Trace Determination of Tamoxifen in Biological Fluids Using Hollow Fiber Liquid-Phase Microextraction Followed by High-Performance Liquid Chromatography-Ultraviolet Detection

Amir Kashtiaray,Sharareh Farhadi,Hamid Reza Sobhi,Bertrand Rochat,Hadi Farahani

doi:10.4236/ajac.2011.24052

Abstract

The applicability of hollow fiber liquid-phase microextraction (HF-LPME) combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) was evaluated for the extraction and determination of tamoxifen (TAM) in biological fluids including human urine and plasma. The drug was extracted from a 15 mL aqueous sample (source phase; SP) into an organic phase impregnated in the pores of the hollow fiber (membrane phase; MP) followed by the back-extraction into a second aqueous solution (receiving phase; RP) located in the lumen of the hollow fiber. The effects of several factors such as the nature of organic solvent, compositions of SP and RP solutions, extraction time, ionic strength and stirring rate on the extraction efficiency were examined and optimized. An enrichment factor of 360 along with substantial sample clean up was obtained under the optimized conditions. The calibration curve showed linearity in the range of 1 - 500 ng?mL–1 and the limit of detection was found to be 0.5 ng?mL–1 in aqueous medium. A reasonable relative recovery (≥89%) and satisfactory intra-assay (3.7% - 4.2%, n = 3) and inter-assay (7.5% - 7.8%, n = 3) precision illustrated good performance of the analytical procedure in spiked human urine and plasma samples.

Highlights

Sample preparation has a direct impact on accuracy, precision, limits of detection and is a determining step of the analytical process, especially when traces have to be determined [1,2,3,4,5,6].The invention of solid phase microextraction (SPME) by Pawliszyn and co-workers [7], basically initiated the interest for microextraction techniques in analytical chemistry
The drug was extracted from a 15 mL aqueous sample into an organic phase impregnated in the pores of the hollow fiber followed by the back-extraction into a second aqueous solution located in the lumen of the hollow fiber
An alternative solvent-minimized sample preparation approach to complement SPME appeared in the middle-to-late 1990s [10,11,12]; liquid-phase microextraction (LPME) utilizes only a small amount of solvent for concentrating analytes from aqueous samples

Summary

Introduction

Sample preparation has a direct impact on accuracy, precision, limits of detection and is a determining step of the analytical process, especially when traces have to be determined [1,2,3,4,5,6].The invention of solid phase microextraction (SPME) by Pawliszyn and co-workers [7], basically initiated the interest for microextraction techniques in analytical chemistry. SPME satisfies most of the requirements of a good sample preparation technique, including simplicity of use, automation, and low consumption of materials [8]. An alternative solvent-minimized sample preparation approach to complement SPME appeared in the middle-to-late 1990s [10,11,12]; liquid-phase microextraction (LPME) utilizes only a small amount of solvent (low microliter range) for concentrating analytes from aqueous samples. It is a miniaturized format of liquid-liquid extraction (LLE) and overcomes many of its disadvantages as well as some of those of SPME (e.g. non-dependence on a commercial supplier and sample carryover). The applications of LPME in environmental and biological analysis have been described in several papers [14,15,16,17,18]

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