Determination of doxazosin and verapamil in human serum by fast LC-MS/MS: application to document non-compliance of patients.
J Chromatogr B Analyt Technol Biomed Life Sci
; 878(30): 3167-73, 2010 Nov 15.
Article
em En
| MEDLINE
| ID: mdl-20974552
ABSTRACT
A rapid and sensitive method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) for simultaneous determination of doxazosin and verapamil in human serum has been developed. Trimipramine-d3 as an isotopic labelled internal standard was used for quantification. Serum samples were prepared by simple liquid-liquid extraction with mixture of tert butyl methyl ether and ethyl acetate (11, vv). The analytes and internal standard were separated on C18 column using an isocratic elution with 5 mM ammonium formate with 0.02% formic acid and 0.02% formic acid in acetonitrile (5545, vv) at a flow rate of 1.1 mL/min. Positive TurboIonSpray mass spectrometry was used with multiple reaction monitoring of the transitions at m/z 455.3â165.2 and 150.2 for verapamil, m/z 452.2â344.4 and 247.4 for doxazosin, m/z 298.2â103.1 for trimipramine-d3. Linearity was achieved between 1 and 500 ng/mL (R² ≥ 0.997) for both analytes. An extensive pre-study method validation was carried out in accordance with FDA guidelines. This assay was successfully applied to determine the serum concentrations of doxazosin and verapamil in suspect non-compliance patients.
Texto completo:
1
Coleções:
01-internacional
Base de dados:
MEDLINE
Assunto principal:
Verapamil
/
Cromatografia Líquida
/
Cooperação do Paciente
/
Doxazossina
/
Espectrometria de Massas em Tandem
/
Hipertensão
/
Anti-Hipertensivos
Tipo de estudo:
Evaluation_studies
Limite:
Humans
Idioma:
En
Revista:
J Chromatogr B Analyt Technol Biomed Life Sci
Ano de publicação:
2010
Tipo de documento:
Article