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  • Measurement of tamsulosin in human serum by liquid chromatography-tandem mass spectrometry.

Measurement of tamsulosin in human serum by liquid chromatography-tandem mass spectrometry.

Journal of chromatography. B, Analytical technologies in the biomedical and life sciences (2013-06-08)
Rita Upreti, Natalie Z M Homer, Gregorio Naredo, Diego F Cobice, Katherine A Hughes, Laurence H Stewart, Brian R Walker, Ruth Andrew
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 (5:95, 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 409→228 and d9-finasteride m/z 382→318, 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.

MATERIALS
Product Number
Brand
Product Description

Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 10 cm × 3 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 5 cm × 4.6 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 2 cm × 2.1 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 10 cm × 4.6 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 3 cm × 2.1 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 25 cm × 2.1 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 5 cm × 2.1 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 10 cm × 2.1 mm
Supelco
Ascentis® Express RP-Amide, 5 μm Guard Cartridge, 5 μm particle size, L × I.D. 5 mm × 3 mm, pkg of 3 ea
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 15 cm × 3 mm
Supelco
Ascentis® Express RP-Amide, 5 μm Guard Cartridge, 5 μm particle size, L × I.D. 5 mm × 2.1 mm, pkg of 3 ea
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 15 cm × 2.1 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 3 cm × 4.6 mm
Supelco
Ascentis® Express RP-Amide, 5 μm Guard Cartridge, 5 μm particle size, L × I.D. 5 mm × 4.6 mm, pkg of 3 ea
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 25 cm × 3 mm
Supelco
Ascentis® Express RP-Amide, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 5 cm × 2.1 mm
Supelco
Ascentis® Express RP-Amide, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 7.5 cm × 2.1 mm
Supelco
Ascentis® Express RP-Amide, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 10 cm × 3 mm
Supelco
Ascentis® Express RP-Amide, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 15 cm × 2.1 mm
Supelco
Ascentis® Express RP-Amide, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 10 cm × 2.1 mm
Supelco
Ascentis® Express RP-Amide, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 3 cm × 3 mm
Supelco
Ascentis® Express RP-Amide, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 5 cm × 3 mm
Supelco
Ascentis® Express RP-Amide, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 2 cm × 2.1 mm
Supelco
Ascentis® Express RP-Amide, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 15 cm × 3 mm
Supelco
Ascentis® Express RP-Amide, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 3 cm × 2.1 mm
Supelco
Ascentis® Express C18, 2 μm Guard Cartridge, 2 μm particle size, L × I.D. 5 mm × 2.1 mm, pkg of 3 ea
Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 10 cm × 3 mm
Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 5 cm × 2.1 mm
Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 25 cm × 3 mm
Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 3 cm × 4.6 mm