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
- Institución
- Consejo Nacional de Investigaciones Científicas y Técnicas
- OAI Identificador
- oai:ri.conicet.gov.ar:11336/44041
Ver los metadatos del registro completo
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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 Técnicas2025-09-29T10:16:58Zoai: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:34982025-09-29 10:16:58.619CONICET 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 |
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CONICET Digital (CONICET) |
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CONICET Digital (CONICET) |
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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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1844614118377521152 |
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13.070432 |