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HPLC column-switching technique for sample preparation and fluorescence determination of propranolol in urine using fused-core columns in both dimensions.

Analytical and bioanalytical chemistry (2013-06-12)
Dalibor Satínský, Lucie Havlíková, Petr Solich
ABSTRACT

A new and fast high-performance liquid chromatography (HPLC) column-switching method using fused-core columns in both dimensions for sample preconcentration and determination of propranolol in human urine has been developed. On-line sample pretreatment and propranolol preconcentration were performed on an Ascentis Express RP-C-18 guard column (5 × 4.6 mm), particle size, 2.7 μm, with mobile phase acetonitrile/water (5:95, v/v) at a flow rate of 2.0 mL min(-1) and at a temperature of 50 °C. Valve switch from pretreatment column to analytical column was set at 4.0 min in a back-flush mode. Separation of propranolol from other endogenous urine compounds was achieved on the fused-core column Ascentis Express RP-Amide (100 × 4.6 mm), particle size, 2.7 μm, with mobile phase acetonitrile/water solution of 0.5% triethylamine, pH adjusted to 4.5 by means of glacial acetic acid (25:75, v/v), at a flow rate of 1.0 mL min(-1) and at a temperature of 50 °C. Fluorescence excitation/emission detection wavelengths were set at 229/338 nm. A volume of 1,500 μL of filtered urine sample solution was injected directly into the column-switching HPLC system. The total analysis time including on-line sample pretreatment was less than 8 min. The experimentally determined limit of detection of the method was found to be 0.015 ng mL(-1).

MATERIALS
Product Number
Brand
Product Description

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. 10 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. 7.5 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 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. 7.5 cm × 2.1 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. 10 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, 5 μm Guard Cartridge, 5 μm particle size, L × I.D. 5 mm × 2.1 mm, pkg of 3 ea
Supelco
Ascentis® Express C8, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 7.5 cm × 2.1 mm
Supelco
Ascentis® Express C8, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 10 cm × 2.1 mm
Supelco
Ascentis® Express C8, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 3 cm × 3 mm
Supelco
Ascentis® Express C8, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 5 cm × 3 mm
Supelco
Ascentis® Express C8, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 3 cm × 2.1 mm
Supelco
Ascentis® Express C8, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 2 cm × 2.1 mm
Supelco
Ascentis® Express C8, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 15 cm × 2.1 mm
Supelco
Ascentis® Express C8, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 10 cm × 3 mm
Supelco
Ascentis® Express C8, 2 μm UHPLC Column, 2 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. 15 cm × 4.6 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 HPLC Column, 5 μm particle size, L × I.D. 7.5 cm × 4.6 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4.6 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 C8, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 7.5 cm × 3 mm
Supelco
Ascentis® Express C8, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 15 cm × 3 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 7.5 cm × 2.1 mm
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, 5 μm Guard Cartridge, 5 μm particle size, L × I.D. 5 mm × 4.6 mm, pkg of 3 ea