Quantificação de vitamina a em concentrados polivitaminicos por cromatografia líquida de alta eficiência

Detalhes bibliográficos
Autor(a) principal: Giacomini, Leandro Zanini
Data de Publicação: 2006
Tipo de documento: Dissertação
Idioma: por
Título da fonte: Biblioteca Digital de Teses e Dissertações do UFSM
Texto Completo: http://repositorio.ufsm.br/handle/1/10144
Resumo: Nowadays the importance and interest for vitamins in human and animal health increased. When vitamin concentration is low in the raw material and is necessary to add multivitamin complexes to the animal diet a representative cost is incorporated to animals nutrition. The proposal of this study was evaluation and validation of a methodology by high performance liquid chromatography to quantify vitamin A in polyvitamin concentrates for animal nutrition. The method developed was adapted for the Micotoxicologic Analysis Laboratory conditions, placed at Universidade Federal de Santa Maria (RS), from a method published at United States Pharmacopoeia . The vitamin A extraction from concentrates was done using hexane as extraction solvent after hydrolysis and saponification. The recovery found for this method was 85.98% with a mean of relative standard deviation (RSD) of 1,52% at the repetition test using premix samples. All analyses were performed using a HPLC system with UV detection at 325 nm, a reversed phase column at 1 mL/min flow rate and 40oC of temperature. The mobile phase used was methanol:water (98:2, v/v) at isocratic mode. The calibration curve was constructed using standard vitamin A (All-trans-retinol) at concentrations varying from 0.475 to 9.50 μg/mL. The correlation coefficient (r2) was 0.9995, the detection limit 0.095 μg/mL and quantification limit of 0.24 μg/mL for Aderex (compound without vitamin A with non uniform particles) fortified samples.Observing the results obtained, in 15 premix samples analyzed, six samples (40 %) of them present values of vitamin A greater than the desired concentration. Four samples (26,67 %) had values bellow the expected and only five (33,33 %) presented values between the minimum and maximum preconized for birds and pig nutrition. In this way, this method was efficient, rapid and precise for routine analysis providing in this way, an important instrument for quality control in animal nutrition area.
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spelling 2017-06-132017-06-132006-02-24http://repositorio.ufsm.br/handle/1/10144Nowadays the importance and interest for vitamins in human and animal health increased. When vitamin concentration is low in the raw material and is necessary to add multivitamin complexes to the animal diet a representative cost is incorporated to animals nutrition. The proposal of this study was evaluation and validation of a methodology by high performance liquid chromatography to quantify vitamin A in polyvitamin concentrates for animal nutrition. The method developed was adapted for the Micotoxicologic Analysis Laboratory conditions, placed at Universidade Federal de Santa Maria (RS), from a method published at United States Pharmacopoeia . The vitamin A extraction from concentrates was done using hexane as extraction solvent after hydrolysis and saponification. The recovery found for this method was 85.98% with a mean of relative standard deviation (RSD) of 1,52% at the repetition test using premix samples. All analyses were performed using a HPLC system with UV detection at 325 nm, a reversed phase column at 1 mL/min flow rate and 40oC of temperature. The mobile phase used was methanol:water (98:2, v/v) at isocratic mode. The calibration curve was constructed using standard vitamin A (All-trans-retinol) at concentrations varying from 0.475 to 9.50 μg/mL. The correlation coefficient (r2) was 0.9995, the detection limit 0.095 μg/mL and quantification limit of 0.24 μg/mL for Aderex (compound without vitamin A with non uniform particles) fortified samples.Observing the results obtained, in 15 premix samples analyzed, six samples (40 %) of them present values of vitamin A greater than the desired concentration. Four samples (26,67 %) had values bellow the expected and only five (33,33 %) presented values between the minimum and maximum preconized for birds and pig nutrition. In this way, this method was efficient, rapid and precise for routine analysis providing in this way, an important instrument for quality control in animal nutrition area.Atualmente o interesse por vitaminas tem sido de grande importância na saúde humana e animal. Suas concentrações nos ingredientes são baixas, sendo necessário a adição nas dietas, através da utilização de complexos multivitamínicos, agregando custos à alimentação que por vezes são representativos. No presente estudo buscou-se a validação do método por cromatografia liquida de alta eficiência para determinação de vitamina A em concentrados multivitamínicos para a nutrição animal. A metodologia de análise de vitamina A foi a partir do método publicado na United States Pharmacopeia , adaptado às condições do Laboratório de Análises Micotoxicológicas da Universidade Federal de Santa Maria. A fase móvel utilizada para a determinação da vitamina (All-trans-retinol) foi composta de metanol: água (98:2 v/v). O comprimento de onda ideal para a vitamina A no detector UV, foi de 325 nm. Utilizou-se coluna de fase reversa C18, vazão de 1 mL/min e temperatura da coluna de 40º C. O tempo de análise cromatográfica ocorreu em 8 minutos, sendo que a vitamina A eluiu em 4,2 minutos. O método mostrou-se linear, apresentando um coeficiente de correlação igual a r = 0,9995, nas concentrações de 0,475 9,50 μg/mL. O limite de quantificação encontrado para amostras nas quais o veiculo para adição de vitaminas apresentavam partículas desuniformes (Aderex) foi de 0,24 μg/mL. A vitamina A foi extraída com o emprego de hexano, após processo de hidrólise e saponificação. O coeficiente de recuperação do método foi de 85,98%. Na análise de repetitividade do método em amostras de premixes obteve-se uma média de CV de 1,52%. De acordo com os resultados encontrados, observa-se que 4 (26,67 %) das amostras de premixes analisadas apresentaram valor abaixo do esperado. Entre as 15 amostras analisadas, 6 (40,0 %) dos premixes apresentaram valores de vitamina A acima da concentração desejada. Somente 5 amostras (33,33 %) apresentaram valores de vitamina A dentro dos parâmetros de mínimo e máximo preconizados para alimentação de aves e suínos. O método mostrou-se eficiente, rápido e preciso para análise de rotina, disponibilizando desta forma, uma importante ferramenta para controle de qualidade na alimentação animal.porUniversidade Federal de Santa MariaPrograma de Pós-Graduação em Medicina VeterináriaUFSMBRMedicina VeterináriaCLAEPremixVitamina AHPLCPremixVitamin ACNPQ::CIENCIAS AGRARIAS::MEDICINA VETERINARIAQuantificação de vitamina a em concentrados polivitaminicos por cromatografia líquida de alta eficiênciaQuantification of vitamin a in polyvitamin concentrated by high performance liquid chromatography analysisinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisMallmann, Carlos Augustohttp://lattes.cnpq.br/5193771213666058Zanella, Irineohttp://lattes.cnpq.br/7498503120935080Lovatto, Paulo Albertohttp://lattes.cnpq.br/6602777713142665http://lattes.cnpq.br/3118907503918438Giacomini, Leandro Zanini500500000007400500300500500f8b7bb02-50a2-468a-91b2-0a75e5374e2f58988882-031e-4852-9e4c-58a8569fce69e90265df-3980-4f01-a256-8a201ba774da4ee7ce5c-76be-4f49-8389-8de5decd84c6info:eu-repo/semantics/openAccessreponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALGiacomini, Leandro Zanini.pdfGiacomini, Leandro Zanini.pdfDissertação de Mestradoapplication/pdf393637http://repositorio.ufsm.br/bitstream/1/10144/1/Giacomini%2c%20Leandro%20Zanini.pdf4c1aed5740da105cb5ba5489ddbf2fe3MD51TEXTGiacomini, Leandro Zanini.pdf.txtGiacomini, Leandro Zanini.pdf.txtExtracted texttext/plain109951http://repositorio.ufsm.br/bitstream/1/10144/2/Giacomini%2c%20Leandro%20Zanini.pdf.txt8d897e7acc8115fc8dce84e82ae7c0e5MD52THUMBNAILGiacomini, Leandro Zanini.pdf.jpgGiacomini, Leandro Zanini.pdf.jpgIM Thumbnailimage/jpeg5034http://repositorio.ufsm.br/bitstream/1/10144/3/Giacomini%2c%20Leandro%20Zanini.pdf.jpgb981b228d0c14aa35eeb4010c9bc6f77MD531/101442023-01-09 09:45:51.237oai:repositorio.ufsm.br:1/10144Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2023-01-09T12:45:51Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false
dc.title.por.fl_str_mv Quantificação de vitamina a em concentrados polivitaminicos por cromatografia líquida de alta eficiência
dc.title.alternative.eng.fl_str_mv Quantification of vitamin a in polyvitamin concentrated by high performance liquid chromatography analysis
title Quantificação de vitamina a em concentrados polivitaminicos por cromatografia líquida de alta eficiência
spellingShingle Quantificação de vitamina a em concentrados polivitaminicos por cromatografia líquida de alta eficiência
Giacomini, Leandro Zanini
CLAE
Premix
Vitamina A
HPLC
Premix
Vitamin A
CNPQ::CIENCIAS AGRARIAS::MEDICINA VETERINARIA
title_short Quantificação de vitamina a em concentrados polivitaminicos por cromatografia líquida de alta eficiência
title_full Quantificação de vitamina a em concentrados polivitaminicos por cromatografia líquida de alta eficiência
title_fullStr Quantificação de vitamina a em concentrados polivitaminicos por cromatografia líquida de alta eficiência
title_full_unstemmed Quantificação de vitamina a em concentrados polivitaminicos por cromatografia líquida de alta eficiência
title_sort Quantificação de vitamina a em concentrados polivitaminicos por cromatografia líquida de alta eficiência
author Giacomini, Leandro Zanini
author_facet Giacomini, Leandro Zanini
author_role author
dc.contributor.advisor1.fl_str_mv Mallmann, Carlos Augusto
dc.contributor.advisor1Lattes.fl_str_mv http://lattes.cnpq.br/5193771213666058
dc.contributor.referee1.fl_str_mv Zanella, Irineo
dc.contributor.referee1Lattes.fl_str_mv http://lattes.cnpq.br/7498503120935080
dc.contributor.referee2.fl_str_mv Lovatto, Paulo Alberto
dc.contributor.referee2Lattes.fl_str_mv http://lattes.cnpq.br/6602777713142665
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/3118907503918438
dc.contributor.author.fl_str_mv Giacomini, Leandro Zanini
contributor_str_mv Mallmann, Carlos Augusto
Zanella, Irineo
Lovatto, Paulo Alberto
dc.subject.por.fl_str_mv CLAE
Premix
Vitamina A
topic CLAE
Premix
Vitamina A
HPLC
Premix
Vitamin A
CNPQ::CIENCIAS AGRARIAS::MEDICINA VETERINARIA
dc.subject.eng.fl_str_mv HPLC
Premix
Vitamin A
dc.subject.cnpq.fl_str_mv CNPQ::CIENCIAS AGRARIAS::MEDICINA VETERINARIA
description Nowadays the importance and interest for vitamins in human and animal health increased. When vitamin concentration is low in the raw material and is necessary to add multivitamin complexes to the animal diet a representative cost is incorporated to animals nutrition. The proposal of this study was evaluation and validation of a methodology by high performance liquid chromatography to quantify vitamin A in polyvitamin concentrates for animal nutrition. The method developed was adapted for the Micotoxicologic Analysis Laboratory conditions, placed at Universidade Federal de Santa Maria (RS), from a method published at United States Pharmacopoeia . The vitamin A extraction from concentrates was done using hexane as extraction solvent after hydrolysis and saponification. The recovery found for this method was 85.98% with a mean of relative standard deviation (RSD) of 1,52% at the repetition test using premix samples. All analyses were performed using a HPLC system with UV detection at 325 nm, a reversed phase column at 1 mL/min flow rate and 40oC of temperature. The mobile phase used was methanol:water (98:2, v/v) at isocratic mode. The calibration curve was constructed using standard vitamin A (All-trans-retinol) at concentrations varying from 0.475 to 9.50 μg/mL. The correlation coefficient (r2) was 0.9995, the detection limit 0.095 μg/mL and quantification limit of 0.24 μg/mL for Aderex (compound without vitamin A with non uniform particles) fortified samples.Observing the results obtained, in 15 premix samples analyzed, six samples (40 %) of them present values of vitamin A greater than the desired concentration. Four samples (26,67 %) had values bellow the expected and only five (33,33 %) presented values between the minimum and maximum preconized for birds and pig nutrition. In this way, this method was efficient, rapid and precise for routine analysis providing in this way, an important instrument for quality control in animal nutrition area.
publishDate 2006
dc.date.issued.fl_str_mv 2006-02-24
dc.date.accessioned.fl_str_mv 2017-06-13
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