Journal
MOLECULES
Volume 24, Issue 9, Pages -Publisher
MDPI
DOI: 10.3390/molecules24091658
Keywords
in-tube SPME-MS; MS; dual ligand organic-silica hybrid monolith capillary; amino acids; plasma samples
Funding
- FAPESP (Fundacao de Amparo a Pesquisa do Estado de Sao Paulo) [2017/02147-0]
- INCT-TM [465458/2014-9]
- CAPES (Coordenacao de Aperfeicoamento de Pessoal de Nivel Superior)
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This work describes the direct coupling of the in-tube solid-phase microextraction (in-tube SPME) technique to a tandem mass spectrometry system (MS/MS) to determine amino acids (AA) and neurotransmitters (NT) (alanine, serine, isoleucine, leucine, aspartic acid, glutamic acid, lysine, methionine, tyrosine, and tryptophan) in plasma samples from schizophrenic patients. An innovative organic-silica hybrid monolithic capillary with bifunctional groups (amino and cyano) was developed and evaluated as an extraction device for in-tube SPME. The morphological and structural aspects of the monolithic phase were evaluated by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), nitrogen sorption experiments, X-ray diffraction (XRD) analyses, and adsorption experiments. In-tube SPME-MS/MS conditions were established to remove matrix, enrich analytes (monolithic capillary) and improve the sensitivity of the MS/MS system. The proposed method was linear from 45 to 360 ng mL(-1) for alanine, from 15 to 300 ng mL(-1) for leucine and isoleucine, from 12 to 102 ng mL(-1) for methionine, from 10 to 102 ng mL(-1) for tyrosine, from 9 to 96 ng mL(-1) for tryptophan, from 12 to 210 ng mL(-1) for serine, from 12 to 90 ng mL(-1) for glutamic acid, from 12 to 102 ng mL(-1) for lysine, and from 6 to 36 ng mL(-1) for aspartic acid. The precision of intra-assays and inter-assays presented CV values ranged from 1.6% to 14.0%. The accuracy of intra-assays and inter-assays presented RSE values from -11.0% to 13.8%, with the exception of the lower limit of quantification (LLOQ) values. The in-tube SPME-MS/MS method was successfully applied to determine the target AA and NT in plasma samples from schizophrenic patients.
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