Improvements in steroid screening in doping control with special emphasis to GC-MS analytical conditions and method validation
Autor(a) principal: | |
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Data de Publicação: | 2006 |
Outros Autores: | , |
Tipo de documento: | Artigo |
Idioma: | eng |
Título da fonte: | Journal of the Brazilian Chemical Society (Online) |
Texto Completo: | http://old.scielo.br/scielo.php?script=sci_arttext&pid=S0103-50532006000200024 |
Resumo: | A procedure is described for the simultaneous determination of androgenic substances including steroids and beta2-agonists. The method involves analysis of hydrolized urinary anabolic compounds using liquid-liquid extraction, with subsequent conversion to trimethylsilylether derivatives for the analysis by GC-MS. Pulse split injection 1/10 of the TMS derivatives at 280 °C into the capillary column, initially maintained at 140 °C then programmed to 180 °C at 40 °C min-1, followed by 3 ºC min-1 to 230 ºC and then 40 ºC min-1 to 300 ºC, resulted in good resolution and peak shape for all compounds. The detection limits of most of the steroids were 1 ng mL-1 except for formebolone and trenbolone (25 ng mL-1). When applied to selected urine samples with evidence of bacterial degradation and metabolites from usual medications/vitamins, the method allowed rapid screening for androgens and other substances monitored in routine. The resolution was adequate to evaluate the endogenous steroid profile relevant to doping control and medical applications. |
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Improvements in steroid screening in doping control with special emphasis to GC-MS analytical conditions and method validationsteroidsanabolicdoping controlgas chromatographymass spectrometryA procedure is described for the simultaneous determination of androgenic substances including steroids and beta2-agonists. The method involves analysis of hydrolized urinary anabolic compounds using liquid-liquid extraction, with subsequent conversion to trimethylsilylether derivatives for the analysis by GC-MS. Pulse split injection 1/10 of the TMS derivatives at 280 °C into the capillary column, initially maintained at 140 °C then programmed to 180 °C at 40 °C min-1, followed by 3 ºC min-1 to 230 ºC and then 40 ºC min-1 to 300 ºC, resulted in good resolution and peak shape for all compounds. The detection limits of most of the steroids were 1 ng mL-1 except for formebolone and trenbolone (25 ng mL-1). When applied to selected urine samples with evidence of bacterial degradation and metabolites from usual medications/vitamins, the method allowed rapid screening for androgens and other substances monitored in routine. The resolution was adequate to evaluate the endogenous steroid profile relevant to doping control and medical applications.Sociedade Brasileira de Química2006-04-01info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersiontext/htmlhttp://old.scielo.br/scielo.php?script=sci_arttext&pid=S0103-50532006000200024Journal of the Brazilian Chemical Society v.17 n.2 2006reponame:Journal of the Brazilian Chemical Society (Online)instname:Sociedade Brasileira de Química (SBQ)instacron:SBQ10.1590/S0103-50532006000200024info:eu-repo/semantics/openAccessMarques,Marlice A. S.Pereira,Henrique M. G.Aquino Neto,Francisco R. deeng2006-04-17T00:00:00Zoai:scielo:S0103-50532006000200024Revistahttp://jbcs.sbq.org.brONGhttps://old.scielo.br/oai/scielo-oai.php||office@jbcs.sbq.org.br1678-47900103-5053opendoar:2006-04-17T00:00Journal of the Brazilian Chemical Society (Online) - Sociedade Brasileira de Química (SBQ)false |
dc.title.none.fl_str_mv |
Improvements in steroid screening in doping control with special emphasis to GC-MS analytical conditions and method validation |
title |
Improvements in steroid screening in doping control with special emphasis to GC-MS analytical conditions and method validation |
spellingShingle |
Improvements in steroid screening in doping control with special emphasis to GC-MS analytical conditions and method validation Marques,Marlice A. S. steroids anabolic doping control gas chromatography mass spectrometry |
title_short |
Improvements in steroid screening in doping control with special emphasis to GC-MS analytical conditions and method validation |
title_full |
Improvements in steroid screening in doping control with special emphasis to GC-MS analytical conditions and method validation |
title_fullStr |
Improvements in steroid screening in doping control with special emphasis to GC-MS analytical conditions and method validation |
title_full_unstemmed |
Improvements in steroid screening in doping control with special emphasis to GC-MS analytical conditions and method validation |
title_sort |
Improvements in steroid screening in doping control with special emphasis to GC-MS analytical conditions and method validation |
author |
Marques,Marlice A. S. |
author_facet |
Marques,Marlice A. S. Pereira,Henrique M. G. Aquino Neto,Francisco R. de |
author_role |
author |
author2 |
Pereira,Henrique M. G. Aquino Neto,Francisco R. de |
author2_role |
author author |
dc.contributor.author.fl_str_mv |
Marques,Marlice A. S. Pereira,Henrique M. G. Aquino Neto,Francisco R. de |
dc.subject.por.fl_str_mv |
steroids anabolic doping control gas chromatography mass spectrometry |
topic |
steroids anabolic doping control gas chromatography mass spectrometry |
description |
A procedure is described for the simultaneous determination of androgenic substances including steroids and beta2-agonists. The method involves analysis of hydrolized urinary anabolic compounds using liquid-liquid extraction, with subsequent conversion to trimethylsilylether derivatives for the analysis by GC-MS. Pulse split injection 1/10 of the TMS derivatives at 280 °C into the capillary column, initially maintained at 140 °C then programmed to 180 °C at 40 °C min-1, followed by 3 ºC min-1 to 230 ºC and then 40 ºC min-1 to 300 ºC, resulted in good resolution and peak shape for all compounds. The detection limits of most of the steroids were 1 ng mL-1 except for formebolone and trenbolone (25 ng mL-1). When applied to selected urine samples with evidence of bacterial degradation and metabolites from usual medications/vitamins, the method allowed rapid screening for androgens and other substances monitored in routine. The resolution was adequate to evaluate the endogenous steroid profile relevant to doping control and medical applications. |
publishDate |
2006 |
dc.date.none.fl_str_mv |
2006-04-01 |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/article |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
format |
article |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
http://old.scielo.br/scielo.php?script=sci_arttext&pid=S0103-50532006000200024 |
url |
http://old.scielo.br/scielo.php?script=sci_arttext&pid=S0103-50532006000200024 |
dc.language.iso.fl_str_mv |
eng |
language |
eng |
dc.relation.none.fl_str_mv |
10.1590/S0103-50532006000200024 |
dc.rights.driver.fl_str_mv |
info:eu-repo/semantics/openAccess |
eu_rights_str_mv |
openAccess |
dc.format.none.fl_str_mv |
text/html |
dc.publisher.none.fl_str_mv |
Sociedade Brasileira de Química |
publisher.none.fl_str_mv |
Sociedade Brasileira de Química |
dc.source.none.fl_str_mv |
Journal of the Brazilian Chemical Society v.17 n.2 2006 reponame:Journal of the Brazilian Chemical Society (Online) instname:Sociedade Brasileira de Química (SBQ) instacron:SBQ |
instname_str |
Sociedade Brasileira de Química (SBQ) |
instacron_str |
SBQ |
institution |
SBQ |
reponame_str |
Journal of the Brazilian Chemical Society (Online) |
collection |
Journal of the Brazilian Chemical Society (Online) |
repository.name.fl_str_mv |
Journal of the Brazilian Chemical Society (Online) - Sociedade Brasileira de Química (SBQ) |
repository.mail.fl_str_mv |
||office@jbcs.sbq.org.br |
_version_ |
1750318166993534976 |