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1.
Biomed Chromatogr ; 20(10): 1049-55, 2006 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-16506283

RESUMO

The combined use of a so-called internal standard and the isotope-labeled derivatization reagent for the quantification of analytes for liquid chromatography-mass spectrometry (LC/MS) was further studied. The sample solution (containing the analytes and an internal standard) was derivatized with the light form of the derivatization reagent, 7-(N,N-dimethylaminosulfonyl)-4-(aminoethyl)piperazino-2,1,3-benzoxadiazole (DBD-PZ-NH(2)) or 7-(N,N-dimethylaminosulfonyl)-4-piperazino-2,1,3-benzoxadiazole (DBD-PZ). A standard solution of the analytes (containing an internal standard) was derivatized with the isotope (d(6))-labeled derivatization reagent, DBD-PZ-NH(2) (D) or DBD-PZ (D), and served as the isotope-labeled internal standards. The peak heights of the targeted analytes derivatives in the sample solution were corrected using those of the internal standard and the heavy form derivatives of the standards, and the calibration curves were constructed. The curve bending of the calibration curves caused by the ion suppression at the ion source was suppressed and the linear dynamic ranges of the calibration curves were expanded. The derivatives of DBD-PZ-NH(2) were about 10 times more sensitively detected than those of DBD-PZ derivatives and, therefore, DBD-PZ-NH(2) might be suitable for sensitive detection.


Assuntos
Cromatografia Líquida/métodos , Espectrometria de Massas por Ionização por Electrospray/métodos , Ácidos Graxos/análise , Marcação por Isótopo/métodos , Estrutura Molecular , Oxidiazóis/química , Oxidiazóis/normas , Piperazinas/química , Piperazinas/normas , Padrões de Referência , Reprodutibilidade dos Testes , Sulfonamidas/química , Sulfonamidas/normas
2.
Biomed Chromatogr ; 20(4): 358-64, 2006 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-16167303

RESUMO

The isotope-labeled benzofurazan derivatization reagent for carboxylic acids, 7-(N,N-dimethylaminosulfonyl)-4-(aminoethyl)piperazino-2,1,3-benzoxadiazole (d6) [DBD-PZ-NH2 (D)] was synthesized. DBD-PZ-NH2 (D) was used for the accurate quantification of fatty acids by liquid chromatography/mass spectrometry (LC/MS). The standard fatty acids were derivatized with DBD-PZ-NH2 (D) to the stable isotope-labeled compounds for the fatty acids derivatives of DBD-PZ-NH2 and used for the internal standards. The obtained calibration curves for fatty acids were linear over the range 0.1-200 microM (r2 > 0.999). Fatty acids in plasma samples were determined after derivatization with DBD-PZ-NH2 and analyzed by LC/MS using standard fatty acid DBD-PZ-NH2 (D) derivatives as internal standards. Furthermore, the relative amounts of fatty acids in two plasma samples were determined after derivatization with DBD-PZ-NH2 and DBD-PZ-NH2) (D). The isotope-labeled derivatization reagent was useful for accurate quantification and the determination of relative amounts of the metabolites in biological samples having the target functional group.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Ácidos Graxos/sangue , Espectrometria de Massas/métodos , Oxidiazóis/síntese química , Piperazinas/síntese química , Animais , Calibragem , Ácidos Carboxílicos/análise , Deutério , Marcação por Isótopo/métodos , Ratos
3.
Biomed Chromatogr ; 19(10): 802-8, 2005 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-15954158

RESUMO

The derivatization regents for carboxylic acids, DAABD-AE (4-[2-(N,N-dimethylamino)ethylaminosulfonyl]7-(2-aminoethylamino)-2,1,3-benzoxadiazole), MePZBD-AE ([4-(4-N-methyl)piperazinosulfonyl]-7-(2-aminoethylamino)-2,1,3-benzoxadiazole) and APZBD-NHMe ([4-(4-N-aminoethyl)piperazinosulfonyl]-7-methylamino-2,1,3-benzoxadiazole) were developed for electrospray ionization-mass spectrometry (ESI-MS). The derivatization reaction with fatty acids was completed at 60 degrees C within 30 min. The derivatives of fatty acids were separated on a reversed-phase column and detected with ESI-MS. The detection limits attained for fatty acids were femtomol range and the calibration curves were linear over the range from 0.1 to 100 pmol (r2 > 0.992) for DAABD-AE and MePZBD-AE. DAABD-NHMe was applied to the analysis of fatty acids in rat plasma samples.


Assuntos
Benzofuranos/síntese química , Ácidos Carboxílicos/química , Cromatografia Líquida de Alta Pressão/métodos , Ácidos Graxos/sangue , Ácidos Graxos/química , Indicadores e Reagentes/síntese química , Espectrometria de Massas por Ionização por Electrospray/métodos , Animais , Benzofuranos/química , Ácidos Graxos/isolamento & purificação , Indicadores e Reagentes/química , Oxidiazóis/síntese química , Oxidiazóis/química , Ratos , Ratos Endogâmicos WKY , Sulfonamidas/síntese química , Sulfonamidas/química
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