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Determination of volatile salivary biomarkers using solid-phase microextraction and GC-MS

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Resumo:This study proposes a solid-phase microextraction (SPME) approach that allows the extraction of target cancer biomarkers directly from saliva with minor pretreatments. Saliva is an exocrine body fluid originated in the oral cavity that contains some of the biomarkers found in blood or serum and is easily accessible [1,2]. The biomarkers present in saliva – deoxyribonucleic acid (DNA), ribonucleic acid (RNA), proteins, other metabolites (organic compounds, lipids, etc), microbiota – are valuable for health-related analyses, including the prognosis and diagnosis of several diseases [2]. Due to this health-related importance, there is a need for simple, rapid, and highly sensitive methods to determine saliva biomarkers, allowing its use in clinical practice. SPME fulfills all mentioned requirements as it combines sampling, preconcentration, and extraction in one step [3]. In this work, several SPME fibers were used in a headspace (HS) mode to extract volatile salivary biomarkers from artificial saliva combined with GC-MS (Figure 1). The target analytes included several phenols, esters, and aldehydes, all related with different oral cavity related diseases or lung cancer. The extraction was performed with several commercial coatings (DVB/CAR/PDMS, PDMS/DVB, PDMS and CAR/PDMS), and a lab-made coating based on the CIM80 metal-organic framework (MOF) [4]. Optimization of the method using the best performing commercial fiber (CAR-PDMS) and the CIM-80 fiber was carried out using a Doehlert’s design. According to the results, the best extraction conditions – a compromise between the extraction efficiencies of all analytes – were 120 min and 50ºC for CAR/PDMS, and 38 min and 70ºC for CIM-80, followed by desorption at the GC injection port at 290ºC and 280 ºC during 5 min, respectively. The commercial fiber provided higher sensitivity than the CIM-80 fiber, while the latter allowed for adequate sensitivity and faster analysis.
Autores principais:Rosa, M. E.
Outros Autores:Negrín-Santamaría, I.; e Silva, F. A.; Trujillo-Rodríguez, M. J.; Freire, M. G.; Pino, V.
Assunto:Cancer biomarkers GC-MS Saliva SPME Volatile organic compounds
Ano:2022
País:Portugal
Tipo de documento:documento de conferência
Tipo de acesso:acesso aberto
Instituição associada:Universidade de Aveiro
Idioma:inglês
Origem:RIA - Repositório Institucional da Universidade de Aveiro
Descrição
Resumo:This study proposes a solid-phase microextraction (SPME) approach that allows the extraction of target cancer biomarkers directly from saliva with minor pretreatments. Saliva is an exocrine body fluid originated in the oral cavity that contains some of the biomarkers found in blood or serum and is easily accessible [1,2]. The biomarkers present in saliva – deoxyribonucleic acid (DNA), ribonucleic acid (RNA), proteins, other metabolites (organic compounds, lipids, etc), microbiota – are valuable for health-related analyses, including the prognosis and diagnosis of several diseases [2]. Due to this health-related importance, there is a need for simple, rapid, and highly sensitive methods to determine saliva biomarkers, allowing its use in clinical practice. SPME fulfills all mentioned requirements as it combines sampling, preconcentration, and extraction in one step [3]. In this work, several SPME fibers were used in a headspace (HS) mode to extract volatile salivary biomarkers from artificial saliva combined with GC-MS (Figure 1). The target analytes included several phenols, esters, and aldehydes, all related with different oral cavity related diseases or lung cancer. The extraction was performed with several commercial coatings (DVB/CAR/PDMS, PDMS/DVB, PDMS and CAR/PDMS), and a lab-made coating based on the CIM80 metal-organic framework (MOF) [4]. Optimization of the method using the best performing commercial fiber (CAR-PDMS) and the CIM-80 fiber was carried out using a Doehlert’s design. According to the results, the best extraction conditions – a compromise between the extraction efficiencies of all analytes – were 120 min and 50ºC for CAR/PDMS, and 38 min and 70ºC for CIM-80, followed by desorption at the GC injection port at 290ºC and 280 ºC during 5 min, respectively. The commercial fiber provided higher sensitivity than the CIM-80 fiber, while the latter allowed for adequate sensitivity and faster analysis.