Dong-Seok Lho

Cyclodextrin-mediated micellar electrokinetic chromatography and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry for the enantiomer separation of racemorphan in human urine

Micellar electrokinetic chromatography (MEKC) was successfully and conveniently applied to the chiral separation with the addition of cyclodextrins (CDs) as chiral selector to the running buffer. Chiral separation depended on the type of CD; in particular, beta-CD was effective for the chiral separation of racemorphan. We investigated the optimal conditions of type and concentration of CD as chiral selector for the routine enantiomeric separation of racemorphan with good reproducibility. The effects of other parameters such as buffer pH and detection wavelength were also investigated to obtain the optimum conditions for the enantiomeric separation of racemorphan. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry was used for confirmation of racemorphan. The optimal conditions for enantiomeric separation of the racemorphan were as follows: 50 mM borate buffer at pH 9.4 with 50 mM SDS, 10 mM beta-CD and 20% 1-propanol, 57 cm x 50 microns fused-silica capillary column, and UV detection at 192 nm. Based on the developed method, racemorphan in human urine was also separated and determined using solid-phase extraction and MEKC.

Identification of a pyrovalerone metabolite in the rat by gas chromatography-mass spectrometry and determination of pyrovalerone by gas chromatography-nitrogen-phosphorus detection.

Pyrovalerone and its hydroxylated metabolite have been identified by gas chromatography-mass spectrometry in rat urine and plasma. A sensitive gas chromatographic method for the quantitative analysis of pyrovalerone in rat urine and plasma is described. The method also permits the quantitative monitoring of the urinary excretion of the drug and its metabolite. Pyrovalerone and its hydroxylated metabolite are detected up to 18 h after a single oral administration to the rat at a dose of 20 mg/kg.

Determination of carphedon in human urine by solid-phase microextraction using capillary gas chromatography with nitrogen–phosphorus detection

Carphedon is a phenyl derivative of nootropil and is effective in increasing physical endurance and cold resistance, and is used for amnesia treatment. Carphedon was extracted from human urine samples by solid-phase microextraction with a 65 microns carbowax-divinylbenzene-coated fiber. This analysis was performed by using capillary gas chromatography with nitrogen-phosphorus detection and optimized at pH 9.6, 30% NaCl, immersion time 10 min and desorption in the GC injector at 250 degrees C for 3 min. The regression equation for carphedon showed good linearity in the range from 0.1 to 10 micrograms ml-1 for human urine samples. The limit of detection was 0.01 microgram ml-1. The developed method is more sensitive and simpler in sample preparation than liquid-liquid extraction and can be applied to doping analysis for stimulants.

A simple device of the dry tetrabromophenolphthalein ethyl ester reagent strip for the detection of methamphetamine

A new device to detect methamphetamine (MA), amphetamine(A) and its metabolites in urine was developed using the paper strip method and the test tube method of dry chemical reagents. The reagent containing tetrabromophenolphthalein ethyl ester (TBPE) and borax. For the TBPE paper strip method, a device was prepared with a window at each end of the reagent paper strip; one window is for the sample application, and the other window is for the methylene chloride. The diffused sample from one window reacts with reagent in the paper and produces color at the point where it meets with methylene chloride which has diffused form the other side. A positive sample produces as red-purple color and the negative sample a greenish color, with a detection limit of 5–10 ppm. The result can be obtained within one minute. For the TBPE test tube method which contains dry reagents, the detection limit is 5 ppm and the result can be obtained within 30 seconds, however the carry-on is not as convenient as the paper strip method. The performance of both methods were evlauated by comparing with the results of gas chromatography (GC) and fluorescence polarization immunoassay (FPIA). The results were proven that both methods were useful as primary screening reagents to detect MA in urine and in dry powder.