A dynamic thermal ATR-FTIR/chemometric approach to the analysis of polymorphic interconversions. Cimetidine as a model drug

Autores
Calvo, Natalia Lorena; Maggio, Ruben Mariano; Kaufman, Teodoro Saul
Año de publicación
2014
Idioma
inglés
Tipo de recurso
artículo
Estado
versión publicada
Descripción
Crystal polymorphism of active ingredients is relevant to the pharmaceutical industry, since polymorphic changes taking place during manufacture or storage of pharmaceutical formulations can affect critical properties of the products. Cimetidine (CIM) has several relevant solid state forms, including four polymorphs (A, B, C and D), an amorphous form (AM) and a monohydrate (M1). Dehydration of M1 has been reported to yield mixtures of polymorphs A, B and C or just a single form. Standards of the solid forms of CIM were prepared and unequivocally characterized by FTIR spectroscopy, digital microscopy, differential scanning calorimetry and solid state 13C NMR spectroscopy. Multivariate curve resolution with alternating least squares (MCR-ALS) was coupled to variable temperature attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) to dynamically characterize the behavior of form M1 of CIM over a temperature range from ambient to 160 °C, without sample pretreatment. MCR-ALS analysis of ATR-FTIR spectra obtained from the tested solid under variable temperature conditions unveiled the pure spectra of the species involved in the polymorphic transitions. This allowed the simultaneous observation of thermochemical and thermophysical events associated to the changes involved in the solid forms, enabling their unequivocal identification and improving the understanding of their thermal behavior. It was demonstrated that under the experimental conditions, dehydration of M1 initially results in the formation of polymorph B; after melting and upon cooling, the latter yields an amorphous solid (AM). It was concluded that the ATR-FTIR/MCR association is a promising and useful technique for monitoring solid-state phase transformations.
Fil: Calvo, Natalia Lorena. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Rosario. Instituto de Química Rosario; Argentina
Fil: Maggio, Ruben Mariano. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Rosario. Instituto de Química Rosario; Argentina
Fil: Kaufman, Teodoro Saul. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Rosario. Instituto de Química Rosario; Argentina
Materia
Cimetidine
Chemometrics
Ftir
Nivel de accesibilidad
acceso abierto
Condiciones de uso
https://creativecommons.org/licenses/by-nc-nd/2.5/ar/
Repositorio
CONICET Digital (CONICET)
Institución
Consejo Nacional de Investigaciones Científicas y Técnicas
OAI Identificador
oai:ri.conicet.gov.ar:11336/5997
Acceder
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network_acronym_str CONICETDig
repository_id_str 3498
network_name_str CONICET Digital (CONICET)
spelling A dynamic thermal ATR-FTIR/chemometric approach to the analysis of polymorphic interconversions. Cimetidine as a model drugCalvo, Natalia LorenaMaggio, Ruben MarianoKaufman, Teodoro SaulCimetidineChemometricsFtirhttps://purl.org/becyt/ford/1.4https://purl.org/becyt/ford/1Crystal polymorphism of active ingredients is relevant to the pharmaceutical industry, since polymorphic changes taking place during manufacture or storage of pharmaceutical formulations can affect critical properties of the products. Cimetidine (CIM) has several relevant solid state forms, including four polymorphs (A, B, C and D), an amorphous form (AM) and a monohydrate (M1). Dehydration of M1 has been reported to yield mixtures of polymorphs A, B and C or just a single form. Standards of the solid forms of CIM were prepared and unequivocally characterized by FTIR spectroscopy, digital microscopy, differential scanning calorimetry and solid state 13C NMR spectroscopy. Multivariate curve resolution with alternating least squares (MCR-ALS) was coupled to variable temperature attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) to dynamically characterize the behavior of form M1 of CIM over a temperature range from ambient to 160 °C, without sample pretreatment. MCR-ALS analysis of ATR-FTIR spectra obtained from the tested solid under variable temperature conditions unveiled the pure spectra of the species involved in the polymorphic transitions. This allowed the simultaneous observation of thermochemical and thermophysical events associated to the changes involved in the solid forms, enabling their unequivocal identification and improving the understanding of their thermal behavior. It was demonstrated that under the experimental conditions, dehydration of M1 initially results in the formation of polymorph B; after melting and upon cooling, the latter yields an amorphous solid (AM). It was concluded that the ATR-FTIR/MCR association is a promising and useful technique for monitoring solid-state phase transformations.Fil: Calvo, Natalia Lorena. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Rosario. Instituto de Química Rosario; ArgentinaFil: Maggio, Ruben Mariano. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Rosario. Instituto de Química Rosario; ArgentinaFil: Kaufman, Teodoro Saul. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Rosario. Instituto de Química Rosario; ArgentinaElsevier2014-04info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionhttp://purl.org/coar/resource_type/c_6501info:ar-repo/semantics/articuloapplication/pdfapplication/pdfapplication/pdfhttp://hdl.handle.net/11336/5997Calvo, Natalia Lorena; Maggio, Ruben Mariano; Kaufman, Teodoro Saul; A dynamic thermal ATR-FTIR/chemometric approach to the analysis of polymorphic interconversions. Cimetidine as a model drug; Elsevier; Journal of Pharmaceutical and Biomedical Analysis; 92; 4-2014; 90-970731-7085enginfo:eu-repo/semantics/altIdentifier/url/http://www.sciencedirect.com/science/article/pii/S0731708513006213info:eu-repo/semantics/altIdentifier/doi/info:eu-repo/semantics/altIdentifier/doi/10.1016/j.jpba.2013.12.036info:eu-repo/semantics/openAccesshttps://creativecommons.org/licenses/by-nc-nd/2.5/ar/reponame:CONICET Digital (CONICET)instname:Consejo Nacional de Investigaciones Científicas y Técnicas2025-09-03T10:08:25Zoai:ri.conicet.gov.ar:11336/5997instacron: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:34982025-09-03 10:08:25.555CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicasfalse
dc.title.none.fl_str_mv A dynamic thermal ATR-FTIR/chemometric approach to the analysis of polymorphic interconversions. Cimetidine as a model drug
title A dynamic thermal ATR-FTIR/chemometric approach to the analysis of polymorphic interconversions. Cimetidine as a model drug
spellingShingle A dynamic thermal ATR-FTIR/chemometric approach to the analysis of polymorphic interconversions. Cimetidine as a model drug
Calvo, Natalia Lorena
Cimetidine
Chemometrics
Ftir
title_short A dynamic thermal ATR-FTIR/chemometric approach to the analysis of polymorphic interconversions. Cimetidine as a model drug
title_full A dynamic thermal ATR-FTIR/chemometric approach to the analysis of polymorphic interconversions. Cimetidine as a model drug
title_fullStr A dynamic thermal ATR-FTIR/chemometric approach to the analysis of polymorphic interconversions. Cimetidine as a model drug
title_full_unstemmed A dynamic thermal ATR-FTIR/chemometric approach to the analysis of polymorphic interconversions. Cimetidine as a model drug
title_sort A dynamic thermal ATR-FTIR/chemometric approach to the analysis of polymorphic interconversions. Cimetidine as a model drug
dc.creator.none.fl_str_mv Calvo, Natalia Lorena
Maggio, Ruben Mariano
Kaufman, Teodoro Saul
author Calvo, Natalia Lorena
author_facet Calvo, Natalia Lorena
Maggio, Ruben Mariano
Kaufman, Teodoro Saul
author_role author
author2 Maggio, Ruben Mariano
Kaufman, Teodoro Saul
author2_role author
author
dc.subject.none.fl_str_mv Cimetidine
Chemometrics
Ftir
topic Cimetidine
Chemometrics
Ftir
purl_subject.fl_str_mv https://purl.org/becyt/ford/1.4
https://purl.org/becyt/ford/1
dc.description.none.fl_txt_mv Crystal polymorphism of active ingredients is relevant to the pharmaceutical industry, since polymorphic changes taking place during manufacture or storage of pharmaceutical formulations can affect critical properties of the products. Cimetidine (CIM) has several relevant solid state forms, including four polymorphs (A, B, C and D), an amorphous form (AM) and a monohydrate (M1). Dehydration of M1 has been reported to yield mixtures of polymorphs A, B and C or just a single form. Standards of the solid forms of CIM were prepared and unequivocally characterized by FTIR spectroscopy, digital microscopy, differential scanning calorimetry and solid state 13C NMR spectroscopy. Multivariate curve resolution with alternating least squares (MCR-ALS) was coupled to variable temperature attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) to dynamically characterize the behavior of form M1 of CIM over a temperature range from ambient to 160 °C, without sample pretreatment. MCR-ALS analysis of ATR-FTIR spectra obtained from the tested solid under variable temperature conditions unveiled the pure spectra of the species involved in the polymorphic transitions. This allowed the simultaneous observation of thermochemical and thermophysical events associated to the changes involved in the solid forms, enabling their unequivocal identification and improving the understanding of their thermal behavior. It was demonstrated that under the experimental conditions, dehydration of M1 initially results in the formation of polymorph B; after melting and upon cooling, the latter yields an amorphous solid (AM). It was concluded that the ATR-FTIR/MCR association is a promising and useful technique for monitoring solid-state phase transformations.
Fil: Calvo, Natalia Lorena. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Rosario. Instituto de Química Rosario; Argentina
Fil: Maggio, Ruben Mariano. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Rosario. Instituto de Química Rosario; Argentina
Fil: Kaufman, Teodoro Saul. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Rosario. Instituto de Química Rosario; Argentina
description Crystal polymorphism of active ingredients is relevant to the pharmaceutical industry, since polymorphic changes taking place during manufacture or storage of pharmaceutical formulations can affect critical properties of the products. Cimetidine (CIM) has several relevant solid state forms, including four polymorphs (A, B, C and D), an amorphous form (AM) and a monohydrate (M1). Dehydration of M1 has been reported to yield mixtures of polymorphs A, B and C or just a single form. Standards of the solid forms of CIM were prepared and unequivocally characterized by FTIR spectroscopy, digital microscopy, differential scanning calorimetry and solid state 13C NMR spectroscopy. Multivariate curve resolution with alternating least squares (MCR-ALS) was coupled to variable temperature attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) to dynamically characterize the behavior of form M1 of CIM over a temperature range from ambient to 160 °C, without sample pretreatment. MCR-ALS analysis of ATR-FTIR spectra obtained from the tested solid under variable temperature conditions unveiled the pure spectra of the species involved in the polymorphic transitions. This allowed the simultaneous observation of thermochemical and thermophysical events associated to the changes involved in the solid forms, enabling their unequivocal identification and improving the understanding of their thermal behavior. It was demonstrated that under the experimental conditions, dehydration of M1 initially results in the formation of polymorph B; after melting and upon cooling, the latter yields an amorphous solid (AM). It was concluded that the ATR-FTIR/MCR association is a promising and useful technique for monitoring solid-state phase transformations.
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/11336/5997
Calvo, Natalia Lorena; Maggio, Ruben Mariano; Kaufman, Teodoro Saul; A dynamic thermal ATR-FTIR/chemometric approach to the analysis of polymorphic interconversions. Cimetidine as a model drug; Elsevier; Journal of Pharmaceutical and Biomedical Analysis; 92; 4-2014; 90-97
0731-7085
url http://hdl.handle.net/11336/5997
identifier_str_mv Calvo, Natalia Lorena; Maggio, Ruben Mariano; Kaufman, Teodoro Saul; A dynamic thermal ATR-FTIR/chemometric approach to the analysis of polymorphic interconversions. Cimetidine as a model drug; Elsevier; Journal of Pharmaceutical and Biomedical Analysis; 92; 4-2014; 90-97
0731-7085
dc.language.none.fl_str_mv eng
language eng
dc.relation.none.fl_str_mv info:eu-repo/semantics/altIdentifier/url/http://www.sciencedirect.com/science/article/pii/S0731708513006213
info:eu-repo/semantics/altIdentifier/doi/
info:eu-repo/semantics/altIdentifier/doi/10.1016/j.jpba.2013.12.036
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
https://creativecommons.org/licenses/by-nc-nd/2.5/ar/
eu_rights_str_mv openAccess
rights_invalid_str_mv https://creativecommons.org/licenses/by-nc-nd/2.5/ar/
dc.format.none.fl_str_mv application/pdf
application/pdf
application/pdf
dc.publisher.none.fl_str_mv Elsevier
publisher.none.fl_str_mv Elsevier
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 13.13397

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