A Tiered Analytical Approach for Investigating Poor Quality Emergency Contraceptives

Autores
Monge, Maria Eugenia; Dwivedi, Prabha; Zhou, Manshui; Payne, Michael; Harris, Chris; House, Blaine; Juggins, Yvonne; Cizmarik, Peter; Newton, Paul N.; Fernández, Facundo M.; Jenkins, David
Año de publicación
2014
Idioma
inglés
Tipo de recurso
artículo
Estado
versión publicada
Descripción
Reproductive health has been deleteriously affected by poor quality medicines. Emergency contraceptive pills (ECPs) are an important birth control method that women can use after unprotected coitus for reducing the risk of pregnancy. In response to the detection of poor quality ECPs commercially available in the Peruvian market we developed a tiered multiplatform analytical strategy. In a survey to assess ECP medicine quality in Peru, 7 out of 25 different batches showed inadequate release of levonorgestrel by dissolution testing or improper amounts of active ingredient. One batch was found to contain a wrong active ingredient, with no detectable levonorgestrel. By combining ultrahigh performance liquid chromatography-ion mobility spectrometry-mass spectrometry (UHPLC-IMS-MS) and direct analysis in real time MS (DARTMS) the unknown compound was identified as the antibiotic sulfamethoxazole. Quantitation by UHPLC-triple quadrupole tandem MS (QqQ-MS/MS) indicated that the wrong ingredient was present in the ECP sample at levels which could have significant physiological effects. Further chemical characterization of the poor quality ECP samples included the identification of the excipients by 2D Diffusion-Ordered Nuclear Magnetic Resonance Spectroscopy (DOSY 1H NMR) indicating the presence of lactose and magnesium stearate.
Fil: Monge, Maria Eugenia. Consejo Nacional de Investigaciones Científicas y Técnicas. Oficina de Coordinación Administrativa Parque Centenario. Centro de Investigaciones en Bionanociencias "Elizabeth Jares Erijman"; Argentina. Georgia Institute of Technology. School of Chemistry and Biochemistry; Estados Unidos
Fil: Dwivedi, Prabha. Georgia Institute of Technology. School of Chemistry and Biochemistry; Estados Unidos
Fil: Zhou, Manshui. Georgia Institute of Technology. School of Chemistry and Biochemistry; Estados Unidos
Fil: Payne, Michael. Product Quality and Compliance; Estados Unidos
Fil: Harris, Chris. Product Quality and Compliance; Estados Unidos
Fil: House, Blaine. Product Quality and Compliance; Estados Unidos
Fil: Juggins, Yvonne. Product Quality and Compliance; Estados Unidos
Fil: Cizmarik, Peter. Product Quality and Compliance; Estados Unidos
Fil: Newton, Paul N.. University of Oxford. Churchill Hospital. Centre for Tropical Medicine; Reino Unido. University of Oxford. Churchill Hospital. WorldWide Antimalarial Resistance Network; Reino Unido. Mahosot Hospital. Microbiology Laboratory. Lao-Oxford-Mahosot Hospital-Wellcome Trust Research Unit; Laos
Fil: Fernández, Facundo M.. Georgia Institute of Technology. School of Chemistry and Biochemistry; Estados Unidos
Fil: Jenkins, David. Product Quality and Compliance; Estados Unidos
Materia
Mass Spectrometry
Liquid Chromatography
Ion Mobility
Nuclear Magnetic Resonance
Contraceptives
Drug quality
Levonorgestrel
Nivel de accesibilidad
acceso abierto
Condiciones de uso
https://creativecommons.org/licenses/by/2.5/ar/
Repositorio
CONICET Digital (CONICET)
Institución
Consejo Nacional de Investigaciones Científicas y Técnicas
OAI Identificador
oai:ri.conicet.gov.ar:11336/4103
Acceder
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oai_identifier_str oai:ri.conicet.gov.ar:11336/4103
network_acronym_str CONICETDig
repository_id_str 3498
network_name_str CONICET Digital (CONICET)
spelling A Tiered Analytical Approach for Investigating Poor Quality Emergency ContraceptivesMonge, Maria EugeniaDwivedi, PrabhaZhou, ManshuiPayne, MichaelHarris, ChrisHouse, BlaineJuggins, YvonneCizmarik, PeterNewton, Paul N.Fernández, Facundo M.Jenkins, DavidMass SpectrometryLiquid ChromatographyIon MobilityNuclear Magnetic ResonanceContraceptivesDrug qualityLevonorgestrelhttps://purl.org/becyt/ford/1.4https://purl.org/becyt/ford/1Reproductive health has been deleteriously affected by poor quality medicines. Emergency contraceptive pills (ECPs) are an important birth control method that women can use after unprotected coitus for reducing the risk of pregnancy. In response to the detection of poor quality ECPs commercially available in the Peruvian market we developed a tiered multiplatform analytical strategy. In a survey to assess ECP medicine quality in Peru, 7 out of 25 different batches showed inadequate release of levonorgestrel by dissolution testing or improper amounts of active ingredient. One batch was found to contain a wrong active ingredient, with no detectable levonorgestrel. By combining ultrahigh performance liquid chromatography-ion mobility spectrometry-mass spectrometry (UHPLC-IMS-MS) and direct analysis in real time MS (DARTMS) the unknown compound was identified as the antibiotic sulfamethoxazole. Quantitation by UHPLC-triple quadrupole tandem MS (QqQ-MS/MS) indicated that the wrong ingredient was present in the ECP sample at levels which could have significant physiological effects. Further chemical characterization of the poor quality ECP samples included the identification of the excipients by 2D Diffusion-Ordered Nuclear Magnetic Resonance Spectroscopy (DOSY 1H NMR) indicating the presence of lactose and magnesium stearate.Fil: Monge, Maria Eugenia. Consejo Nacional de Investigaciones Científicas y Técnicas. Oficina de Coordinación Administrativa Parque Centenario. Centro de Investigaciones en Bionanociencias "Elizabeth Jares Erijman"; Argentina. Georgia Institute of Technology. School of Chemistry and Biochemistry; Estados UnidosFil: Dwivedi, Prabha. Georgia Institute of Technology. School of Chemistry and Biochemistry; Estados UnidosFil: Zhou, Manshui. Georgia Institute of Technology. School of Chemistry and Biochemistry; Estados UnidosFil: Payne, Michael. Product Quality and Compliance; Estados UnidosFil: Harris, Chris. Product Quality and Compliance; Estados UnidosFil: House, Blaine. Product Quality and Compliance; Estados UnidosFil: Juggins, Yvonne. Product Quality and Compliance; Estados UnidosFil: Cizmarik, Peter. Product Quality and Compliance; Estados UnidosFil: Newton, Paul N.. University of Oxford. Churchill Hospital. Centre for Tropical Medicine; Reino Unido. University of Oxford. Churchill Hospital. WorldWide Antimalarial Resistance Network; Reino Unido. Mahosot Hospital. Microbiology Laboratory. Lao-Oxford-Mahosot Hospital-Wellcome Trust Research Unit; LaosFil: Fernández, Facundo M.. Georgia Institute of Technology. School of Chemistry and Biochemistry; Estados UnidosFil: Jenkins, David. Product Quality and Compliance; Estados UnidosPublic Library of Science2014-04info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionhttp://purl.org/coar/resource_type/c_6501info:ar-repo/semantics/articuloapplication/pdfapplication/pdfhttp://hdl.handle.net/11336/4103Monge, Maria Eugenia; Dwivedi, Prabha; Zhou, Manshui; Payne, Michael; Harris, Chris; et al.; A Tiered Analytical Approach for Investigating Poor Quality Emergency Contraceptives; Public Library of Science; Plos One; 9; 4; 4-2014; 1-111932-6203enginfo:eu-repo/semantics/altIdentifier/url/http://journals.plos.org/plosone/article?id=10.1371/journal.pone.0095353info:eu-repo/semantics/altIdentifier/url/http://www.ncbi.nlm.nih.gov/pmc/articles/PMC3991657/info:eu-repo/semantics/altIdentifier/doi/10.1371%2Fjournal.pone.0095353info:eu-repo/semantics/altIdentifier/issn/1932-6203info:eu-repo/semantics/openAccesshttps://creativecommons.org/licenses/by/2.5/ar/reponame:CONICET Digital (CONICET)instname:Consejo Nacional de Investigaciones Científicas y Técnicas2025-09-29T10:16:07Zoai:ri.conicet.gov.ar:11336/4103instacron: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 10:16:07.617CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicasfalse
dc.title.none.fl_str_mv A Tiered Analytical Approach for Investigating Poor Quality Emergency Contraceptives
title A Tiered Analytical Approach for Investigating Poor Quality Emergency Contraceptives
spellingShingle A Tiered Analytical Approach for Investigating Poor Quality Emergency Contraceptives
Monge, Maria Eugenia
Mass Spectrometry
Liquid Chromatography
Ion Mobility
Nuclear Magnetic Resonance
Contraceptives
Drug quality
Levonorgestrel
title_short A Tiered Analytical Approach for Investigating Poor Quality Emergency Contraceptives
title_full A Tiered Analytical Approach for Investigating Poor Quality Emergency Contraceptives
title_fullStr A Tiered Analytical Approach for Investigating Poor Quality Emergency Contraceptives
title_full_unstemmed A Tiered Analytical Approach for Investigating Poor Quality Emergency Contraceptives
title_sort A Tiered Analytical Approach for Investigating Poor Quality Emergency Contraceptives
dc.creator.none.fl_str_mv Monge, Maria Eugenia
Dwivedi, Prabha
Zhou, Manshui
Payne, Michael
Harris, Chris
House, Blaine
Juggins, Yvonne
Cizmarik, Peter
Newton, Paul N.
Fernández, Facundo M.
Jenkins, David
author Monge, Maria Eugenia
author_facet Monge, Maria Eugenia
Dwivedi, Prabha
Zhou, Manshui
Payne, Michael
Harris, Chris
House, Blaine
Juggins, Yvonne
Cizmarik, Peter
Newton, Paul N.
Fernández, Facundo M.
Jenkins, David
author_role author
author2 Dwivedi, Prabha
Zhou, Manshui
Payne, Michael
Harris, Chris
House, Blaine
Juggins, Yvonne
Cizmarik, Peter
Newton, Paul N.
Fernández, Facundo M.
Jenkins, David
author2_role author
author
author
author
author
author
author
author
author
author
dc.subject.none.fl_str_mv Mass Spectrometry
Liquid Chromatography
Ion Mobility
Nuclear Magnetic Resonance
Contraceptives
Drug quality
Levonorgestrel
topic Mass Spectrometry
Liquid Chromatography
Ion Mobility
Nuclear Magnetic Resonance
Contraceptives
Drug quality
Levonorgestrel
purl_subject.fl_str_mv https://purl.org/becyt/ford/1.4
https://purl.org/becyt/ford/1
dc.description.none.fl_txt_mv Reproductive health has been deleteriously affected by poor quality medicines. Emergency contraceptive pills (ECPs) are an important birth control method that women can use after unprotected coitus for reducing the risk of pregnancy. In response to the detection of poor quality ECPs commercially available in the Peruvian market we developed a tiered multiplatform analytical strategy. In a survey to assess ECP medicine quality in Peru, 7 out of 25 different batches showed inadequate release of levonorgestrel by dissolution testing or improper amounts of active ingredient. One batch was found to contain a wrong active ingredient, with no detectable levonorgestrel. By combining ultrahigh performance liquid chromatography-ion mobility spectrometry-mass spectrometry (UHPLC-IMS-MS) and direct analysis in real time MS (DARTMS) the unknown compound was identified as the antibiotic sulfamethoxazole. Quantitation by UHPLC-triple quadrupole tandem MS (QqQ-MS/MS) indicated that the wrong ingredient was present in the ECP sample at levels which could have significant physiological effects. Further chemical characterization of the poor quality ECP samples included the identification of the excipients by 2D Diffusion-Ordered Nuclear Magnetic Resonance Spectroscopy (DOSY 1H NMR) indicating the presence of lactose and magnesium stearate.
Fil: Monge, Maria Eugenia. Consejo Nacional de Investigaciones Científicas y Técnicas. Oficina de Coordinación Administrativa Parque Centenario. Centro de Investigaciones en Bionanociencias "Elizabeth Jares Erijman"; Argentina. Georgia Institute of Technology. School of Chemistry and Biochemistry; Estados Unidos
Fil: Dwivedi, Prabha. Georgia Institute of Technology. School of Chemistry and Biochemistry; Estados Unidos
Fil: Zhou, Manshui. Georgia Institute of Technology. School of Chemistry and Biochemistry; Estados Unidos
Fil: Payne, Michael. Product Quality and Compliance; Estados Unidos
Fil: Harris, Chris. Product Quality and Compliance; Estados Unidos
Fil: House, Blaine. Product Quality and Compliance; Estados Unidos
Fil: Juggins, Yvonne. Product Quality and Compliance; Estados Unidos
Fil: Cizmarik, Peter. Product Quality and Compliance; Estados Unidos
Fil: Newton, Paul N.. University of Oxford. Churchill Hospital. Centre for Tropical Medicine; Reino Unido. University of Oxford. Churchill Hospital. WorldWide Antimalarial Resistance Network; Reino Unido. Mahosot Hospital. Microbiology Laboratory. Lao-Oxford-Mahosot Hospital-Wellcome Trust Research Unit; Laos
Fil: Fernández, Facundo M.. Georgia Institute of Technology. School of Chemistry and Biochemistry; Estados Unidos
Fil: Jenkins, David. Product Quality and Compliance; Estados Unidos
description Reproductive health has been deleteriously affected by poor quality medicines. Emergency contraceptive pills (ECPs) are an important birth control method that women can use after unprotected coitus for reducing the risk of pregnancy. In response to the detection of poor quality ECPs commercially available in the Peruvian market we developed a tiered multiplatform analytical strategy. In a survey to assess ECP medicine quality in Peru, 7 out of 25 different batches showed inadequate release of levonorgestrel by dissolution testing or improper amounts of active ingredient. One batch was found to contain a wrong active ingredient, with no detectable levonorgestrel. By combining ultrahigh performance liquid chromatography-ion mobility spectrometry-mass spectrometry (UHPLC-IMS-MS) and direct analysis in real time MS (DARTMS) the unknown compound was identified as the antibiotic sulfamethoxazole. Quantitation by UHPLC-triple quadrupole tandem MS (QqQ-MS/MS) indicated that the wrong ingredient was present in the ECP sample at levels which could have significant physiological effects. Further chemical characterization of the poor quality ECP samples included the identification of the excipients by 2D Diffusion-Ordered Nuclear Magnetic Resonance Spectroscopy (DOSY 1H NMR) indicating the presence of lactose and magnesium stearate.
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/11336/4103
Monge, Maria Eugenia; Dwivedi, Prabha; Zhou, Manshui; Payne, Michael; Harris, Chris; et al.; A Tiered Analytical Approach for Investigating Poor Quality Emergency Contraceptives; Public Library of Science; Plos One; 9; 4; 4-2014; 1-11
1932-6203
url http://hdl.handle.net/11336/4103
identifier_str_mv Monge, Maria Eugenia; Dwivedi, Prabha; Zhou, Manshui; Payne, Michael; Harris, Chris; et al.; A Tiered Analytical Approach for Investigating Poor Quality Emergency Contraceptives; Public Library of Science; Plos One; 9; 4; 4-2014; 1-11
1932-6203
dc.language.none.fl_str_mv eng
language eng
dc.relation.none.fl_str_mv info:eu-repo/semantics/altIdentifier/url/http://journals.plos.org/plosone/article?id=10.1371/journal.pone.0095353
info:eu-repo/semantics/altIdentifier/url/http://www.ncbi.nlm.nih.gov/pmc/articles/PMC3991657/
info:eu-repo/semantics/altIdentifier/doi/10.1371%2Fjournal.pone.0095353
info:eu-repo/semantics/altIdentifier/issn/1932-6203
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
https://creativecommons.org/licenses/by/2.5/ar/
eu_rights_str_mv openAccess
rights_invalid_str_mv https://creativecommons.org/licenses/by/2.5/ar/
dc.format.none.fl_str_mv application/pdf
application/pdf
dc.publisher.none.fl_str_mv Public Library of Science
publisher.none.fl_str_mv Public Library of Science
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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