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  • Hollow-fiber liquid-phase microextraction and chiral LC-MS/MS analysis of venlafaxine and its metabolites in plasma.

Hollow-fiber liquid-phase microextraction and chiral LC-MS/MS analysis of venlafaxine and its metabolites in plasma.

Bioanalysis (2013-03-15)
Patrícia da Fonseca, Pierina Sueli Bonato
ABSTRACT

An enantioselective analytical method was developed and validated for determination of venlafaxine and its metabolites O-desmethylvenlafaxine and N-desmethylvenlafaxine in plasma samples. The method employed LC-MS/MS analysis and hollow-fiber liquid-phase microextraction (HF LPME) for sample preparation. After HF LPME optimization the following condition was established: sample volume of 4 ml, sample agitation at 1750 rpm, 20 min of extraction, 0.1 mol/l acetic acid as acceptor phase, 1-octanol as organic phase and donor phase pH adjustment to 10. Under these conditions, the method was linear over the concentration range of 5-500 ng/ml with quantification limits of 5 ng/ml. The use of HF LPME for sample preparation provided suitable recoveries, efficient clean-up and low consumption of organic solvent.

MATERIALS
Product Number
Brand
Product Description

Supelco
Venlafaxine hydrochloride solution, 1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®
Supelco
O-Desmethylvenlafaxine solution, 100 μg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®
Venlafaxine for system suitability, European Pharmacopoeia (EP) Reference Standard
Venlafaxine hydrochloride, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
1-Octanol, ≥98%, FCC, FG
Sigma-Aldrich
1-Octanol, anhydrous, ≥99%
Supelco
1-Octanol, analytical standard
Sigma-Aldrich
1-Octanol, ACS reagent, ≥99%
Sigma-Aldrich
1-Octanol, ReagentPlus®, 99%
Sigma-Aldrich
1-Octanol, suitable for HPLC, ≥99%
Sigma-Aldrich
1-Octanol, natural, ≥98%, FCC