Multiple responses optimization in the development of a headspace gas chromatography method for the determination of residual solvents in pharmaceuticals

Autores
Teglia, Carla Mariela; Montemurro, Milagros; de Zan, María Mercedes; Cámara, María Silvia
Año de publicación
2015
Idioma
inglés
Tipo de recurso
artículo
Estado
versión publicada
Descripción
An efficient generic static headspace gas chromatography (HSGC) method was developed, optimized and validated for the routine determination of several residual solvents (RS) in drug substance, using a strategy with two sets of calibration. Dimethylsulfoxide (DMSO) was selected as the sample diluent and internal standards were used to minimize signal variations due to the preparative step. A gas chromatograph from Agilent Model 6890 equipped with flame ionization detector (FID) and a DB?624 (30 m x 0.53 mm i.d., 3.00 µm film thickness) column was used. The inlet split ratio was 5:1. The influencing factors in the chromatographic separation of the analytes were determined through a fractional factorial experimental design. Significant variables: the initial temperature (IT), the final temperature (FT) of the oven and the carrier gas flow rate (F) were optimized using a central composite design. Response transformation and desirability function were applied to find out the optimal combination of the chromatographic variables to achieve an adequate resolution of the analytes and short analysis time. These conditions were: 30ºC for IT, 158ºC for FT and 1.90 mL/min for F. The method was proven to be accurate, linear in a wide range and very sensitive for the analyzed solvents, through a comprehensive validation made according ICH guidelines.
Fil: Teglia, Carla Mariela. Universidad Nacional del Litoral. Facultad de Bioquímica y Ciencias Biológicas. Departamento de Química. Cátedra de Química Analítica; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Santa Fe; Argentina
Fil: Montemurro, Milagros. Universidad Nacional del Litoral. Facultad de Bioquímica y Ciencias Biológicas. Departamento de Química. Cátedra de Química Analítica; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Santa Fe; Argentina
Fil: de Zan, María Mercedes. Universidad Nacional del Litoral. Facultad de Bioquímica y Ciencias Biológicas. Departamento de Química. Cátedra de Química Analítica; Argentina
Fil: Cámara, María Silvia. Universidad Nacional del Litoral. Facultad de Bioquímica y Ciencias Biológicas. Departamento de Química. Cátedra de Química Analítica; Argentina
Materia
RESIDUALS
SOLVENTS
PHARMACEUTICALS
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:11336/44041
Acceder
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oai_identifier_str oai:ri.conicet.gov.ar:11336/44041
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network_name_str CONICET Digital (CONICET)
spelling Multiple responses optimization in the development of a headspace gas chromatography method for the determination of residual solvents in pharmaceuticalsTeglia, Carla MarielaMontemurro, Milagrosde Zan, María MercedesCámara, María SilviaRESIDUALSSOLVENTSPHARMACEUTICALShttps://purl.org/becyt/ford/1.4https://purl.org/becyt/ford/1An efficient generic static headspace gas chromatography (HSGC) method was developed, optimized and validated for the routine determination of several residual solvents (RS) in drug substance, using a strategy with two sets of calibration. Dimethylsulfoxide (DMSO) was selected as the sample diluent and internal standards were used to minimize signal variations due to the preparative step. A gas chromatograph from Agilent Model 6890 equipped with flame ionization detector (FID) and a DB?624 (30 m x 0.53 mm i.d., 3.00 µm film thickness) column was used. The inlet split ratio was 5:1. The influencing factors in the chromatographic separation of the analytes were determined through a fractional factorial experimental design. Significant variables: the initial temperature (IT), the final temperature (FT) of the oven and the carrier gas flow rate (F) were optimized using a central composite design. Response transformation and desirability function were applied to find out the optimal combination of the chromatographic variables to achieve an adequate resolution of the analytes and short analysis time. These conditions were: 30ºC for IT, 158ºC for FT and 1.90 mL/min for F. The method was proven to be accurate, linear in a wide range and very sensitive for the analyzed solvents, through a comprehensive validation made according ICH guidelines.Fil: Teglia, Carla Mariela. Universidad Nacional del Litoral. Facultad de Bioquímica y Ciencias Biológicas. Departamento de Química. Cátedra de Química Analítica; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Santa Fe; ArgentinaFil: Montemurro, Milagros. Universidad Nacional del Litoral. Facultad de Bioquímica y Ciencias Biológicas. Departamento de Química. Cátedra de Química Analítica; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Santa Fe; ArgentinaFil: de Zan, María Mercedes. Universidad Nacional del Litoral. Facultad de Bioquímica y Ciencias Biológicas. Departamento de Química. Cátedra de Química Analítica; ArgentinaFil: Cámara, María Silvia. Universidad Nacional del Litoral. Facultad de Bioquímica y Ciencias Biológicas. Departamento de Química. Cátedra de Química Analítica; ArgentinaElsevier2015-10info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionhttp://purl.org/coar/resource_type/c_6501info:ar-repo/semantics/articuloapplication/pdfapplication/pdfhttp://hdl.handle.net/11336/44041Teglia, Carla Mariela; Montemurro, Milagros; de Zan, María Mercedes; Cámara, María Silvia; Multiple responses optimization in the development of a headspace gas chromatography method for the determination of residual solvents in pharmaceuticals; Elsevier; Journal of Pharmaceutical Analysis; 5; 5; 10-2015; 296-3062095-1779CONICET DigitalCONICETenginfo:eu-repo/semantics/altIdentifier/doi/10.1016/j.jpha.2015.02.004info:eu-repo/semantics/altIdentifier/url/https://www.sciencedirect.com/science/article/pii/S2095177915000325info:eu-repo/semantics/openAccesshttps://creativecommons.org/licenses/by-nc-nd/2.5/ar/reponame:CONICET Digital (CONICET)instname:Consejo Nacional de Investigaciones Científicas y Técnicas2025-10-22T11:47:07Zoai:ri.conicet.gov.ar:11336/44041instacron: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:34982025-10-22 11:47:07.753CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicasfalse
dc.title.none.fl_str_mv Multiple responses optimization in the development of a headspace gas chromatography method for the determination of residual solvents in pharmaceuticals
title Multiple responses optimization in the development of a headspace gas chromatography method for the determination of residual solvents in pharmaceuticals
spellingShingle Multiple responses optimization in the development of a headspace gas chromatography method for the determination of residual solvents in pharmaceuticals
Teglia, Carla Mariela
RESIDUALS
SOLVENTS
PHARMACEUTICALS
title_short Multiple responses optimization in the development of a headspace gas chromatography method for the determination of residual solvents in pharmaceuticals
title_full Multiple responses optimization in the development of a headspace gas chromatography method for the determination of residual solvents in pharmaceuticals
title_fullStr Multiple responses optimization in the development of a headspace gas chromatography method for the determination of residual solvents in pharmaceuticals
title_full_unstemmed Multiple responses optimization in the development of a headspace gas chromatography method for the determination of residual solvents in pharmaceuticals
title_sort Multiple responses optimization in the development of a headspace gas chromatography method for the determination of residual solvents in pharmaceuticals
dc.creator.none.fl_str_mv Teglia, Carla Mariela
Montemurro, Milagros
de Zan, María Mercedes
Cámara, María Silvia
author Teglia, Carla Mariela
author_facet Teglia, Carla Mariela
Montemurro, Milagros
de Zan, María Mercedes
Cámara, María Silvia
author_role author
author2 Montemurro, Milagros
de Zan, María Mercedes
Cámara, María Silvia
author2_role author
author
author
dc.subject.none.fl_str_mv RESIDUALS
SOLVENTS
PHARMACEUTICALS
topic RESIDUALS
SOLVENTS
PHARMACEUTICALS
purl_subject.fl_str_mv https://purl.org/becyt/ford/1.4
https://purl.org/becyt/ford/1
dc.description.none.fl_txt_mv An efficient generic static headspace gas chromatography (HSGC) method was developed, optimized and validated for the routine determination of several residual solvents (RS) in drug substance, using a strategy with two sets of calibration. Dimethylsulfoxide (DMSO) was selected as the sample diluent and internal standards were used to minimize signal variations due to the preparative step. A gas chromatograph from Agilent Model 6890 equipped with flame ionization detector (FID) and a DB?624 (30 m x 0.53 mm i.d., 3.00 µm film thickness) column was used. The inlet split ratio was 5:1. The influencing factors in the chromatographic separation of the analytes were determined through a fractional factorial experimental design. Significant variables: the initial temperature (IT), the final temperature (FT) of the oven and the carrier gas flow rate (F) were optimized using a central composite design. Response transformation and desirability function were applied to find out the optimal combination of the chromatographic variables to achieve an adequate resolution of the analytes and short analysis time. These conditions were: 30ºC for IT, 158ºC for FT and 1.90 mL/min for F. The method was proven to be accurate, linear in a wide range and very sensitive for the analyzed solvents, through a comprehensive validation made according ICH guidelines.
Fil: Teglia, Carla Mariela. Universidad Nacional del Litoral. Facultad de Bioquímica y Ciencias Biológicas. Departamento de Química. Cátedra de Química Analítica; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Santa Fe; Argentina
Fil: Montemurro, Milagros. Universidad Nacional del Litoral. Facultad de Bioquímica y Ciencias Biológicas. Departamento de Química. Cátedra de Química Analítica; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Santa Fe; Argentina
Fil: de Zan, María Mercedes. Universidad Nacional del Litoral. Facultad de Bioquímica y Ciencias Biológicas. Departamento de Química. Cátedra de Química Analítica; Argentina
Fil: Cámara, María Silvia. Universidad Nacional del Litoral. Facultad de Bioquímica y Ciencias Biológicas. Departamento de Química. Cátedra de Química Analítica; Argentina
description An efficient generic static headspace gas chromatography (HSGC) method was developed, optimized and validated for the routine determination of several residual solvents (RS) in drug substance, using a strategy with two sets of calibration. Dimethylsulfoxide (DMSO) was selected as the sample diluent and internal standards were used to minimize signal variations due to the preparative step. A gas chromatograph from Agilent Model 6890 equipped with flame ionization detector (FID) and a DB?624 (30 m x 0.53 mm i.d., 3.00 µm film thickness) column was used. The inlet split ratio was 5:1. The influencing factors in the chromatographic separation of the analytes were determined through a fractional factorial experimental design. Significant variables: the initial temperature (IT), the final temperature (FT) of the oven and the carrier gas flow rate (F) were optimized using a central composite design. Response transformation and desirability function were applied to find out the optimal combination of the chromatographic variables to achieve an adequate resolution of the analytes and short analysis time. These conditions were: 30ºC for IT, 158ºC for FT and 1.90 mL/min for F. The method was proven to be accurate, linear in a wide range and very sensitive for the analyzed solvents, through a comprehensive validation made according ICH guidelines.
publishDate 2015
dc.date.none.fl_str_mv 2015-10
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/11336/44041
Teglia, Carla Mariela; Montemurro, Milagros; de Zan, María Mercedes; Cámara, María Silvia; Multiple responses optimization in the development of a headspace gas chromatography method for the determination of residual solvents in pharmaceuticals; Elsevier; Journal of Pharmaceutical Analysis; 5; 5; 10-2015; 296-306
2095-1779
CONICET Digital
CONICET
url http://hdl.handle.net/11336/44041
identifier_str_mv Teglia, Carla Mariela; Montemurro, Milagros; de Zan, María Mercedes; Cámara, María Silvia; Multiple responses optimization in the development of a headspace gas chromatography method for the determination of residual solvents in pharmaceuticals; Elsevier; Journal of Pharmaceutical Analysis; 5; 5; 10-2015; 296-306
2095-1779
CONICET Digital
CONICET
dc.language.none.fl_str_mv eng
language eng
dc.relation.none.fl_str_mv info:eu-repo/semantics/altIdentifier/doi/10.1016/j.jpha.2015.02.004
info:eu-repo/semantics/altIdentifier/url/https://www.sciencedirect.com/science/article/pii/S2095177915000325
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
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 12.982451

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