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  • Liquid-chromatographic quantification compared with gas-chromatographic-mass-spectrometric determination of verapamil and norverapamil in plasma.

Liquid-chromatographic quantification compared with gas-chromatographic-mass-spectrometric determination of verapamil and norverapamil in plasma.

Clinical chemistry (1988-12-01)
P A Hynning, P Anderson, U Bondesson, L O Boréus
ABSTRACT

A high-performance liquid chromatographic (HPLC) method for determining verapamil and norverapamil in plasma is presented and compared with gas chromatography/mass spectrometry (GC-MS). The plasma samples were extracted at alkaline pH with hexane containing 2-butanol (20 mL/L) and then back-extracted into phosphate buffer (0.1 mol/L, pH 3.0). For chromatography we used a reversed-phase column (Supelcosil LC-18 DB) with a mobile phase of the phosphate buffer and acetonitrile (70/30 by vol). Fluorescence detection was used (excitation at 203 nm, emission at 320 nm). Overall analytical recovery was 85%. Standard curves were linear from 1 to 1000 micrograms/L. The detection limit was 1 microgram/L. The assays are accurate and precise. We found no interferences by those substances tested. Results by HPLC and GC-MS agreed well (r = 0.99) for both verapamil and norverapamil determinations.

MATERIALS
Product Number
Brand
Product Description

Supelco
SUPELCOSIL LC-18-S HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4.6 mm
Supelco
SUPELCOSIL LC-NH2-NP HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4.6 mm
Supelco
SUPELCOSIL LC-18-S HPLC Column, 5 μm particle size, L × I.D. 25 cm × 2.1 mm
Supelco
SUPELCOSIL LC-18-S HPLC Column, 5 μm particle size, L × I.D. 15 cm × 4.6 mm
Supelco
SUPELCOSIL LC-NH2-NP Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 4 mm
Supelco
SUPELCOSIL LC-18-DB HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4.6 mm
Supelco
SUPELCOSIL LC-18-DB HPLC Column, 3 μm particle size, L × I.D. 15 cm × 4.6 mm
Supelco
SUPELCOSIL LC-18-DB HPLC Column, 5 μm particle size, L × I.D. 5 cm × 4.6 mm
Supelco
SUPELCOSIL LC-18-DB HPLC Column, 3 μm particle size, L × I.D. 3.3 cm × 3 mm
Supelco
SUPELCOSIL LC-18-DB HPLC Column, 5 μm particle size, L × I.D. 30 cm × 4 mm
Supelco
SUPELCOSIL LC-18-DB HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4 mm
Supelco
SUPELCOSIL LC-18-DB HPLC Column, 3 μm particle size, L × I.D. 15 cm × 3 mm
Supelco
SUPELCOSIL LC-18-DB HPLC Column, 3 μm particle size, L × I.D. 7.5 cm × 4.6 mm
Supelco
SUPELCOSIL LC-18 Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 3 mm
Supelco
SUPELCOSIL LC-18-DB HPLC Column, 3 μm particle size, L × I.D. 3.3 cm × 4.6 mm
Supelco
SUPELCOSIL LC-18-DB HPLC Column, 5 μm particle size, L × I.D. 15 cm × 4.6 mm
Supelco
SUPELCOSIL LC-18 Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 4 mm
Supelco
SUPELCOSIL LC-18-DB Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 4 mm
Supelco
SUPELCOSIL LC-18-DB Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 4 mm
Supelco
SUPELCOSIL LC-18 Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 4 mm
Supelco
SUPELCOSIL LC-18-DB Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 2.1 mm
Supelco
SUPELCOSIL LC-18 Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 2.1 mm