaction liquid chromatography (HILIC) is an alternative mode of reverse phase LC-MS/MS to determine polar compounds. The sample preparation step has been required in the development of LC-MS/MS methods, in order to eliminate the endogenous compounds and to preconcentrate the drugs, often present at trace levels in biological samples. Microextraction by packaged sorbent (MEPS) is based on the miniaturization of the solid phase extraction technique (SPE), where the volumes of the biological sample and the solvent (eluent) were reduced from milliliters to microliters. In MEPS, a microcolumn with solid-packing sorbent is connected to the needle of a microsyringe, integrated into the microsyringe, as a plug with polyethylene filters on both sides. In this project, a fused silica capillary with silica hybrid monolithic phase with amine groups and nanoparticles will be developed and used as a needle of the MEPS technique. The MEPS/HILIC-MS/MS method will be developed and validated to determine carbidopa, levodopa, dopamine, 3-O-methyldopa and benserazide in plasma samples from patients with Parkinson's disease. Plasma concentrations of levodopa, 3-O-methyldopa, peripheral dopamine-decaboxylase inhibitors (carbidopa and benserazide) and dopamine will be determined in patients with Parkinson's disease undergoing prolonged treatment with levodopa / carbidopa or levodopa / benserazide with symptoms of motor fluctuations (wearing-off) and dyskinesias. This study could be help to define the appropriate dosage regimen. (AU)

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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)
GRECCO, CAROLINE FERNANDES; SOUZA, ISRAEL D.; COSTA QUEIROZ, MARIA EUGENIA. Recent development of chromatographic methods to determine parabens in breast milk samples: A review. JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES, v. 1093, p. 82-90, . (17/03726-3, 17/02147-0)
Academic Publications
(References retrieved automatically from State of São Paulo Research Institutions)
GRECCO, Caroline Fernandes. Development of a monolithic phase with amino groups and nanoparticles for the determination of carbidopa, levodopa, benserazide, dopamine and 3-O-methyldopa in plasma samples from patients with Parkinson\'s disease by HILIC-MS / MS in column switching mode. 2019. Master's Dissertation - Universidade de São Paulo (USP). Faculdade de Filosofia, Ciências e Letras de Ribeirão Preto (PCARP/BC) Ribeirão Preto.

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