Perfil cromatográfico e análise multivariada para o controle de qualidade de amostras comerciais do gênero Phyllanthus (quebra-pedra)

Detalhes bibliográficos
Autor(a) principal: Martins, Lucia Regina Rocha
Data de Publicação: 2008
Tipo de documento: Tese
Idioma: por
Título da fonte: Repositório Institucional da UFSCAR
Texto Completo: https://repositorio.ufscar.br/handle/ufscar/6137
Resumo: This work present the development and application of methods by High Performance Liquid Chromatography (HPLC) to the quality control of vegetable samples known as stone breaker , that correspond to Phyllanthus species, two of them entered in Brazilian Pharmacopoeia: P.niruri L. and P. tenellus Roxb. A chromatographic profile analytical method was developed and validated, using HPLC with diode array detection (DAD), for the analysis of aqueous extracts of Phyllanthus authentic samples, which consisted of six species grown under controlled conditions in two different sites (Campinas and São Carlos, Brazil) and also not cultivated samples, collected in 27 cities of São Paulo state. Chemometric methods of exploratory analysis were used to interpret the chromatographic informations, such as Principal Component Analysis (PCA) and Hierarquical Cluster Analysis (HCA). Classification models (SIMCA, KNN e PLS-DA) were developed and validated and demonstrated that the Phyllanthus species can be differentiated from each other through their chromatographic profiles and multivariate analysis. The chromatographic method was applied in the analysis of 25 stone breaker commercial samples and their authenticity was determined by the classification models: the results showed that most products are produced with the P. tenellus species, although they are marketed as P. niruri; two samples was determined as adulteration since they were not classified as any Phyllanthus species. A chemical marker was purified by semi-preparative HPLC-UV from the crude aqueous extract of P. niruri specie; spectroscopy characterization determined its structure as corilagin, an hydrolisable tannin. An analytical method by HPLC-UV was developed and validated for quantification of this marker in extracts of Phyllanthus species and stone breaker commercial samples. For the cultivated samples, there was significant variability in the concentration of corilagin according to the place of cultivation and the time of year; among the non-cultivated P. tenellus samples, there was large differences in the marker concentration, result of the influence of different habitats in secondary metabolism of the plant. The corilagin quantification therefore was not feasible to determine the authenticity/quality of commercial samples, but can be used in the monitoring of Phyllanthus cultivated species. In two commercial samples the marker was not detected, which characterized as adulterated samples of stone breaker .
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spelling Martins, Lucia Regina RochaCass, Quezia Bezerrahttp://genos.cnpq.br:12010/dwlattes/owa/prc_imp_cv_int?f_cod=K4781559E6http://lattes.cnpq.br/03018048229986469c6ffb0d-2ea2-4130-816c-9c84af0e88012016-06-02T20:34:15Z2009-10-292016-06-02T20:34:15Z2008-12-05MARTINS, Lucia Regina Rocha. Chromatographic profile and multivaried analysis to quality control of commercial samples of the Phyllanthus genus (stone breaker). 2008. 154 f. Tese (Doutorado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2008.https://repositorio.ufscar.br/handle/ufscar/6137This work present the development and application of methods by High Performance Liquid Chromatography (HPLC) to the quality control of vegetable samples known as stone breaker , that correspond to Phyllanthus species, two of them entered in Brazilian Pharmacopoeia: P.niruri L. and P. tenellus Roxb. A chromatographic profile analytical method was developed and validated, using HPLC with diode array detection (DAD), for the analysis of aqueous extracts of Phyllanthus authentic samples, which consisted of six species grown under controlled conditions in two different sites (Campinas and São Carlos, Brazil) and also not cultivated samples, collected in 27 cities of São Paulo state. Chemometric methods of exploratory analysis were used to interpret the chromatographic informations, such as Principal Component Analysis (PCA) and Hierarquical Cluster Analysis (HCA). Classification models (SIMCA, KNN e PLS-DA) were developed and validated and demonstrated that the Phyllanthus species can be differentiated from each other through their chromatographic profiles and multivariate analysis. The chromatographic method was applied in the analysis of 25 stone breaker commercial samples and their authenticity was determined by the classification models: the results showed that most products are produced with the P. tenellus species, although they are marketed as P. niruri; two samples was determined as adulteration since they were not classified as any Phyllanthus species. A chemical marker was purified by semi-preparative HPLC-UV from the crude aqueous extract of P. niruri specie; spectroscopy characterization determined its structure as corilagin, an hydrolisable tannin. An analytical method by HPLC-UV was developed and validated for quantification of this marker in extracts of Phyllanthus species and stone breaker commercial samples. For the cultivated samples, there was significant variability in the concentration of corilagin according to the place of cultivation and the time of year; among the non-cultivated P. tenellus samples, there was large differences in the marker concentration, result of the influence of different habitats in secondary metabolism of the plant. The corilagin quantification therefore was not feasible to determine the authenticity/quality of commercial samples, but can be used in the monitoring of Phyllanthus cultivated species. In two commercial samples the marker was not detected, which characterized as adulterated samples of stone breaker .O presente trabalho apresenta o desenvolvimento e aplicação de métodos por Cromatografia Líquida de Alta Eficiência (CLAE) para o controle de qualidade de amostras vegetais conhecidas como quebra-pedra , que correspondem a espécies do gênero Phyllanthus, duas delas inscritas na Farmacopéia Brasileira: P.niruri L. e P. tenellus Roxb. Um método analítico de perfil cromatográfico foi desenvolvido e validado, utilizando CLAE com detecção por arranjo de diodos (DAD), para a análise de extratos aquosos de amostras autênticas de Phyllanthus, que consistiram de seis espécies cultivadas sob condições controladas, em dois diferentes locais (Campinas e São Carlos/SP, Brasil) e também de amostras não cultivadas, coletadas em 27 municípios do estado de São Paulo. Para a interpretação das informações cromatográficas, métodos quimiométricos de análise exploratória foram utilizados: Análise de Componentes Principais (PCA) e Análise de Agrupamentos Hierárquicos (HCA). Modelos quimiométricos de classificação (SIMCA, KNN e PLS-DA) foram elaborados e validados e demonstraram que as espécies de Phyllanthus podem ser diferenciadas entre si através de seus perfis cromatográficos e análise multivariada. O método cromatográfico foi aplicado na análise de 25 amostras comerciais de quebra-pedra e sua autenticidade foi determinada através dos modelos de classificação: os resultados demonstraram que a maior parte dos produtos é produzida com a espécie P. tenellus, embora sejam comercializados como P. niruri; para duas amostras foi determinada adulteração, uma vez que não foram classificadas como nenhuma espécie de Phyllanthus. Utilizando CLAE-UV semi-preparativa, um marcador químico foi purificado a partir do extrato aquoso bruto da espécie P. niruri; a caracterização espectroscópica determinou sua estrutura como sendo a corilagina, um tanino hidrolisável. Um método analítico por CLAE-UV foi desenvolvido e validado para a quantificação desse marcador em extratos de espécies de Phyllanthus e em amostras comerciais de quebra-pedra . Para as amostras cultivadas, verificou-se significativa variabilidade na concentração de corilagina em função do local de cultivo e da época do ano; entre as amostras não-cultivadas de P. tenellus, houve grandes diferenças na concentração do marcador, resultado da influência de diferentes habitat s no metabolismo secundário do vegetal. A quantificação de corilagina, portanto, não se mostrou viável na determinação da autenticidade/qualidade de amostras comerciais, porém pode ser utilizada no monitoramento de espécies cultivadas de Phyllanthus. Em duas amostras comerciais o marcador não foi detectado, o que as caracterizou como amostras adulteradas de quebra-pedra .Universidade Federal de Minas Geraisapplication/pdfporUniversidade Federal de São CarlosPrograma de Pós-Graduação em Química - PPGQUFSCarBRCromatografia líquida de alta eficiênciaPhyllanthusPerfil cromatográficoControle de qualidadeCIENCIAS EXATAS E DA TERRA::QUIMICAPerfil cromatográfico e análise multivariada para o controle de qualidade de amostras comerciais do gênero Phyllanthus (quebra-pedra)Chromatographic profile and multivaried analysis to quality control of commercial samples of the Phyllanthus genus (stone breaker)info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesis-1-1867fc213-f339-49e1-a669-a1e54cf68bf1info:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFSCARinstname:Universidade Federal de São Carlos (UFSCAR)instacron:UFSCARORIGINAL2186.pdfapplication/pdf7582063https://repositorio.ufscar.br/bitstream/ufscar/6137/1/2186.pdf715da59653caf8b9238d64f51054ac22MD51THUMBNAIL2186.pdf.jpg2186.pdf.jpgIM Thumbnailimage/jpeg9470https://repositorio.ufscar.br/bitstream/ufscar/6137/2/2186.pdf.jpgc98b1e23f842b58cee544226069351dfMD52ufscar/61372023-09-18 18:31:09.932oai:repositorio.ufscar.br:ufscar/6137Repositório InstitucionalPUBhttps://repositorio.ufscar.br/oai/requestopendoar:43222023-09-18T18:31:09Repositório Institucional da UFSCAR - Universidade Federal de São Carlos (UFSCAR)false
dc.title.por.fl_str_mv Perfil cromatográfico e análise multivariada para o controle de qualidade de amostras comerciais do gênero Phyllanthus (quebra-pedra)
dc.title.alternative.eng.fl_str_mv Chromatographic profile and multivaried analysis to quality control of commercial samples of the Phyllanthus genus (stone breaker)
title Perfil cromatográfico e análise multivariada para o controle de qualidade de amostras comerciais do gênero Phyllanthus (quebra-pedra)
spellingShingle Perfil cromatográfico e análise multivariada para o controle de qualidade de amostras comerciais do gênero Phyllanthus (quebra-pedra)
Martins, Lucia Regina Rocha
Cromatografia líquida de alta eficiência
Phyllanthus
Perfil cromatográfico
Controle de qualidade
CIENCIAS EXATAS E DA TERRA::QUIMICA
title_short Perfil cromatográfico e análise multivariada para o controle de qualidade de amostras comerciais do gênero Phyllanthus (quebra-pedra)
title_full Perfil cromatográfico e análise multivariada para o controle de qualidade de amostras comerciais do gênero Phyllanthus (quebra-pedra)
title_fullStr Perfil cromatográfico e análise multivariada para o controle de qualidade de amostras comerciais do gênero Phyllanthus (quebra-pedra)
title_full_unstemmed Perfil cromatográfico e análise multivariada para o controle de qualidade de amostras comerciais do gênero Phyllanthus (quebra-pedra)
title_sort Perfil cromatográfico e análise multivariada para o controle de qualidade de amostras comerciais do gênero Phyllanthus (quebra-pedra)
author Martins, Lucia Regina Rocha
author_facet Martins, Lucia Regina Rocha
author_role author
dc.contributor.authorlattes.por.fl_str_mv http://lattes.cnpq.br/0301804822998646
dc.contributor.author.fl_str_mv Martins, Lucia Regina Rocha
dc.contributor.advisor1.fl_str_mv Cass, Quezia Bezerra
dc.contributor.advisor1Lattes.fl_str_mv http://genos.cnpq.br:12010/dwlattes/owa/prc_imp_cv_int?f_cod=K4781559E6
dc.contributor.authorID.fl_str_mv 9c6ffb0d-2ea2-4130-816c-9c84af0e8801
contributor_str_mv Cass, Quezia Bezerra
dc.subject.por.fl_str_mv Cromatografia líquida de alta eficiência
Phyllanthus
Perfil cromatográfico
Controle de qualidade
topic Cromatografia líquida de alta eficiência
Phyllanthus
Perfil cromatográfico
Controle de qualidade
CIENCIAS EXATAS E DA TERRA::QUIMICA
dc.subject.cnpq.fl_str_mv CIENCIAS EXATAS E DA TERRA::QUIMICA
description This work present the development and application of methods by High Performance Liquid Chromatography (HPLC) to the quality control of vegetable samples known as stone breaker , that correspond to Phyllanthus species, two of them entered in Brazilian Pharmacopoeia: P.niruri L. and P. tenellus Roxb. A chromatographic profile analytical method was developed and validated, using HPLC with diode array detection (DAD), for the analysis of aqueous extracts of Phyllanthus authentic samples, which consisted of six species grown under controlled conditions in two different sites (Campinas and São Carlos, Brazil) and also not cultivated samples, collected in 27 cities of São Paulo state. Chemometric methods of exploratory analysis were used to interpret the chromatographic informations, such as Principal Component Analysis (PCA) and Hierarquical Cluster Analysis (HCA). Classification models (SIMCA, KNN e PLS-DA) were developed and validated and demonstrated that the Phyllanthus species can be differentiated from each other through their chromatographic profiles and multivariate analysis. The chromatographic method was applied in the analysis of 25 stone breaker commercial samples and their authenticity was determined by the classification models: the results showed that most products are produced with the P. tenellus species, although they are marketed as P. niruri; two samples was determined as adulteration since they were not classified as any Phyllanthus species. A chemical marker was purified by semi-preparative HPLC-UV from the crude aqueous extract of P. niruri specie; spectroscopy characterization determined its structure as corilagin, an hydrolisable tannin. An analytical method by HPLC-UV was developed and validated for quantification of this marker in extracts of Phyllanthus species and stone breaker commercial samples. For the cultivated samples, there was significant variability in the concentration of corilagin according to the place of cultivation and the time of year; among the non-cultivated P. tenellus samples, there was large differences in the marker concentration, result of the influence of different habitats in secondary metabolism of the plant. The corilagin quantification therefore was not feasible to determine the authenticity/quality of commercial samples, but can be used in the monitoring of Phyllanthus cultivated species. In two commercial samples the marker was not detected, which characterized as adulterated samples of stone breaker .
publishDate 2008
dc.date.issued.fl_str_mv 2008-12-05
dc.date.available.fl_str_mv 2009-10-29
2016-06-02T20:34:15Z
dc.date.accessioned.fl_str_mv 2016-06-02T20:34:15Z
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
dc.type.driver.fl_str_mv info:eu-repo/semantics/doctoralThesis
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dc.identifier.citation.fl_str_mv MARTINS, Lucia Regina Rocha. Chromatographic profile and multivaried analysis to quality control of commercial samples of the Phyllanthus genus (stone breaker). 2008. 154 f. Tese (Doutorado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2008.
dc.identifier.uri.fl_str_mv https://repositorio.ufscar.br/handle/ufscar/6137
identifier_str_mv MARTINS, Lucia Regina Rocha. Chromatographic profile and multivaried analysis to quality control of commercial samples of the Phyllanthus genus (stone breaker). 2008. 154 f. Tese (Doutorado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2008.
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