Eletrodo de diamante dopado com boro para a determinação voltamétrica/amperométrica de antihelmínticos e anti-hipertensivos

Detalhes bibliográficos
Ano de defesa: 2014
Autor(a) principal: Lourenção, Bruna Cláudia
Orientador(a): Fatibello Filho, Orlando lattes
Banca de defesa: Não Informado pela instituição
Tipo de documento: Tese
Tipo de acesso: Acesso aberto
Idioma: por
Instituição de defesa: Universidade Federal de São Carlos
Programa de Pós-Graduação: Programa de Pós-Graduação em Química - PPGQ
Departamento: Não Informado pela instituição
País: BR
Palavras-chave em Português:
Área do conhecimento CNPq:
Link de acesso: https://repositorio.ufscar.br/handle/20.500.14289/6308
Resumo: In this work it was developed, firstly, one method for determination of anthelmintic albendazole (ABZ) using differential pulse voltammetry (DPV) and the boron doped diamond (BDD) electrode catholically pretreated (BDD-CPT). The corresponding analytical curve showed linear response in the concentration range from 0.08 to 8.36 ^mol L-1 with detection limit (LD) of 0.06 ^mol L-1. The proposed method was applied in the determination of ABZ in three pharmaceutical formulations with similar results those obtained using a comparative method. The second part of this work it was to develop two electroanalytical procedures using the amperometry technique coupled to a flow injection analysis system (FIA) for the individual determination of two anthelmintic, the ivermectin (IVM) and levamisole (LVM), where it was used the BDD electrode anodically pretreated (BDD-APT) for LVM and BDD-CPT for IVM. Good linear ranges were obtained for the respective analytical curves with values of 0.60 to 50.0 ^mol L-1 for IVM and 0.01 to 6.00 ^mol L 1 for LVM with LD of 0.30 ^mol L 1 and 1.0 nmol L 1, respectively. These analytes were determined in samples of commercial pharmaceutical formulations and synthetic urine and the results obtained are in agreement with the results obtained using two comparative methods (one for each analyte). The analytical frequencies for each method were 48 and 56 determinations per hour for IVM and LVM, respectively. Another procedure was developed for simultaneous determination of two anthelmintics LVM and albendazole sulfoxide (ABZ-SO) in synthetic urine samples using a FIA system with multiple pulses amperometry (MPA) detection and the BDD-APT electrode. This method was applied for directly determination of ABZ-SO and for indirectly determination of LVM. The employed sequence of dual-potential waveform as a function of time, previously optimized, were Edet1 = +1.40 V / ms 200 (pulse potential at which occurs only ABZ-SO oxidation) and Edet2 = 1.90 V / 200 ms (pulse potential at which the oxidation of both anthelmintic, ABZ-SO and LVM, occurs). The analytical curves showed linearity from 2.00 to 100.0 ^mol L-1 (ABZ-SO) and 0.03 to 1.00 ^mol L-1 (LVM), with LD of 1.00 ^mol L-1 and 6.0 nmol L-1 for ABZ-SO and LVM, respectively. Samples of synthetic urine doped with two different concentrations of ABZ-SO and LVM presented recoveries from 93.3 to 100%. The procedure was simple, accurate and fast, with an analytical frequency of 53 samples per hour. In the last one procedure it was developed a method for simultaneous determination of hydrochlorothiazide (HTZ) and enalapril (ENP) (antihypertensives) using a FIA-MPA system and BDD-CPT electrode. The FIA-MPA method was also proposed based on the direct determination of HTZ and indirect of ENP. The sequence application of the pulses as a function of time, were, Edet1 = +1.50 V / ms 150 (pulse potential at which HTZ occurs) and Edet2 = +1.80 V / ms 150 (pulse potential at which oxidation of both analytes (HTZ and ENP) occurs). The analytical curves presented linearity from 0.40 to 8.00 ^mol L -1 to HTZ and from 0.03 to 1.00 ^mol L-1 to HTZ and LD obtained for HTZ and ENP were 0.20 and 0.01 ^mol L-1, respectively. It was analysed three pharmaceutical commercial samples containing both analytes and the results obtained using the FIA-MPA method are in agreement with those obtained using a comparative method (HPLC) with a confidence level of 95%. The procedure was simple and fast, with an analytical frequency of 89 samples per hour.
id SCAR_ef349078d463caf6f4bd2654db45ebb9
oai_identifier_str oai:repositorio.ufscar.br:20.500.14289/6308
network_acronym_str SCAR
network_name_str Repositório Institucional da UFSCAR
repository_id_str
spelling Lourenção, Bruna CláudiaFatibello Filho, Orlandohttp://lattes.cnpq.br/9859737944357808http://lattes.cnpq.br/0205548799348406226e09e2-e217-4c82-8304-a156d0cca0d72016-06-02T20:34:53Z2014-09-092016-06-02T20:34:53Z2014-06-27LOURENÇÃO, Bruna Cláudia. Boron doped diamond electrode for the voltametric/ amperometric determination of anthelmintic and antihypertensive drugs. 2014. 151 f. Tese (Doutorado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2014.https://repositorio.ufscar.br/handle/20.500.14289/6308In this work it was developed, firstly, one method for determination of anthelmintic albendazole (ABZ) using differential pulse voltammetry (DPV) and the boron doped diamond (BDD) electrode catholically pretreated (BDD-CPT). The corresponding analytical curve showed linear response in the concentration range from 0.08 to 8.36 ^mol L-1 with detection limit (LD) of 0.06 ^mol L-1. The proposed method was applied in the determination of ABZ in three pharmaceutical formulations with similar results those obtained using a comparative method. The second part of this work it was to develop two electroanalytical procedures using the amperometry technique coupled to a flow injection analysis system (FIA) for the individual determination of two anthelmintic, the ivermectin (IVM) and levamisole (LVM), where it was used the BDD electrode anodically pretreated (BDD-APT) for LVM and BDD-CPT for IVM. Good linear ranges were obtained for the respective analytical curves with values of 0.60 to 50.0 ^mol L-1 for IVM and 0.01 to 6.00 ^mol L 1 for LVM with LD of 0.30 ^mol L 1 and 1.0 nmol L 1, respectively. These analytes were determined in samples of commercial pharmaceutical formulations and synthetic urine and the results obtained are in agreement with the results obtained using two comparative methods (one for each analyte). The analytical frequencies for each method were 48 and 56 determinations per hour for IVM and LVM, respectively. Another procedure was developed for simultaneous determination of two anthelmintics LVM and albendazole sulfoxide (ABZ-SO) in synthetic urine samples using a FIA system with multiple pulses amperometry (MPA) detection and the BDD-APT electrode. This method was applied for directly determination of ABZ-SO and for indirectly determination of LVM. The employed sequence of dual-potential waveform as a function of time, previously optimized, were Edet1 = +1.40 V / ms 200 (pulse potential at which occurs only ABZ-SO oxidation) and Edet2 = 1.90 V / 200 ms (pulse potential at which the oxidation of both anthelmintic, ABZ-SO and LVM, occurs). The analytical curves showed linearity from 2.00 to 100.0 ^mol L-1 (ABZ-SO) and 0.03 to 1.00 ^mol L-1 (LVM), with LD of 1.00 ^mol L-1 and 6.0 nmol L-1 for ABZ-SO and LVM, respectively. Samples of synthetic urine doped with two different concentrations of ABZ-SO and LVM presented recoveries from 93.3 to 100%. The procedure was simple, accurate and fast, with an analytical frequency of 53 samples per hour. In the last one procedure it was developed a method for simultaneous determination of hydrochlorothiazide (HTZ) and enalapril (ENP) (antihypertensives) using a FIA-MPA system and BDD-CPT electrode. The FIA-MPA method was also proposed based on the direct determination of HTZ and indirect of ENP. The sequence application of the pulses as a function of time, were, Edet1 = +1.50 V / ms 150 (pulse potential at which HTZ occurs) and Edet2 = +1.80 V / ms 150 (pulse potential at which oxidation of both analytes (HTZ and ENP) occurs). The analytical curves presented linearity from 0.40 to 8.00 ^mol L -1 to HTZ and from 0.03 to 1.00 ^mol L-1 to HTZ and LD obtained for HTZ and ENP were 0.20 and 0.01 ^mol L-1, respectively. It was analysed three pharmaceutical commercial samples containing both analytes and the results obtained using the FIA-MPA method are in agreement with those obtained using a comparative method (HPLC) with a confidence level of 95%. The procedure was simple and fast, with an analytical frequency of 89 samples per hour.Neste trabalho de doutorado desenvolveu-se, primeiramente, um método para determinação do anti-helmíntico albendazol (ABZ) utilizando-se voltametria de pulso diferencial (DPV) e o eletrodo de diamante dopado com boro (BDD) pré-tratado catodicamente (BDD-CPT). A curva analítica obtida apresentou resposta linear de 0,08 a 8,36 ^mol L-1 com um LD de 0,06 ^mol L-1. O método foi aplicado na determinação de ABZ em três formulações farmacêuticas com resultados similares aos obtidos empregando-se um método comparativo. A segunda etapa do trabalho teve como objetivo o desenvolvimento de dois procedimentos eletroanalíticos utilizando um sistema de análise por injeção em fluxo (FIA) e detecção amperométrica para a determinação individual de dois anti-helmíticos, a ivermectina (IVM) e o levamisol (LVM), sendo empregado o BDD pré-tratado anodicamente (BDD-APT) para o LVM e o BDD-CPT, para a IVM. As correspondentes curvas analíticas apresentaram boas linearidades nas faixas de concentrações de 0,60 a 50,0 ^mol L-1 (IVM) e 0,01 a 6,00 ^mol L-1 (LVM), com LDs iguais a 0,30 ^mol L-1 e 1,0 nmol L-1, respectivamente. Estes analitos foram determinados em amostras comerciais de formulações farmacêuticas e amostras de urina sintética sendo os resultados obtidos concordantes com os resultados obtidos empregando-se dois métodos comparativos (um para cada analito). A frequência analítica para cada método foi de 48 e 56 determinações por hora para IVM e LVM, respectivamente. Outro procedimento desenvolvido foi a determinação simultânea de dois anti-helmínticos, LVM e sulfóxido de albendazol (ABZ-SO), em amostras de urina sintética utilizando um sistema FIA com detecção por amperometria de múltiplos pulsos (MPA) empregando-se um eletrodo de BDD-APT. O método proposto foi baseado na determinação direta do ABZ-SO e indireta da LVM. A sequência de aplicação dos pulsos em função do tempo, previamente otimizada, foi, Edet1 = +1,40 V / 200 ms (pulso de potencial no qual ocorre a oxidação apenas de ABZ-SO) e Edet2 = +1,90 V /200 ms (pulso de potencial no qual ocorre a oxidação de ambos os anti-helmínticos ABZ-SO e LVM). As curvas analíticas obtidas apresentaram linearidades de 2.00 a 100,0 ^mol L1 (ABZ-SO) e 0,03 a 1,00 ^mol L1 (LVM), com LDs de 1.00^mol L-1 e 6,0 nmol L-1 para ABZ-SO e LVM, respectivamente. Amostras de urina sintética dopadas com ABZ-SO e LVM em duas diferentes concentrações apresentaram recuperações de 93,3 a 100 %. O procedimento desenvolvido mostrou-se simples, preciso e rápido, com uma frequência analítica de 53 determinações por hora. No último procedimento desenvolveu-se um método para a determinação simultânea de hidroclorotiazida (HTZ) e o enalapril (ENP) (anti-hipertensivos) utilizando-se um sistema FIA-MPA e o eletrodo de BDD-CPT. O método FIA-MPA proposto também foi baseado na determinação direta da HTZ e indireta do ENP. A sequência de aplicação dos pulsos em função do tempo utilizada foi, Edet1 = +1,50V / 150 ms (pulso de potencial no qual ocorre a oxidação apenas do HTZ) e Edet2 = +1,80V / 150 ms (pulso de potencial no qual ocorre a oxidação de ambos os analitos (HTZ e ENP)). As curvas analíticas obtidas apresentaram linearidades de 0,40 a 8,00 ^mol L-1 para o HTZ e de 0,03 a 1,00 ^mol L-1 para o ENP e os LDs obtidos para HTZ e ENP foram de 0,20 ^mol L 1 e 0,01 ^mol L 1, respectivamente. Foram analisadas três amostras comerciais farmacêuticas contendo os dois analitos e os resultados obtidos empregando-se o método FIA-FIA-MPA estão em concordância com aqueles obtidos empregando-se um método comparativo (HPLC) em um nível de confiança de 95%. O procedimento desenvolvido mostrou-se simples e rápido, com uma frequência analítica de 89 determinações por hora.Universidade Federal de Minas Geraisapplication/pdfporUniversidade Federal de São CarlosPrograma de Pós-Graduação em Química - PPGQUFSCarBRQuímica analíticaMétodos eletroanalíticosSistema de análise por injeção em fluxoAmperometria de múltiplos pulsosAnti-helmínticosAnti-hipertensivosCIENCIAS EXATAS E DA TERRA::QUIMICAEletrodo de diamante dopado com boro para a determinação voltamétrica/amperométrica de antihelmínticos e anti-hipertensivosBoron doped diamond electrode for the voltametric/ amperometric determination of anthelmintic and antihypertensive drugsinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesis7a1dec22-4b2d-4dba-8971-ab07f55c7d54info:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFSCARinstname:Universidade Federal de São Carlos (UFSCAR)instacron:UFSCARORIGINAL6134.pdfapplication/pdf6629660https://repositorio.ufscar.br/bitstreams/14f877fb-2c1c-46ea-9859-19949c2bc5d9/downloada8afd4d15c98e0427e0d70f440a39debMD51trueAnonymousREADTEXT6134.pdf.txt6134.pdf.txtExtracted texttext/plain0https://repositorio.ufscar.br/bitstreams/a5ddbeff-f947-4cfe-b7b8-dfed15ec29e3/downloadd41d8cd98f00b204e9800998ecf8427eMD56falseAnonymousREADTHUMBNAIL6134.pdf.jpg6134.pdf.jpgIM Thumbnailimage/jpeg8978https://repositorio.ufscar.br/bitstreams/9dde868c-a4ed-4e35-91e3-04a4d277cd2d/download4d03d62d3bcb253491942b0f9bd39842MD57falseAnonymousREAD20.500.14289/63082025-02-06 05:00:10.83open.accessoai:repositorio.ufscar.br:20.500.14289/6308https://repositorio.ufscar.brRepositório InstitucionalPUBhttps://repositorio.ufscar.br/oai/requestrepositorio.sibi@ufscar.bropendoar:43222025-02-06T08:00:10Repositório Institucional da UFSCAR - Universidade Federal de São Carlos (UFSCAR)false
dc.title.por.fl_str_mv Eletrodo de diamante dopado com boro para a determinação voltamétrica/amperométrica de antihelmínticos e anti-hipertensivos
dc.title.alternative.eng.fl_str_mv Boron doped diamond electrode for the voltametric/ amperometric determination of anthelmintic and antihypertensive drugs
title Eletrodo de diamante dopado com boro para a determinação voltamétrica/amperométrica de antihelmínticos e anti-hipertensivos
spellingShingle Eletrodo de diamante dopado com boro para a determinação voltamétrica/amperométrica de antihelmínticos e anti-hipertensivos
Lourenção, Bruna Cláudia
Química analítica
Métodos eletroanalíticos
Sistema de análise por injeção em fluxo
Amperometria de múltiplos pulsos
Anti-helmínticos
Anti-hipertensivos
CIENCIAS EXATAS E DA TERRA::QUIMICA
title_short Eletrodo de diamante dopado com boro para a determinação voltamétrica/amperométrica de antihelmínticos e anti-hipertensivos
title_full Eletrodo de diamante dopado com boro para a determinação voltamétrica/amperométrica de antihelmínticos e anti-hipertensivos
title_fullStr Eletrodo de diamante dopado com boro para a determinação voltamétrica/amperométrica de antihelmínticos e anti-hipertensivos
title_full_unstemmed Eletrodo de diamante dopado com boro para a determinação voltamétrica/amperométrica de antihelmínticos e anti-hipertensivos
title_sort Eletrodo de diamante dopado com boro para a determinação voltamétrica/amperométrica de antihelmínticos e anti-hipertensivos
author Lourenção, Bruna Cláudia
author_facet Lourenção, Bruna Cláudia
author_role author
dc.contributor.authorlattes.por.fl_str_mv http://lattes.cnpq.br/0205548799348406
dc.contributor.author.fl_str_mv Lourenção, Bruna Cláudia
dc.contributor.advisor1.fl_str_mv Fatibello Filho, Orlando
dc.contributor.advisor1Lattes.fl_str_mv http://lattes.cnpq.br/9859737944357808
dc.contributor.authorID.fl_str_mv 226e09e2-e217-4c82-8304-a156d0cca0d7
contributor_str_mv Fatibello Filho, Orlando
dc.subject.por.fl_str_mv Química analítica
Métodos eletroanalíticos
Sistema de análise por injeção em fluxo
Amperometria de múltiplos pulsos
Anti-helmínticos
Anti-hipertensivos
topic Química analítica
Métodos eletroanalíticos
Sistema de análise por injeção em fluxo
Amperometria de múltiplos pulsos
Anti-helmínticos
Anti-hipertensivos
CIENCIAS EXATAS E DA TERRA::QUIMICA
dc.subject.cnpq.fl_str_mv CIENCIAS EXATAS E DA TERRA::QUIMICA
description In this work it was developed, firstly, one method for determination of anthelmintic albendazole (ABZ) using differential pulse voltammetry (DPV) and the boron doped diamond (BDD) electrode catholically pretreated (BDD-CPT). The corresponding analytical curve showed linear response in the concentration range from 0.08 to 8.36 ^mol L-1 with detection limit (LD) of 0.06 ^mol L-1. The proposed method was applied in the determination of ABZ in three pharmaceutical formulations with similar results those obtained using a comparative method. The second part of this work it was to develop two electroanalytical procedures using the amperometry technique coupled to a flow injection analysis system (FIA) for the individual determination of two anthelmintic, the ivermectin (IVM) and levamisole (LVM), where it was used the BDD electrode anodically pretreated (BDD-APT) for LVM and BDD-CPT for IVM. Good linear ranges were obtained for the respective analytical curves with values of 0.60 to 50.0 ^mol L-1 for IVM and 0.01 to 6.00 ^mol L 1 for LVM with LD of 0.30 ^mol L 1 and 1.0 nmol L 1, respectively. These analytes were determined in samples of commercial pharmaceutical formulations and synthetic urine and the results obtained are in agreement with the results obtained using two comparative methods (one for each analyte). The analytical frequencies for each method were 48 and 56 determinations per hour for IVM and LVM, respectively. Another procedure was developed for simultaneous determination of two anthelmintics LVM and albendazole sulfoxide (ABZ-SO) in synthetic urine samples using a FIA system with multiple pulses amperometry (MPA) detection and the BDD-APT electrode. This method was applied for directly determination of ABZ-SO and for indirectly determination of LVM. The employed sequence of dual-potential waveform as a function of time, previously optimized, were Edet1 = +1.40 V / ms 200 (pulse potential at which occurs only ABZ-SO oxidation) and Edet2 = 1.90 V / 200 ms (pulse potential at which the oxidation of both anthelmintic, ABZ-SO and LVM, occurs). The analytical curves showed linearity from 2.00 to 100.0 ^mol L-1 (ABZ-SO) and 0.03 to 1.00 ^mol L-1 (LVM), with LD of 1.00 ^mol L-1 and 6.0 nmol L-1 for ABZ-SO and LVM, respectively. Samples of synthetic urine doped with two different concentrations of ABZ-SO and LVM presented recoveries from 93.3 to 100%. The procedure was simple, accurate and fast, with an analytical frequency of 53 samples per hour. In the last one procedure it was developed a method for simultaneous determination of hydrochlorothiazide (HTZ) and enalapril (ENP) (antihypertensives) using a FIA-MPA system and BDD-CPT electrode. The FIA-MPA method was also proposed based on the direct determination of HTZ and indirect of ENP. The sequence application of the pulses as a function of time, were, Edet1 = +1.50 V / ms 150 (pulse potential at which HTZ occurs) and Edet2 = +1.80 V / ms 150 (pulse potential at which oxidation of both analytes (HTZ and ENP) occurs). The analytical curves presented linearity from 0.40 to 8.00 ^mol L -1 to HTZ and from 0.03 to 1.00 ^mol L-1 to HTZ and LD obtained for HTZ and ENP were 0.20 and 0.01 ^mol L-1, respectively. It was analysed three pharmaceutical commercial samples containing both analytes and the results obtained using the FIA-MPA method are in agreement with those obtained using a comparative method (HPLC) with a confidence level of 95%. The procedure was simple and fast, with an analytical frequency of 89 samples per hour.
publishDate 2014
dc.date.available.fl_str_mv 2014-09-09
2016-06-02T20:34:53Z
dc.date.issued.fl_str_mv 2014-06-27
dc.date.accessioned.fl_str_mv 2016-06-02T20:34:53Z
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
dc.type.driver.fl_str_mv info:eu-repo/semantics/doctoralThesis
format doctoralThesis
status_str publishedVersion
dc.identifier.citation.fl_str_mv LOURENÇÃO, Bruna Cláudia. Boron doped diamond electrode for the voltametric/ amperometric determination of anthelmintic and antihypertensive drugs. 2014. 151 f. Tese (Doutorado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2014.
dc.identifier.uri.fl_str_mv https://repositorio.ufscar.br/handle/20.500.14289/6308
identifier_str_mv LOURENÇÃO, Bruna Cláudia. Boron doped diamond electrode for the voltametric/ amperometric determination of anthelmintic and antihypertensive drugs. 2014. 151 f. Tese (Doutorado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2014.
url https://repositorio.ufscar.br/handle/20.500.14289/6308
dc.language.iso.fl_str_mv por
language por
dc.relation.authority.fl_str_mv 7a1dec22-4b2d-4dba-8971-ab07f55c7d54
dc.rights.driver.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
dc.publisher.none.fl_str_mv Universidade Federal de São Carlos
dc.publisher.program.fl_str_mv Programa de Pós-Graduação em Química - PPGQ
dc.publisher.initials.fl_str_mv UFSCar
dc.publisher.country.fl_str_mv BR
publisher.none.fl_str_mv Universidade Federal de São Carlos
dc.source.none.fl_str_mv reponame:Repositório Institucional da UFSCAR
instname:Universidade Federal de São Carlos (UFSCAR)
instacron:UFSCAR
instname_str Universidade Federal de São Carlos (UFSCAR)
instacron_str UFSCAR
institution UFSCAR
reponame_str Repositório Institucional da UFSCAR
collection Repositório Institucional da UFSCAR
bitstream.url.fl_str_mv https://repositorio.ufscar.br/bitstreams/14f877fb-2c1c-46ea-9859-19949c2bc5d9/download
https://repositorio.ufscar.br/bitstreams/a5ddbeff-f947-4cfe-b7b8-dfed15ec29e3/download
https://repositorio.ufscar.br/bitstreams/9dde868c-a4ed-4e35-91e3-04a4d277cd2d/download
bitstream.checksum.fl_str_mv a8afd4d15c98e0427e0d70f440a39deb
d41d8cd98f00b204e9800998ecf8427e
4d03d62d3bcb253491942b0f9bd39842
bitstream.checksumAlgorithm.fl_str_mv MD5
MD5
MD5
repository.name.fl_str_mv Repositório Institucional da UFSCAR - Universidade Federal de São Carlos (UFSCAR)
repository.mail.fl_str_mv repositorio.sibi@ufscar.br
_version_ 1851145941397012480