Measurement of tamsulosin in human serum by liquid chromatography-tandem mass spectrometry.
J Chromatogr B Analyt Technol Biomed Life Sci
; 930: 121-8, 2013 Jul 01.
Article
em En
| MEDLINE
| ID: mdl-23743242
ABSTRACT
A simple, sensitive and robust method to extract tamsulosin from human serum, and quantify by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed and validated and is applicable as a measure of compliance in clinical research. Tamsulosin was extracted from human serum (100µL) via liquid-liquid extraction with methyl tert-butyl ether (2mL) following dilution with 0.1M ammonium hydroxide (100µL), achieving 99.9% analyte recovery. Internal standard, d9-finasteride, was synthesised in-house. Analyte and internal standard were separated on an Ascentis(®) Express C18 (100mm×3mm, 2.7µm) column using a gradient elution with mobile phases methanol and 2mM aqueous ammonium acetate (595, v/v). Total run-time was 6min. Tamsulosin was quantified using a triple quadrupole mass spectrometer operated in multi-reaction-monitoring (MRM) mode using positive electrospray ionisation. Mass transitions monitored for quantitation were tamsulosin m/z 409â228 and d9-finasteride m/z 382â318, with the structural formulae of ions confirmed by Fourier transform ion cyclotron resonance mass spectrometry (within 10ppm). The limit of quantitation was 0.2ng/mL, and the method was validated in the linear range 0.2-50ng/mL with acceptable inter- and intra-assay precision and accuracy and stability suitable for routine laboratory practice. The method was successfully applied to samples taken from research volunteers in a clinical study of benign prostatic hyperplasia.
Texto completo:
1
Bases de dados:
MEDLINE
Assunto principal:
Sulfonamidas
/
Cromatografia Líquida
/
Espectrometria de Massas em Tandem
Tipo de estudo:
Diagnostic_studies
/
Prognostic_studies
Limite:
Adolescent
/
Adult
/
Humans
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Male
/
Middle aged
Idioma:
En
Revista:
J Chromatogr B Analyt Technol Biomed Life Sci
Assunto da revista:
ENGENHARIA BIOMEDICA
Ano de publicação:
2013
Tipo de documento:
Article
País de afiliação:
Reino Unido