Determinação cromatográfica e eletroforética de diuréticos e laxantes em formulações farmacêuticas a base de plantas medicinais

Detalhes bibliográficos
Autor(a) principal: Moreira, Ana Paula Lançanova
Data de Publicação: 2012
Tipo de documento: Dissertação
Idioma: por
Título da fonte: Manancial - Repositório Digital da UFSM
Texto Completo: http://repositorio.ufsm.br/handle/1/5914
Resumo: The use of herbal medicines as an alternative treatment has increased by the belief that natural products do not cause damage to health. However cases in which natural products are added of synthetic drugs not declared, presumably to enhance the effectiveness them have been reported in the literature. In the case of weight loss formulations the main adulterants found are appetite suppressants, antidepressants, benzodiazepines, diuretics and laxatives. The identification of these frauds is only possible by applying the analytical methods able to detect the presence of adulterants in the formulations. This paper describes the development of two methods employing separation techniques with electrochemical detection for the determination of diuretics and laxatives as adulterants in herbal products. The method employing capillary zone electrophoresis (CZE) with contactless conductivity detection (C4D) allows the simultaneous determination of amiloride, chlorthalidone, hydrochlorothiazide, furosemide and phenolphthalein in the following optimized conditions: working electrolyte phosphate buffer 20 mmol L-1 (pH 9.2) containing 30% methanol (v/v) separation potential -15 kV, temperature 25 °C, injection hydrodynamic by gravity in 20 cm for 60 seconds. The method employing ion pair chromatography (IPC) with pulsed amperometric detection (PAD) allows the determination of hydrochlorothiazide, chlorthalidone and furosemide on the following conditions: mobile phase phosphate buffer 5 mmol L-1 (pH 4.5) containing SDS 0.3 mmol L-1 and 50% methanol (v/v), sample potential of +0.8 V, the cleaning potential of -0.2 V and +1.0 V, and flow rate of 1.0 mL/min. Both methods were validated in the parameters of linearity, limit of detection limit of quantification, precision, accuracy and selectivity, and were applied in the analysis of 26 samples of natural weight loss products purchased from pharmacies in nine Brazilian states. In three of 26 samples were identified the presence of illegal diuretic hydrochlorothiazide in concentrations ranging from 0.6 to 7.0 mg/capsule. In addition, five other samples called naturals contained declared on the label of the packaging the presence of synthetic diuretics hydrochlorothiazide or furosemide. Both methods were able to identify the adulterants present in samples with high selectivity and sensitivity. Furthermore, they presented very approximate results in the concentration of adulterants found in the formulations. There is still no unified regulation established by the government for control of herbal products. Each country has its laws, but the marketing is global. Maybe this is the reason why the adulteration of natural products has been a recurring practice in various parts of the world. Therefore, effective regulation for the natural products can result in the reduction of these offenses, and punishment of offenders, thus ensuring the rights of consumers to make quality treatment, safe and effective, without prejudice to health. Keywords: Pharmaceutical formulations, adulterants, diuretics, laxatives, methods of separation, electrochemical detection.
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spelling Determinação cromatográfica e eletroforética de diuréticos e laxantes em formulações farmacêuticas a base de plantas medicinaisChromatographic and electrophoretic determination of diuretics and laxatives in herbal-based pharmaceutical formulationsFormulações farmacêuticasAdulterantesDiuréticosLaxantesMétodos de separaçãoDetecção eletroquímicaPharmaceutical formulationsAdulterantsDiureticsLaxativesMethods of separationElectrochemical detectionCNPQ::CIENCIAS DA SAUDE::FARMACIAThe use of herbal medicines as an alternative treatment has increased by the belief that natural products do not cause damage to health. However cases in which natural products are added of synthetic drugs not declared, presumably to enhance the effectiveness them have been reported in the literature. In the case of weight loss formulations the main adulterants found are appetite suppressants, antidepressants, benzodiazepines, diuretics and laxatives. The identification of these frauds is only possible by applying the analytical methods able to detect the presence of adulterants in the formulations. This paper describes the development of two methods employing separation techniques with electrochemical detection for the determination of diuretics and laxatives as adulterants in herbal products. The method employing capillary zone electrophoresis (CZE) with contactless conductivity detection (C4D) allows the simultaneous determination of amiloride, chlorthalidone, hydrochlorothiazide, furosemide and phenolphthalein in the following optimized conditions: working electrolyte phosphate buffer 20 mmol L-1 (pH 9.2) containing 30% methanol (v/v) separation potential -15 kV, temperature 25 °C, injection hydrodynamic by gravity in 20 cm for 60 seconds. The method employing ion pair chromatography (IPC) with pulsed amperometric detection (PAD) allows the determination of hydrochlorothiazide, chlorthalidone and furosemide on the following conditions: mobile phase phosphate buffer 5 mmol L-1 (pH 4.5) containing SDS 0.3 mmol L-1 and 50% methanol (v/v), sample potential of +0.8 V, the cleaning potential of -0.2 V and +1.0 V, and flow rate of 1.0 mL/min. Both methods were validated in the parameters of linearity, limit of detection limit of quantification, precision, accuracy and selectivity, and were applied in the analysis of 26 samples of natural weight loss products purchased from pharmacies in nine Brazilian states. In three of 26 samples were identified the presence of illegal diuretic hydrochlorothiazide in concentrations ranging from 0.6 to 7.0 mg/capsule. In addition, five other samples called naturals contained declared on the label of the packaging the presence of synthetic diuretics hydrochlorothiazide or furosemide. Both methods were able to identify the adulterants present in samples with high selectivity and sensitivity. Furthermore, they presented very approximate results in the concentration of adulterants found in the formulations. There is still no unified regulation established by the government for control of herbal products. Each country has its laws, but the marketing is global. Maybe this is the reason why the adulteration of natural products has been a recurring practice in various parts of the world. Therefore, effective regulation for the natural products can result in the reduction of these offenses, and punishment of offenders, thus ensuring the rights of consumers to make quality treatment, safe and effective, without prejudice to health. Keywords: Pharmaceutical formulations, adulterants, diuretics, laxatives, methods of separation, electrochemical detection.Coordenação de Aperfeiçoamento de Pessoal de Nível SuperiorO uso de ervas medicinais como tratamento alternativo tem crescido por se acreditar que produtos naturais não causam danos à saúde. No entanto casos de adulteração de produtos naturais com adição não declarada de fármacos sintéticos, presumidamente para aumentar a eficácia dos mesmos, têm sido relatados na literatura. No caso de formulações emagrecedoras os principais adulterantes já encontrados são anorexígenos, antidepressivos, benzodiazepínicos, diuréticos e laxantes. A identificação destas fraudes só é possível com a aplicação de metodologias analíticas capazes de detectar a presença destes adulterantes nas formulações. Este trabalho descreve o desenvolvimento de duas metodologias empregando técnicas de separação com detecção eletroquímica para a determinação de diuréticos e laxantes como adulterantes em produtos naturais. O método empregando eletroforese capilar de zona (CZE) com detecção por condutividade sem contato (C4D) permite a determinação simultânea de amilorida, clortalidona, hidroclorotiazida, furosemida e fenolftaleína nas condições otimizadas: eletrólito de trabalho tampão fosfato 20 mmol L-1 (pH 9,2) contendo metanol 30% (v/v), potencial de separação -15 Kv, temperatura 25 °C; injeção hidrodinâmica por gravidade em 20 cm durante 60 s. O método empregando cromatografia de par iônico (IPC) com detecção por amperometria pulsada (PAD) permite a determinação de hidroclorotiazida, clortalidona e furosemida nas seguintes condições: fase móvel tampão fosfato 5 mmol L-1 (pH 4,5) contendo SDS 0,3 mmol L-1 e metanol 50% (v/v); potencial de amostragem de +0,8 V; potenciais de limpeza de -0,2 V e +1,0 V; e fluxo de 1,0 mL/min. Os dois métodos foram validados nos parâmetros de linearidade, limite de detecção, limite de quantificação, precisão, exatidão e seletividade e, foram aplicados na análise de 26 amostras de produtos naturais emagrecedores adquiridos de farmácias de manipulação de nove estados brasileiros. Em três das 26 amostras foi identificada a presença ilegal do diurético hidroclorotiazida em concentrações que variaram de 0,6 a 7,0 mg/cápsula. Além disso, outras cinco amostras ditas naturais continham declarado no rótulo das embalagens a presença dos diuréticos sintéticos hidroclorotiazida ou furosemida. Os dois métodos foram capazes de identificar os adulterantes presentes nas amostras com alta seletividade e sensibilidade. Além disso, apresentaram resultados bastante aproximados com relação às concentrações encontradas dos adulterantes nas formulações. Ainda não existe uma regulamentação unificada estabelecida pelos órgãos governamentais para o controle de produtos fitoterápicos. Cada país tem a sua legislação, porém a comercialização destes produtos é globalizada. Talvez por isso a adulteração de produtos naturais vem sendo uma prática recorrente em diversas partes do mundo. Logo, uma regulamentação efetiva para os produtos de origem natural, pode resultar na redução destas infrações, ou punição dos infratores, garantindo assim os direitos dos consumidores de realizar um tratamento de qualidade, seguro e eficaz, sem prejuízo à saúde.Universidade Federal de Santa MariaBRFarmáciaUFSMPrograma de Pós-Graduação em Ciências FarmacêuticasCarvalho, Leandro Machado dehttp://lattes.cnpq.br/6652387343920028Fröehlich, Pedro Eduardohttp://lattes.cnpq.br/5554403984004797Rolim, Clarice Madalena Buenohttp://lattes.cnpq.br/2270654658839508Moreira, Ana Paula Lançanova2013-04-292013-04-292012-07-20info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisapplication/pdfapplication/pdfMOREIRA, Ana Paula Lançanova. Chromatographic and electrophoretic determination of diuretics and laxatives in herbal-based pharmaceutical formulations. 2012. 84 f. Dissertação (Mestrado em Farmacologia) - Universidade Federal de Santa Maria, Santa Maria, 2012.http://repositorio.ufsm.br/handle/1/5914porinfo:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSM2023-06-14T17:35:58Zoai:repositorio.ufsm.br:1/5914Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2023-06-14T17:35:58Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false
dc.title.none.fl_str_mv Determinação cromatográfica e eletroforética de diuréticos e laxantes em formulações farmacêuticas a base de plantas medicinais
Chromatographic and electrophoretic determination of diuretics and laxatives in herbal-based pharmaceutical formulations
title Determinação cromatográfica e eletroforética de diuréticos e laxantes em formulações farmacêuticas a base de plantas medicinais
spellingShingle Determinação cromatográfica e eletroforética de diuréticos e laxantes em formulações farmacêuticas a base de plantas medicinais
Moreira, Ana Paula Lançanova
Formulações farmacêuticas
Adulterantes
Diuréticos
Laxantes
Métodos de separação
Detecção eletroquímica
Pharmaceutical formulations
Adulterants
Diuretics
Laxatives
Methods of separation
Electrochemical detection
CNPQ::CIENCIAS DA SAUDE::FARMACIA
title_short Determinação cromatográfica e eletroforética de diuréticos e laxantes em formulações farmacêuticas a base de plantas medicinais
title_full Determinação cromatográfica e eletroforética de diuréticos e laxantes em formulações farmacêuticas a base de plantas medicinais
title_fullStr Determinação cromatográfica e eletroforética de diuréticos e laxantes em formulações farmacêuticas a base de plantas medicinais
title_full_unstemmed Determinação cromatográfica e eletroforética de diuréticos e laxantes em formulações farmacêuticas a base de plantas medicinais
title_sort Determinação cromatográfica e eletroforética de diuréticos e laxantes em formulações farmacêuticas a base de plantas medicinais
author Moreira, Ana Paula Lançanova
author_facet Moreira, Ana Paula Lançanova
author_role author
dc.contributor.none.fl_str_mv Carvalho, Leandro Machado de
http://lattes.cnpq.br/6652387343920028
Fröehlich, Pedro Eduardo
http://lattes.cnpq.br/5554403984004797
Rolim, Clarice Madalena Bueno
http://lattes.cnpq.br/2270654658839508
dc.contributor.author.fl_str_mv Moreira, Ana Paula Lançanova
dc.subject.por.fl_str_mv Formulações farmacêuticas
Adulterantes
Diuréticos
Laxantes
Métodos de separação
Detecção eletroquímica
Pharmaceutical formulations
Adulterants
Diuretics
Laxatives
Methods of separation
Electrochemical detection
CNPQ::CIENCIAS DA SAUDE::FARMACIA
topic Formulações farmacêuticas
Adulterantes
Diuréticos
Laxantes
Métodos de separação
Detecção eletroquímica
Pharmaceutical formulations
Adulterants
Diuretics
Laxatives
Methods of separation
Electrochemical detection
CNPQ::CIENCIAS DA SAUDE::FARMACIA
description The use of herbal medicines as an alternative treatment has increased by the belief that natural products do not cause damage to health. However cases in which natural products are added of synthetic drugs not declared, presumably to enhance the effectiveness them have been reported in the literature. In the case of weight loss formulations the main adulterants found are appetite suppressants, antidepressants, benzodiazepines, diuretics and laxatives. The identification of these frauds is only possible by applying the analytical methods able to detect the presence of adulterants in the formulations. This paper describes the development of two methods employing separation techniques with electrochemical detection for the determination of diuretics and laxatives as adulterants in herbal products. The method employing capillary zone electrophoresis (CZE) with contactless conductivity detection (C4D) allows the simultaneous determination of amiloride, chlorthalidone, hydrochlorothiazide, furosemide and phenolphthalein in the following optimized conditions: working electrolyte phosphate buffer 20 mmol L-1 (pH 9.2) containing 30% methanol (v/v) separation potential -15 kV, temperature 25 °C, injection hydrodynamic by gravity in 20 cm for 60 seconds. The method employing ion pair chromatography (IPC) with pulsed amperometric detection (PAD) allows the determination of hydrochlorothiazide, chlorthalidone and furosemide on the following conditions: mobile phase phosphate buffer 5 mmol L-1 (pH 4.5) containing SDS 0.3 mmol L-1 and 50% methanol (v/v), sample potential of +0.8 V, the cleaning potential of -0.2 V and +1.0 V, and flow rate of 1.0 mL/min. Both methods were validated in the parameters of linearity, limit of detection limit of quantification, precision, accuracy and selectivity, and were applied in the analysis of 26 samples of natural weight loss products purchased from pharmacies in nine Brazilian states. In three of 26 samples were identified the presence of illegal diuretic hydrochlorothiazide in concentrations ranging from 0.6 to 7.0 mg/capsule. In addition, five other samples called naturals contained declared on the label of the packaging the presence of synthetic diuretics hydrochlorothiazide or furosemide. Both methods were able to identify the adulterants present in samples with high selectivity and sensitivity. Furthermore, they presented very approximate results in the concentration of adulterants found in the formulations. There is still no unified regulation established by the government for control of herbal products. Each country has its laws, but the marketing is global. Maybe this is the reason why the adulteration of natural products has been a recurring practice in various parts of the world. Therefore, effective regulation for the natural products can result in the reduction of these offenses, and punishment of offenders, thus ensuring the rights of consumers to make quality treatment, safe and effective, without prejudice to health. Keywords: Pharmaceutical formulations, adulterants, diuretics, laxatives, methods of separation, electrochemical detection.
publishDate 2012
dc.date.none.fl_str_mv 2012-07-20
2013-04-29
2013-04-29
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 MOREIRA, Ana Paula Lançanova. Chromatographic and electrophoretic determination of diuretics and laxatives in herbal-based pharmaceutical formulations. 2012. 84 f. Dissertação (Mestrado em Farmacologia) - Universidade Federal de Santa Maria, Santa Maria, 2012.
http://repositorio.ufsm.br/handle/1/5914
identifier_str_mv MOREIRA, Ana Paula Lançanova. Chromatographic and electrophoretic determination of diuretics and laxatives in herbal-based pharmaceutical formulations. 2012. 84 f. Dissertação (Mestrado em Farmacologia) - Universidade Federal de Santa Maria, Santa Maria, 2012.
url http://repositorio.ufsm.br/handle/1/5914
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language por
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application/pdf
dc.publisher.none.fl_str_mv Universidade Federal de Santa Maria
BR
Farmácia
UFSM
Programa de Pós-Graduação em Ciências Farmacêuticas
publisher.none.fl_str_mv Universidade Federal de Santa Maria
BR
Farmácia
UFSM
Programa de Pós-Graduação em Ciências Farmacêuticas
dc.source.none.fl_str_mv reponame:Manancial - Repositório Digital da UFSM
instname:Universidade Federal de Santa Maria (UFSM)
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instname_str Universidade Federal de Santa Maria (UFSM)
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institution UFSM
reponame_str Manancial - Repositório Digital da UFSM
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repository.name.fl_str_mv Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)
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