heroin and betadex

A method has been developed for the detection of a mixture of morphine, codeine, 6-acetyl morphine (6-AM) and normorphine using capillary zone electrophoresis (CZE). The method utilized urinary 6-AM as a diagnostic indicator of heroin abuse because it is not a product of either morphine or codeine metabolism. The electrophoretic separation was achieved using an uncoated (50 microm I.D.) fused-silica capillary, 77 cm long, containing the detector window 10.0 cm from the outlet end. The running buffer (pH 6.0) contained 50 mM sodium phosphate and 0.015 M beta-cyclodextrins (beta-CD). The samples were first extracted using a mixed-mode solid-phase extraction procedure and then analyzed by CZE. The UV absorbance detection was monitored at 214 nm. It has been found that beta-CDs can improve separation efficiency due to their hydrophobic cavity. The effect of the concentration of beta-CD and pH was also evaluated. The application of electrokinetic injection with field amplified sample stacking results in low detection limits (40 ng/ml for each analyte) and the method has good reproducibility, precision, accuracy, and high recovery.

Topics: beta-Cyclodextrins; Cyclodextrins; Electrophoresis, Capillary; Heroin; Humans; Spectrophotometry, Ultraviolet; Technology, Pharmaceutical

The present paper describes the methodological optimization and validation of a capillary zone electrophoresis method for the rapid determination of heroin, secondary products and additives present in clandestine heroin samples, by using 20 mM beta-cyclodextrins in phosphate buffer, pH 3.23. Applied potential was 15 kV and separation temperature was 24 degrees C; detection was by UV absorption at 200 nm wavelength. Heroin samples were first dissolved in CHCl3-MeOH (96:4, v/v) and injected by pressure (0.5 p.s.i., 3 s; 1 p.s.i.=6894.76 Pa) after evaporation of the organic mixture and reconstitution in aqueous buffer. Under the described conditions, phenylethylamine (internal standard), morphine, monoacetylmorphine, heroin, acetylcodeine, papaverine, codeine and narcotine were baseline resolved in less than 10 min. The limit of detection was better than 1 microg/ml for each analyte. The study of the intra-day and day-to-day precision showed, in terms of migration times, RSDs < or = 0.71% and, in terms of peak areas, RSDs < or = 3.2%. Also, the evaluation of linearity and analytical accuracy of the method provided good results for all the analytes investigated, thus allowing its application to real cases of seized controlled drug preparations.

Topics: beta-Cyclodextrins; Cyclodextrins; Electrophoresis, Capillary; Heroin; Illicit Drugs; Reference Standards; Reproducibility of Results; Sensitivity and Specificity