[PMID]: | 28939282 |
[Au] Autor: | Cuervo D; Loli C; Fernández-Álvarez M; Muñoz G; Carreras D |
[Ad] Endereço: | Laboratorio de Control del Dopaje, Agencia Española de Protección de la Salud en el Deporte, Ministerio de Educación, Cultura y Deporte, Gobierno de España, c/El Greco s/n, 28040, Madrid, Spain. Electronic address: dario.cuervo@aepsad.gob.es. |
[Ti] Título: | Determination of doping peptides via solid-phase microelution and accurate-mass quadrupole time-of-flight LC-MS. |
[So] Source: | J Chromatogr B Analyt Technol Biomed Life Sci;1065-1066:134-144, 2017 Oct 15. |
[Is] ISSN: | 1873-376X |
[Cp] País de publicação: | Netherlands |
[La] Idioma: | eng |
[Ab] Resumo: | A complete analytical protocol for the determination of 25 doping-related peptidic drugs and 3 metabolites in urine was developed by means of accurate-mass quadrupole time-of-flight (Q-TOF) LC-MS analysis following solid-phase extraction (SPE) on microplates and conventional SPE pre-treatment for initial testing and confirmation, respectively. These substances included growth hormone releasing factors, gonadotropin releasing factors and anti-diuretic hormones, with molecular weights ranging from 540 to 1320Da. Optimal experimental conditions were stablished after investigation of different parameters concerning sample preparation and instrumental analysis. Weak cation exchange SPE followed by C18 HPLC chromatography and accurate mass detection provided the required sensitivity and selectivity for all the target peptides under study. 2mg SPE on 96-well microplates can be used in combination with full scan MS detection for the initial testing, thus providing a fast, cost-effective and high-throughput protocol for the processing of a large batch of samples simultaneously. On the other hand, extraction on 30mg SPE cartridges and subsequent target MS/MS determination was the protocol of choice for confirmatory purposes. The methodology was validated in terms of selectivity, recovery, matrix effect, precision, sensitivity (limit of detection, LOD), cross contamination, carryover, robustness and stability. Recoveries ranged from 6 to 70% (microplates) and 17-95% (cartridges), with LODs from 0.1 to 1ng/mL. The suitability of the method was assessed by analyzing different spiked or excreted urines containing some of the target substances. |
[Mh] Termos MeSH primário: |
Doping nos Esportes Peptídeos/urina Extração em Fase Sólida/métodos Espectrometria de Massas em Tandem/métodos
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[Mh] Termos MeSH secundário: |
Antidiuréticos/isolamento & purificação Antidiuréticos/urina Cromatografia Líquida de Alta Pressão/métodos Hormônio Liberador de Gonadotropina/isolamento & purificação Hormônio Liberador de Gonadotropina/urina Hormônio Liberador de Hormônio do Crescimento/isolamento & purificação Hormônio Liberador de Hormônio do Crescimento/urina Seres Humanos Limite de Detecção Peptídeos/isolamento & purificação Reprodutibilidade dos Testes
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[Pt] Tipo de publicação: | JOURNAL ARTICLE |
[Nm] Nome de substância:
| 0 (Antidiuretic Agents); 0 (Peptides); 33515-09-2 (Gonadotropin-Releasing Hormone); 9034-39-3 (Growth Hormone-Releasing Hormone) |
[Em] Mês de entrada: | 1710 |
[Cu] Atualização por classe: | 171030 |
[Lr] Data última revisão:
| 171030 |
[Sb] Subgrupo de revista: | IM |
[Da] Data de entrada para processamento: | 170924 |
[St] Status: | MEDLINE |
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