Avaliação da presença de aminas estimulantes, diureticas e anorexigenas em suplementos alimentares empregando eletroforese capilar

Detalhes bibliográficos
Autor(a) principal: Lapinski, Jéssica
Data de Publicação: 2021
Tipo de documento: Dissertação
Idioma: por
Título da fonte: Manancial - Repositório Digital da UFSM
dARK ID: ark:/26339/0013000014dvc
Texto Completo: http://repositorio.ufsm.br/handle/1/21257
Resumo: The consumption of dietary supplements has been increasing in recent years, due to its easy acquisition in both physical stores and websites. It is demonstrated mainly by the billionaire income of the global market involving dietary supplements. Thus, new products are launched frequently and increasingly appealing as to their rapid effectiveness related to fat burning and weight loss. It leads to an alarming scenario in relation to the safety of these products, since fraud and adulteration in the formulations are quite recurrent. In this context, the National Health Surveillance Agency (Anvisa) published a few years ago the regulatory framework for dietary supplements in order to standardize, regularize and narrow the gaps in the legalization of these products. Thus, it is necessary to have fast, sensitive and selective analytical methods for investigating the most probable mixtures of drugs as potential adulterants. This work proposed the development of an analytical method employing capillary electrophoresis with UV and C4D detection based on the micellar electrokinetic chromatography (MEKC) technique for the study and determination of 10 drugs (caffeine, synephrine, yohimbine, fenproporex, amfepramone topiramate, sibutramine, hydrochlorothiazide, furosemide and amiloride). From selectivity criteria, the method was validated for 5 drugs studied in the initial hypothetical mixture (caffeine, synephrine, yohimbine, hydrochlorothiazide and femproporex). The method was applied in the study of 20 samples of dietary supplements marketed in Brazil using the following optimized analytical conditions: working electrolyte phosphate buffer 50 mmol L-1 (pH 9.6) containing 20% acetonitrile (v/v) and sodium dodecyl sulfate (SDS) 50 mmol L-1, separation potential -15 kV, temperature 25 °C, hydrodynamic injection by gravity at 20 cm for 50 s. The method was validated according to the parameters of linearity, limit of detection, limit of quantification, precision and accuracy. In the studied samples, it was possible to detect that 20% of the samples contained hydrochlorothiazide as a diuretic drug and 5% had a caffeine concentration above that considered acceptable doses. Of the 5 drugs validated in the method by MEKC, caffeine, synephrine, hydrochlorothiazide and yohimbine were detected and quantified in the studied samples. The method proved to be effective in identifying stimulants, diuretics and anorectic as adulterants present in dietary supplements with good selectivity and detection sensitivity.
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spelling Avaliação da presença de aminas estimulantes, diureticas e anorexigenas em suplementos alimentares empregando eletroforese capilarEvaluation of the presence of stimulant, diuretic and anorexic amines in dietary supplements by capillary electrophoresisSuplementos alimentaresEletroforese capilarMEKCAdulteraçãoFood supplementsCapillary electrophoresisAdulterationCNPQ::CIENCIAS DA SAUDE::FARMACIAThe consumption of dietary supplements has been increasing in recent years, due to its easy acquisition in both physical stores and websites. It is demonstrated mainly by the billionaire income of the global market involving dietary supplements. Thus, new products are launched frequently and increasingly appealing as to their rapid effectiveness related to fat burning and weight loss. It leads to an alarming scenario in relation to the safety of these products, since fraud and adulteration in the formulations are quite recurrent. In this context, the National Health Surveillance Agency (Anvisa) published a few years ago the regulatory framework for dietary supplements in order to standardize, regularize and narrow the gaps in the legalization of these products. Thus, it is necessary to have fast, sensitive and selective analytical methods for investigating the most probable mixtures of drugs as potential adulterants. This work proposed the development of an analytical method employing capillary electrophoresis with UV and C4D detection based on the micellar electrokinetic chromatography (MEKC) technique for the study and determination of 10 drugs (caffeine, synephrine, yohimbine, fenproporex, amfepramone topiramate, sibutramine, hydrochlorothiazide, furosemide and amiloride). From selectivity criteria, the method was validated for 5 drugs studied in the initial hypothetical mixture (caffeine, synephrine, yohimbine, hydrochlorothiazide and femproporex). The method was applied in the study of 20 samples of dietary supplements marketed in Brazil using the following optimized analytical conditions: working electrolyte phosphate buffer 50 mmol L-1 (pH 9.6) containing 20% acetonitrile (v/v) and sodium dodecyl sulfate (SDS) 50 mmol L-1, separation potential -15 kV, temperature 25 °C, hydrodynamic injection by gravity at 20 cm for 50 s. The method was validated according to the parameters of linearity, limit of detection, limit of quantification, precision and accuracy. In the studied samples, it was possible to detect that 20% of the samples contained hydrochlorothiazide as a diuretic drug and 5% had a caffeine concentration above that considered acceptable doses. Of the 5 drugs validated in the method by MEKC, caffeine, synephrine, hydrochlorothiazide and yohimbine were detected and quantified in the studied samples. The method proved to be effective in identifying stimulants, diuretics and anorectic as adulterants present in dietary supplements with good selectivity and detection sensitivity.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESO consumo de suplementos alimentares vem aumentando nos últimos anos, fato ligado à sua fácil aquisição tanto em lojas físicas quanto em websites. O que nos mostra isso são os faturamentos bilionários do mercado global de suplementos alimentares. Assim, novos produtos são lançados com frequência e cada vez mais apelativos quanto a sua rápida eficácia relacionada à queima de gordura e perda de peso, o que leva a um cenário alarmante em relação à segurança destes produtos, visto que as fraudes e adulterações nas formulações são bastante recorrentes. Neste contexto, a Agência Nacional de Vigilância Sanitária (Anvisa) publicou há poucos anos o marco regulatório dos suplementos alimentares com o objetivo de padronizar, regularizar e estreitar as lacunas existentes na legalização destes produtos. Diante disto, faz-se necessário a existência de métodos analíticos rápidos, sensíveis e seletivos de análise de misturas prováveis de fármacos como potenciais adulterantes. Este trabalho propôs o desenvolvimento de um método analítico empregando eletroforese capilar com detecção UV e C4D baseado na técnica de cromatografia eletrocinética micelar (MEKC) para o estudo e a determinação de 10 fármacos (cafeína, sinefrina, ioimbina, femproporex, anfepramona topiramato, sibutramina, hidroclorotiazida, furosemida e amilorida). Por critérios de seletividade, foi realizada a validação do método para 5 fármacos estudados na mistura hipotética inicial (cafeína, sinefrina, ioimbina, hidroclorotiazida e femproporex). O método foi aplicado no estudo de 20 amostras de suplementos alimentares comercializados no Brasil nas condições analíticas otimizadas: eletrólito de trabalho tampão fosfato 50 mmol L-1 (pH 9,6) contendo acetonitrila 20% (v/v) e dodecil sulfato de sódio (SDS) 50 mmol L-1, potencial de separação -15 kV, temperatura 25°C, injeção hidrodinâmica por gravidade em 20 cm durante 50 s. O método foi validado de acordo com os parâmetros de linearidade, limite de detecção, limite de quantificação, precisão e exatidão. Nas amostras estudadas, foi possível detectar que 20 % das amostras continham a hidroclorotiazida como fármaco diurético e 5% apresentavam uma concentração de cafeína acima da considerada aceitável e sem declaração prévia. Dos 5 fármacos validados no método por MEKC, cafeína, sinefrina, hidroclorotiazida e ioimbina foram detectados e quantificados nas amostras estudadas. O método se mostrou eficaz na identificação de estimulantes, diuréticos e anorexígenos como adulterantes presentes em suplementos alimentares com boa seletividade e sensibilidade de detecção.Universidade Federal de Santa MariaBrasilFarmáciaUFSMPrograma de Pós-Graduação em Ciências FarmacêuticasCentro de Ciências da SaúdeCarvalho, Leandro Machado dehttp://lattes.cnpq.br/6652387343920028Bairros, André Valle deTavares, Idylla SilvaLapinski, Jéssica2021-06-29T18:13:02Z2021-06-29T18:13:02Z2021-01-26info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisapplication/pdfhttp://repositorio.ufsm.br/handle/1/21257ark:/26339/0013000014dvcporAttribution-NonCommercial-NoDerivatives 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-nd/4.0/info:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSM2022-10-06T17:25:26Zoai:repositorio.ufsm.br:1/21257Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2022-10-06T17:25:26Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false
dc.title.none.fl_str_mv Avaliação da presença de aminas estimulantes, diureticas e anorexigenas em suplementos alimentares empregando eletroforese capilar
Evaluation of the presence of stimulant, diuretic and anorexic amines in dietary supplements by capillary electrophoresis
title Avaliação da presença de aminas estimulantes, diureticas e anorexigenas em suplementos alimentares empregando eletroforese capilar
spellingShingle Avaliação da presença de aminas estimulantes, diureticas e anorexigenas em suplementos alimentares empregando eletroforese capilar
Lapinski, Jéssica
Suplementos alimentares
Eletroforese capilar
MEKC
Adulteração
Food supplements
Capillary electrophoresis
Adulteration
CNPQ::CIENCIAS DA SAUDE::FARMACIA
title_short Avaliação da presença de aminas estimulantes, diureticas e anorexigenas em suplementos alimentares empregando eletroforese capilar
title_full Avaliação da presença de aminas estimulantes, diureticas e anorexigenas em suplementos alimentares empregando eletroforese capilar
title_fullStr Avaliação da presença de aminas estimulantes, diureticas e anorexigenas em suplementos alimentares empregando eletroforese capilar
title_full_unstemmed Avaliação da presença de aminas estimulantes, diureticas e anorexigenas em suplementos alimentares empregando eletroforese capilar
title_sort Avaliação da presença de aminas estimulantes, diureticas e anorexigenas em suplementos alimentares empregando eletroforese capilar
author Lapinski, Jéssica
author_facet Lapinski, Jéssica
author_role author
dc.contributor.none.fl_str_mv Carvalho, Leandro Machado de
http://lattes.cnpq.br/6652387343920028
Bairros, André Valle de
Tavares, Idylla Silva
dc.contributor.author.fl_str_mv Lapinski, Jéssica
dc.subject.por.fl_str_mv Suplementos alimentares
Eletroforese capilar
MEKC
Adulteração
Food supplements
Capillary electrophoresis
Adulteration
CNPQ::CIENCIAS DA SAUDE::FARMACIA
topic Suplementos alimentares
Eletroforese capilar
MEKC
Adulteração
Food supplements
Capillary electrophoresis
Adulteration
CNPQ::CIENCIAS DA SAUDE::FARMACIA
description The consumption of dietary supplements has been increasing in recent years, due to its easy acquisition in both physical stores and websites. It is demonstrated mainly by the billionaire income of the global market involving dietary supplements. Thus, new products are launched frequently and increasingly appealing as to their rapid effectiveness related to fat burning and weight loss. It leads to an alarming scenario in relation to the safety of these products, since fraud and adulteration in the formulations are quite recurrent. In this context, the National Health Surveillance Agency (Anvisa) published a few years ago the regulatory framework for dietary supplements in order to standardize, regularize and narrow the gaps in the legalization of these products. Thus, it is necessary to have fast, sensitive and selective analytical methods for investigating the most probable mixtures of drugs as potential adulterants. This work proposed the development of an analytical method employing capillary electrophoresis with UV and C4D detection based on the micellar electrokinetic chromatography (MEKC) technique for the study and determination of 10 drugs (caffeine, synephrine, yohimbine, fenproporex, amfepramone topiramate, sibutramine, hydrochlorothiazide, furosemide and amiloride). From selectivity criteria, the method was validated for 5 drugs studied in the initial hypothetical mixture (caffeine, synephrine, yohimbine, hydrochlorothiazide and femproporex). The method was applied in the study of 20 samples of dietary supplements marketed in Brazil using the following optimized analytical conditions: working electrolyte phosphate buffer 50 mmol L-1 (pH 9.6) containing 20% acetonitrile (v/v) and sodium dodecyl sulfate (SDS) 50 mmol L-1, separation potential -15 kV, temperature 25 °C, hydrodynamic injection by gravity at 20 cm for 50 s. The method was validated according to the parameters of linearity, limit of detection, limit of quantification, precision and accuracy. In the studied samples, it was possible to detect that 20% of the samples contained hydrochlorothiazide as a diuretic drug and 5% had a caffeine concentration above that considered acceptable doses. Of the 5 drugs validated in the method by MEKC, caffeine, synephrine, hydrochlorothiazide and yohimbine were detected and quantified in the studied samples. The method proved to be effective in identifying stimulants, diuretics and anorectic as adulterants present in dietary supplements with good selectivity and detection sensitivity.
publishDate 2021
dc.date.none.fl_str_mv 2021-06-29T18:13:02Z
2021-06-29T18:13:02Z
2021-01-26
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
dc.type.driver.fl_str_mv info:eu-repo/semantics/masterThesis
format masterThesis
status_str publishedVersion
dc.identifier.uri.fl_str_mv http://repositorio.ufsm.br/handle/1/21257
dc.identifier.dark.fl_str_mv ark:/26339/0013000014dvc
url http://repositorio.ufsm.br/handle/1/21257
identifier_str_mv ark:/26339/0013000014dvc
dc.language.iso.fl_str_mv por
language por
dc.rights.driver.fl_str_mv Attribution-NonCommercial-NoDerivatives 4.0 International
http://creativecommons.org/licenses/by-nc-nd/4.0/
info:eu-repo/semantics/openAccess
rights_invalid_str_mv Attribution-NonCommercial-NoDerivatives 4.0 International
http://creativecommons.org/licenses/by-nc-nd/4.0/
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
dc.publisher.none.fl_str_mv Universidade Federal de Santa Maria
Brasil
Farmácia
UFSM
Programa de Pós-Graduação em Ciências Farmacêuticas
Centro de Ciências da Saúde
publisher.none.fl_str_mv Universidade Federal de Santa Maria
Brasil
Farmácia
UFSM
Programa de Pós-Graduação em Ciências Farmacêuticas
Centro de Ciências da Saúde
dc.source.none.fl_str_mv reponame:Manancial - Repositório Digital da UFSM
instname:Universidade Federal de Santa Maria (UFSM)
instacron:UFSM
instname_str Universidade Federal de Santa Maria (UFSM)
instacron_str UFSM
institution UFSM
reponame_str Manancial - Repositório Digital da UFSM
collection Manancial - Repositório Digital da UFSM
repository.name.fl_str_mv Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)
repository.mail.fl_str_mv atendimento.sib@ufsm.br||tedebc@gmail.com
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