Your browser doesn't support javascript.
loading
Mostrar: 20 | 50 | 100
Resultados 1 - 3 de 3
Filtrar
Mais filtros










Base de dados
Intervalo de ano de publicação
1.
Shokuhin Eiseigaku Zasshi ; 60(4): 96-107, 2019.
Artigo em Japonês | MEDLINE | ID: mdl-31474657

RESUMO

LC/Tribrid Orbitrap was developed to determine phosphodiesterase-5 (PDE-5) inhibitors and their analogs as adulterants in dietary supplements. High-resolution MS/MS and MS3 spectra of PDE-5 inhibitors and their analogs were obtained by LC/Tribrid Orbitrap using both higher-energy collisional dissociation and collision-induced dissociation. We investigated dietary supplements that claim to enhance men's sexual performance, and detected PDE-5 inhibitors and their analogs. We also estimated the structures of the PDE-5 inhibitor analogs and the impurities of PDE-5 inhibitors and their analogs in the dietary supplements.


Assuntos
Suplementos Nutricionais/análise , Inibidores da Fosfodiesterase 5/análise , Espectrometria de Massas em Tandem , Cromatografia Líquida , Nucleotídeo Cíclico Fosfodiesterase do Tipo 5
2.
J AOAC Int ; 95(4): 1048-52, 2012.
Artigo em Inglês | MEDLINE | ID: mdl-22970570

RESUMO

A sildenafil-related compound was detected in a dietary supplement marketed as an aphrodisiac. The compound was detected during analysis of the dietary supplement using LC-UV and LC/electrospray ionization-MS. The structure of the compound was established using high resolution MS, NMR spectrometry, and X-ray crystal structure analysis. The compound was identified as 5-(5-((3,5-dimethylpiperazin-1-yl)sulfonyl)-2-ethoxyphenyl)-l-methyl-7-((1-methyl-4-nitro-1H-imidazol-5-yl)thio)-3-propyl-1H-pyrazolo[4,3-d] pyrimidine. Based on this structure, the compound was named nitroprodenafil. The dietary supplement was found to contain 90 mg nitroprodenafil/capsule. This article describes the structural characterization of a new sildenafil-related compound. The compound was detected during analysis of a dietary supplement using LC-UV and LC/electrospray ionization (ESI)-MS. The structure was established using high resolution MS (HRMS), NMR spectrometry, and X-ray crystal structure analysis. The structures of methisosildenafil, thiomethisosildenafil, and this new analog, named nitroprodenafil (21), are shown in Figure 1. In the Demizu et al. report, the compound is named mutaprodenafil instead ofnitroprodenafil. Considering the naming right, the authors of this paper think the use of mutaprodenafil is appropriate as the compound name, although nitroprodenafil is used.


Assuntos
Cromatografia Líquida/métodos , Suplementos Nutricionais/análise , Espectrometria de Massas/métodos , Piperazinas/análise , Sulfonas/análise , Cápsulas , Técnicas de Química Analítica/métodos , Cristalografia por Raios X/métodos , Contaminação de Medicamentos , Espectroscopia de Ressonância Magnética/métodos , Modelos Químicos , Piperazinas/química , Purinas/análise , Purinas/química , Reprodutibilidade dos Testes , Citrato de Sildenafila , Espectrometria de Massas por Ionização por Electrospray/métodos , Sulfonas/química , Raios Ultravioleta
3.
J AOAC Int ; 94(6): 1770-7, 2011.
Artigo em Inglês | MEDLINE | ID: mdl-22320083

RESUMO

An analog of aildenafil, which is a potent and highly selective inhibitor of phosphodiesterase 5, was found in a dietary supplement marketed for enhancement of sexual function. The compound was isolated by silica gel column chromatography, and its structure was identified by means of 13C-NMR spectrometry, 1H-NMR spectrometry, high-resolution MS, and X-ray structure determination. The compound was identified to be sulfoaildenafil (other names: thioaildenafil, dimethyl sildenafil thione, and thiomethisosildenafil). Sulfoaildenafil is very similar to the compound thiohomosildenafil. As it is difficult to distinguish between them by LC-photodiode array detector analysis, ultra-performance LC (UPLC)/MS, ion trap LC/MS/MS (LC/IT-MS/MS), and GC/MS were performed. The mass spectra of thiohomosildenafil by UPLC/MS and LC/IT-MS/MS showed mass fragments of m/z 58, 72, and 355, and the mass spectrum by GC/MS showed mass fragments of m/z 56, 72, and 420. Some of these fragments had low intensities, but they were useful for distinguishing between the two compounds. The relationship between aildenafil (other names: dimethylsildenafil and methisosildenafil) and homosildenafil is similar to that between sulfoaildenafil and thiohomosildenafil. Therefore, these compounds were also examined.


Assuntos
Suplementos Nutricionais/análise , Piperazinas/análise , Sulfonas/análise , Cromatografia Líquida/métodos , Nucleotídeo Cíclico Fosfodiesterase do Tipo 5/análise , Cromatografia Gasosa-Espectrometria de Massas/métodos , Espectroscopia de Ressonância Magnética/métodos , Estrutura Molecular , Inibidores da Fosfodiesterase 5/análise , Espectrometria de Massas em Tandem/métodos
SELEÇÃO DE REFERÊNCIAS
DETALHE DA PESQUISA