Determination of Thiamine in Wheat Flours Using a Validated Isocratic HPLC-Fluorescence Method Previously Optimized by Box-Behnken Design

Autores
Michlig, Nicolás; Van de Velde, Franco; Freyre, Marcelino Ricardo; Bernardi, Cecilia
Año de publicación
2014
Idioma
inglés
Tipo de recurso
artículo
Estado
versión publicada
Descripción
The main purpose of this work was to optimize and validate a new isocratic high-performance liquid chromatography method for thiamine analysis in wheat flours. Thiamine was previously derivatized into thiochrome and determined by fluorescence detection (excitation wavelength, 366 nm; emission wavelength, 435 nm). The mobile phase consisted of buffer phosphate (0.02 M) and organic modifier (methanol 88 %; acetonitrile 12 %). Optimization was done using a Box-Behnken design (three factors at three levels) where organic modifier proportion (A), varying from 20 to 90 %, mobile phase pH (B), varying from 5.8 to 7.8, and flow rate (C), varying from 0.5 to 1 mL min-1, were the studied variables. Peak width was the studied response. Optimal chromatographic conditions that minimized response were A = 90 %, B = 6.00, and C = 1 mL min-1. Using optimal conditions, thiochrome extractions with isobutanol and solid-phase extraction (SPE) employing styrene-divinylbenzene adsorbent cartridges were compared. Method validation, using thiamine standard solutions and both types of thiochrome isolation, included linearity studies, limits of detection and quantification, and calibration and analytical sensitivity quantifications. Standard addition method was employed to quantify thiamine in wheat flours. Good precision results were obtained by both extraction methods. Recoveries ranged from 63 to 65 % for isobutanol and 84 to 101 % for SPE, including sample extraction, thiamine derivatization, thiochrome purification, and chromatographic separation. Taking into account better obtained SPE recoveries, acceptable precision, and isobutanol irritant action on the eyes and skin of operator, SPE using styrene-divinylbenzene adsorbent could be chosen for routine thiamine analysis in wheat flour samples.
Fil: Michlig, Nicolás. Universidad Nacional del Litoral. Facultad de Ingeniería Química. Instituto de Tecnología de los Alimentos; Argentina
Fil: Van de Velde, Franco. Consejo Nacional de Investigaciones Científicas y Técnicas; Argentina. Universidad Nacional del Litoral. Facultad de Ingeniería Química. Instituto de Tecnología de los Alimentos; Argentina
Fil: Freyre, Marcelino Ricardo. Universidad Nacional del Litoral. Facultad de Ingeniería Química. Instituto de Tecnología de los Alimentos; Argentina
Fil: Bernardi, Cecilia. Universidad Nacional del Litoral. Facultad de Ingeniería Química. Instituto de Tecnología de los Alimentos; Argentina
Materia
CHROMATOGRAPHIC OPTIMIZATION
THIAMINE
THIOCHROME SOLID-PHASE EXTRACTION
Nivel de accesibilidad
acceso abierto
Condiciones de uso
https://creativecommons.org/licenses/by-nc-sa/2.5/ar/
Repositorio
CONICET Digital (CONICET)
Institución
Consejo Nacional de Investigaciones Científicas y Técnicas
OAI Identificador
oai:ri.conicet.gov.ar:11336/92743
Acceder
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network_name_str CONICET Digital (CONICET)
spelling Determination of Thiamine in Wheat Flours Using a Validated Isocratic HPLC-Fluorescence Method Previously Optimized by Box-Behnken DesignMichlig, NicolásVan de Velde, FrancoFreyre, Marcelino RicardoBernardi, CeciliaCHROMATOGRAPHIC OPTIMIZATIONTHIAMINETHIOCHROME SOLID-PHASE EXTRACTIONhttps://purl.org/becyt/ford/1.4https://purl.org/becyt/ford/1The main purpose of this work was to optimize and validate a new isocratic high-performance liquid chromatography method for thiamine analysis in wheat flours. Thiamine was previously derivatized into thiochrome and determined by fluorescence detection (excitation wavelength, 366 nm; emission wavelength, 435 nm). The mobile phase consisted of buffer phosphate (0.02 M) and organic modifier (methanol 88 %; acetonitrile 12 %). Optimization was done using a Box-Behnken design (three factors at three levels) where organic modifier proportion (A), varying from 20 to 90 %, mobile phase pH (B), varying from 5.8 to 7.8, and flow rate (C), varying from 0.5 to 1 mL min-1, were the studied variables. Peak width was the studied response. Optimal chromatographic conditions that minimized response were A = 90 %, B = 6.00, and C = 1 mL min-1. Using optimal conditions, thiochrome extractions with isobutanol and solid-phase extraction (SPE) employing styrene-divinylbenzene adsorbent cartridges were compared. Method validation, using thiamine standard solutions and both types of thiochrome isolation, included linearity studies, limits of detection and quantification, and calibration and analytical sensitivity quantifications. Standard addition method was employed to quantify thiamine in wheat flours. Good precision results were obtained by both extraction methods. Recoveries ranged from 63 to 65 % for isobutanol and 84 to 101 % for SPE, including sample extraction, thiamine derivatization, thiochrome purification, and chromatographic separation. Taking into account better obtained SPE recoveries, acceptable precision, and isobutanol irritant action on the eyes and skin of operator, SPE using styrene-divinylbenzene adsorbent could be chosen for routine thiamine analysis in wheat flour samples.Fil: Michlig, Nicolás. Universidad Nacional del Litoral. Facultad de Ingeniería Química. Instituto de Tecnología de los Alimentos; ArgentinaFil: Van de Velde, Franco. Consejo Nacional de Investigaciones Científicas y Técnicas; Argentina. Universidad Nacional del Litoral. Facultad de Ingeniería Química. Instituto de Tecnología de los Alimentos; ArgentinaFil: Freyre, Marcelino Ricardo. Universidad Nacional del Litoral. Facultad de Ingeniería Química. Instituto de Tecnología de los Alimentos; ArgentinaFil: Bernardi, Cecilia. Universidad Nacional del Litoral. Facultad de Ingeniería Química. Instituto de Tecnología de los Alimentos; ArgentinaSpringer2014-04info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionhttp://purl.org/coar/resource_type/c_6501info:ar-repo/semantics/articuloapplication/pdfapplication/pdfhttp://hdl.handle.net/11336/92743Michlig, Nicolás; Van de Velde, Franco; Freyre, Marcelino Ricardo; Bernardi, Cecilia; Determination of Thiamine in Wheat Flours Using a Validated Isocratic HPLC-Fluorescence Method Previously Optimized by Box-Behnken Design; Springer; Food Analytical Methods; 7; 4; 4-2014; 828-8351936-9751CONICET DigitalCONICETenginfo:eu-repo/semantics/altIdentifier/url/http://link.springer.com/article/10.1007%2Fs12161-013-9688-3info:eu-repo/semantics/altIdentifier/doi/10.1007/s12161-013-9688-3info:eu-repo/semantics/openAccesshttps://creativecommons.org/licenses/by-nc-sa/2.5/ar/reponame:CONICET Digital (CONICET)instname:Consejo Nacional de Investigaciones Científicas y Técnicas2025-09-29T09:49:06Zoai:ri.conicet.gov.ar:11336/92743instacron:CONICETInstitucionalhttp://ri.conicet.gov.ar/Organismo científico-tecnológicoNo correspondehttp://ri.conicet.gov.ar/oai/requestdasensio@conicet.gov.ar; lcarlino@conicet.gov.arArgentinaNo correspondeNo correspondeNo correspondeopendoar:34982025-09-29 09:49:07.279CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicasfalse
dc.title.none.fl_str_mv Determination of Thiamine in Wheat Flours Using a Validated Isocratic HPLC-Fluorescence Method Previously Optimized by Box-Behnken Design
title Determination of Thiamine in Wheat Flours Using a Validated Isocratic HPLC-Fluorescence Method Previously Optimized by Box-Behnken Design
spellingShingle Determination of Thiamine in Wheat Flours Using a Validated Isocratic HPLC-Fluorescence Method Previously Optimized by Box-Behnken Design
Michlig, Nicolás
CHROMATOGRAPHIC OPTIMIZATION
THIAMINE
THIOCHROME SOLID-PHASE EXTRACTION
title_short Determination of Thiamine in Wheat Flours Using a Validated Isocratic HPLC-Fluorescence Method Previously Optimized by Box-Behnken Design
title_full Determination of Thiamine in Wheat Flours Using a Validated Isocratic HPLC-Fluorescence Method Previously Optimized by Box-Behnken Design
title_fullStr Determination of Thiamine in Wheat Flours Using a Validated Isocratic HPLC-Fluorescence Method Previously Optimized by Box-Behnken Design
title_full_unstemmed Determination of Thiamine in Wheat Flours Using a Validated Isocratic HPLC-Fluorescence Method Previously Optimized by Box-Behnken Design
title_sort Determination of Thiamine in Wheat Flours Using a Validated Isocratic HPLC-Fluorescence Method Previously Optimized by Box-Behnken Design
dc.creator.none.fl_str_mv Michlig, Nicolás
Van de Velde, Franco
Freyre, Marcelino Ricardo
Bernardi, Cecilia
author Michlig, Nicolás
author_facet Michlig, Nicolás
Van de Velde, Franco
Freyre, Marcelino Ricardo
Bernardi, Cecilia
author_role author
author2 Van de Velde, Franco
Freyre, Marcelino Ricardo
Bernardi, Cecilia
author2_role author
author
author
dc.subject.none.fl_str_mv CHROMATOGRAPHIC OPTIMIZATION
THIAMINE
THIOCHROME SOLID-PHASE EXTRACTION
topic CHROMATOGRAPHIC OPTIMIZATION
THIAMINE
THIOCHROME SOLID-PHASE EXTRACTION
purl_subject.fl_str_mv https://purl.org/becyt/ford/1.4
https://purl.org/becyt/ford/1
dc.description.none.fl_txt_mv The main purpose of this work was to optimize and validate a new isocratic high-performance liquid chromatography method for thiamine analysis in wheat flours. Thiamine was previously derivatized into thiochrome and determined by fluorescence detection (excitation wavelength, 366 nm; emission wavelength, 435 nm). The mobile phase consisted of buffer phosphate (0.02 M) and organic modifier (methanol 88 %; acetonitrile 12 %). Optimization was done using a Box-Behnken design (three factors at three levels) where organic modifier proportion (A), varying from 20 to 90 %, mobile phase pH (B), varying from 5.8 to 7.8, and flow rate (C), varying from 0.5 to 1 mL min-1, were the studied variables. Peak width was the studied response. Optimal chromatographic conditions that minimized response were A = 90 %, B = 6.00, and C = 1 mL min-1. Using optimal conditions, thiochrome extractions with isobutanol and solid-phase extraction (SPE) employing styrene-divinylbenzene adsorbent cartridges were compared. Method validation, using thiamine standard solutions and both types of thiochrome isolation, included linearity studies, limits of detection and quantification, and calibration and analytical sensitivity quantifications. Standard addition method was employed to quantify thiamine in wheat flours. Good precision results were obtained by both extraction methods. Recoveries ranged from 63 to 65 % for isobutanol and 84 to 101 % for SPE, including sample extraction, thiamine derivatization, thiochrome purification, and chromatographic separation. Taking into account better obtained SPE recoveries, acceptable precision, and isobutanol irritant action on the eyes and skin of operator, SPE using styrene-divinylbenzene adsorbent could be chosen for routine thiamine analysis in wheat flour samples.
Fil: Michlig, Nicolás. Universidad Nacional del Litoral. Facultad de Ingeniería Química. Instituto de Tecnología de los Alimentos; Argentina
Fil: Van de Velde, Franco. Consejo Nacional de Investigaciones Científicas y Técnicas; Argentina. Universidad Nacional del Litoral. Facultad de Ingeniería Química. Instituto de Tecnología de los Alimentos; Argentina
Fil: Freyre, Marcelino Ricardo. Universidad Nacional del Litoral. Facultad de Ingeniería Química. Instituto de Tecnología de los Alimentos; Argentina
Fil: Bernardi, Cecilia. Universidad Nacional del Litoral. Facultad de Ingeniería Química. Instituto de Tecnología de los Alimentos; Argentina
description The main purpose of this work was to optimize and validate a new isocratic high-performance liquid chromatography method for thiamine analysis in wheat flours. Thiamine was previously derivatized into thiochrome and determined by fluorescence detection (excitation wavelength, 366 nm; emission wavelength, 435 nm). The mobile phase consisted of buffer phosphate (0.02 M) and organic modifier (methanol 88 %; acetonitrile 12 %). Optimization was done using a Box-Behnken design (three factors at three levels) where organic modifier proportion (A), varying from 20 to 90 %, mobile phase pH (B), varying from 5.8 to 7.8, and flow rate (C), varying from 0.5 to 1 mL min-1, were the studied variables. Peak width was the studied response. Optimal chromatographic conditions that minimized response were A = 90 %, B = 6.00, and C = 1 mL min-1. Using optimal conditions, thiochrome extractions with isobutanol and solid-phase extraction (SPE) employing styrene-divinylbenzene adsorbent cartridges were compared. Method validation, using thiamine standard solutions and both types of thiochrome isolation, included linearity studies, limits of detection and quantification, and calibration and analytical sensitivity quantifications. Standard addition method was employed to quantify thiamine in wheat flours. Good precision results were obtained by both extraction methods. Recoveries ranged from 63 to 65 % for isobutanol and 84 to 101 % for SPE, including sample extraction, thiamine derivatization, thiochrome purification, and chromatographic separation. Taking into account better obtained SPE recoveries, acceptable precision, and isobutanol irritant action on the eyes and skin of operator, SPE using styrene-divinylbenzene adsorbent could be chosen for routine thiamine analysis in wheat flour samples.
publishDate 2014
dc.date.none.fl_str_mv 2014-04
dc.type.none.fl_str_mv info:eu-repo/semantics/article
info:eu-repo/semantics/publishedVersion
http://purl.org/coar/resource_type/c_6501
info:ar-repo/semantics/articulo
format article
status_str publishedVersion
dc.identifier.none.fl_str_mv http://hdl.handle.net/11336/92743
Michlig, Nicolás; Van de Velde, Franco; Freyre, Marcelino Ricardo; Bernardi, Cecilia; Determination of Thiamine in Wheat Flours Using a Validated Isocratic HPLC-Fluorescence Method Previously Optimized by Box-Behnken Design; Springer; Food Analytical Methods; 7; 4; 4-2014; 828-835
1936-9751
CONICET Digital
CONICET
url http://hdl.handle.net/11336/92743
identifier_str_mv Michlig, Nicolás; Van de Velde, Franco; Freyre, Marcelino Ricardo; Bernardi, Cecilia; Determination of Thiamine in Wheat Flours Using a Validated Isocratic HPLC-Fluorescence Method Previously Optimized by Box-Behnken Design; Springer; Food Analytical Methods; 7; 4; 4-2014; 828-835
1936-9751
CONICET Digital
CONICET
dc.language.none.fl_str_mv eng
language eng
dc.relation.none.fl_str_mv info:eu-repo/semantics/altIdentifier/url/http://link.springer.com/article/10.1007%2Fs12161-013-9688-3
info:eu-repo/semantics/altIdentifier/doi/10.1007/s12161-013-9688-3
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
https://creativecommons.org/licenses/by-nc-sa/2.5/ar/
eu_rights_str_mv openAccess
rights_invalid_str_mv https://creativecommons.org/licenses/by-nc-sa/2.5/ar/
dc.format.none.fl_str_mv application/pdf
application/pdf
dc.publisher.none.fl_str_mv Springer
publisher.none.fl_str_mv Springer
dc.source.none.fl_str_mv reponame:CONICET Digital (CONICET)
instname:Consejo Nacional de Investigaciones Científicas y Técnicas
reponame_str CONICET Digital (CONICET)
collection CONICET Digital (CONICET)
instname_str Consejo Nacional de Investigaciones Científicas y Técnicas
repository.name.fl_str_mv CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicas
repository.mail.fl_str_mv dasensio@conicet.gov.ar; lcarlino@conicet.gov.ar
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score 13.070432

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