In this study, we present a capillary electrochromatographic method for separation of basic compounds of interest in forensic science (amphetamine,methamphetamine, 3,4-methylenedioxyamphetamine, 3,4- methylenedioxymethamphetamine, 3,4-methylenedioxyethylamphetamine, cocaine, codeine, heroin,morphine, and 6-monoacethylmorphine). Several analytical conditions were taken into account to completely separate in the same run the 10 drugs of abuse analyzed. Chromatographic retention, selectivity and efficiency were evaluated in dependence of the type of stationary phase (CN and RP-C18 derivatized silica particles), mobile phase composition, buffer type and pH, sample injection. The optimum separation parameters were set up using a mixture of aqueous sodium phosphate buffer (pH 2.5)/acetonitrile (80/20, v/v) as the mobile phase, 10 kV and 20 æC as applied voltage and capillary temperature, respectively. Under these conditions all the studied analytes were baseline resolved within 20 min. The method performance was investigated in terms of precision, linearity, sensitivity and accuracy to demonstrate the applicability of the developed capillary electrochromatographic system to forensic analysis. Calibration curves provided a good linearity over a working range of 1001200 ng/mL for all analytes. Limits of detection and quantification were in the range 512 ng/mL and 1030 ng/mL, respectively. Then the method was applied to the analysis of a human urine sample spiked with a basic compounds mixture. Urine samples pre-treatmentwas carried out through a solid phase extraction (SPE) procedure on strong cation exchange (SCX) cartridges.
Capillary electrochromatographic separation of illicit drugs employing a cyano stationary phase
Z Aturki;G D'Orazio;S Fanali;A Rocco;
2009
Abstract
In this study, we present a capillary electrochromatographic method for separation of basic compounds of interest in forensic science (amphetamine,methamphetamine, 3,4-methylenedioxyamphetamine, 3,4- methylenedioxymethamphetamine, 3,4-methylenedioxyethylamphetamine, cocaine, codeine, heroin,morphine, and 6-monoacethylmorphine). Several analytical conditions were taken into account to completely separate in the same run the 10 drugs of abuse analyzed. Chromatographic retention, selectivity and efficiency were evaluated in dependence of the type of stationary phase (CN and RP-C18 derivatized silica particles), mobile phase composition, buffer type and pH, sample injection. The optimum separation parameters were set up using a mixture of aqueous sodium phosphate buffer (pH 2.5)/acetonitrile (80/20, v/v) as the mobile phase, 10 kV and 20 æC as applied voltage and capillary temperature, respectively. Under these conditions all the studied analytes were baseline resolved within 20 min. The method performance was investigated in terms of precision, linearity, sensitivity and accuracy to demonstrate the applicability of the developed capillary electrochromatographic system to forensic analysis. Calibration curves provided a good linearity over a working range of 1001200 ng/mL for all analytes. Limits of detection and quantification were in the range 512 ng/mL and 1030 ng/mL, respectively. Then the method was applied to the analysis of a human urine sample spiked with a basic compounds mixture. Urine samples pre-treatmentwas carried out through a solid phase extraction (SPE) procedure on strong cation exchange (SCX) cartridges.I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
