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Title

EXTRACTION AND DETERMINATION OF PYRIDINE DERIVATIVES IN HUMAN URINE USING ELECTROMEMBRANE EXTRACTION COUPLED TO DISPERSIVE LIQUID–LIQUID MICROEXTRACTION FOLLOWED BY GAS CHROMATOGRAPHIC ANALYSIS

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Abstract

 THERE ARE MOST OF PYRIDINE DERIVATIVES IN CIGARETTE SMOKE WHICH HAVE RELATIVELY HIGH TOXICITY. SO IT IS IMPORTANT TO DIAGNOSIS SMOKERS FOR MANY AGENCIES OR CLINICAL CENTERS. THE PRESENCE OF THESE TOXIC COMPOUNDS IN CIGARETTE SMOKE HAS BEEN RECOGNIZED AS AN IMPORTANT ISSUE FOR DEVELOPMENT OF DIFFERENT METHODS FOR THE ANALYSIS OF THESE COMPOUNDS, BUT MOST OF THESE METHODS WERE PERFORMED IN WATER AND NOT COMPLICATED MATRICES SUCH AS BIOLOGICAL FLUIDS. SAMPLE PRECONCENTRATION AND CLEANUP MUST BE CARRIED OUT IN COMPLICATED MATRICES.A LARGE NUMBER OF MODERN SAMPLE PREPARATION TECHNIQUES SUCH DISPERSIVE LIQUID-LIQUID MICROEXTRACTION (DLLME) [1] AND ELECTROMEMBRANE EXTRACTION (EME) [2] METHODS HAVE BEEN INTRODUCED. RECENTLY, YAMINI ET AL. HAVE COUPLED EME TO DLLME SO THAT THEY BENEFITED FROM HIGH CLEANUP ABILITY OF EME METHOD AS WELL AS DLLME COMPATIBILITY WITH GC INSTRUMENT [3]. IN THIS WORK, EME-DLLME IS USED FOR EXTRACTION AND DETERMINATION OF SOME OF PYRIDINE DERIVATIVES (3-MTHYLPYRIDINE, 2, 4-LUTIDINE, QUINOLINE AND 4-DIMETHYLAMINOPYRIDINE) IN URINE SAMPLES. TO THIS END, IONIZED FORMS OF THE ANALYTES WERE FIRST EXTRACTED INTO AN AQUEOUS ACCEPTOR PHASE USING EME METHOD. THEN, DLLME WAS APPLIED TO TRANSFER THE TARGET ANALYTES INTO FINAL ORGANIC PHASE WHICH IS GC COMPATIBLE.BOTH OF EME AND DLLME VARIABLES WERE OPTIMIZED. THE SLM WAS A MIXTURE OF 90% NPOE AND 10% DI- (2-ETHYLHEXYL) PHOSPHATE (DEHP). AN ELECTRIC FIELD OF 100 V WAS APPLIED TO TRANSFER THE ANALYTES INTO ACIDIC ACCEPTOR SOLUTION WITH PH 1.0. ACCEPTOR SOLUTION WERE TRANSFERRED TO 1 ML OF THE ALKALINE SOLUTION (PH=13) AND THEN DLLME PROCEDURE WAS PERFORMED. CHLOROFORM AND METHANOL WERE USED AS EXTRACTION AND DISPERSER SOLVENT, RESPECTIVELY. PRECONCENTRATION FACTORS IN THE RANGE OF 40-263 AND SATISFACTORY REPEATABILITIES (2.3<RSD%<5.3) WERE OBTAINED IN DIFFERENT MATRICES. THE METHOD WAS APPLIED FOR DETERMINATION AND QUANTIFICATION OF PYRIDINE COMPOUNDS IN SMOKERS’ REAL SAMPLES. THE PROPOSED TECHNIQUE CAN BE INTRODUCED AS A SIMPLE, FAST AND INEXPENSIVE METHOD FOR DIAGNOSIS SMOKERS.

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