Seungki Kim

Determination of amphetamine, methamphetamine and dimethamphetamine in Human Urine by Solid-Phase Microextraction (SPME)-Gas Chromatography/Mass Spectrometry

A simple and rapid assay method for three stimulant drugs (amphetamine, methamphetamine, and dimethamphetamine) in human urine using solid-phase microextraction was developed. In solid-phase microextraction, the drugs were equilibrated between the adsorbent coated-fiber and aqueous sample matrix. After adsorption of the analytes, the fiber was directly transferred to the injector of a gas chromatograph, where the analytes were thermally desorbed and subsequently separated by the gas chromatograph and detected by mass spectrometer. The solid-phase microextraction method, which did not require solvents, was found to be a fast and simple analytical method. We optimized the solid-phase microextraction technique, for factors such as the NaCl salt effect (30%), pH effect (pH=12.4), equilibration time (30 min), desorption time (1 min) and coated-fiber type (100 microm poly(dimethylsiloxane)) and detected the stimulants in human urine, obtained from human subjects. The detection limits of each drug were below 1-10 ng/ml. The developed method can be applied to the abused drug test.

Solid-phase microextraction for the determination of pethidine and methadone in human urine using gas chromatography with nitrogen–phosphorus detection

A simple and rapid analytical method is presented for the determination of pethidine (meperidine) and methadone in human urine using solid-phase microextraction (SPME) and gas chromatography with nitrogen-phosphorus detection (GC-NPD). After the analytes had been partitioned between an extracting phase and the aqueous sample matrix, the needle of the coating fiber assembly was injected directly into the GC injector. The analytes were thermally desorbed in the heated injector (240 degrees C) and subsequently separated and detected by the GC-NPD system. The factors influencing the SPME method, such as the salt (NaCl) effect (15%), pH (pH 11), and equilibration time (30 min), were optimized. The calibration graphs for urine samples showed a good linearity. The detection limit was below 1 ng ml-1 for both drugs.

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.

Determination of six iodotrihalomethanes in drinking water in Korea

Trihalomethanes (THMs) are chemicals regulated by Environmental Protection Agencys first drinking water regulation issued after the passage of the Safe Drinking Water Act. Among THMs, iodotrihalomethanes (I-THMs) are produced by treating water containing iodides ion with chlorine or ozone. I-THMs are more carcinogenic and biotoxic than chlorinated or brominated THMs. The purpose of this study was to analyze of I-THMs in drinking water using the liquid-liquid extraction (LLE) method with various extraction solvents. The calibration curves ranged from 0.01 to 20 ng/mL and the correlation coefficient showed a good linearity of 0.99 or more. The method detection limit ranged from 0.01 to 0.10 ng/mL. The accuracy of the LLE method ranged from 99.43 to 112.40%, and its precision ranged from 1.10 to 10.36%. Good recoveries (71.35-118.60%) were obtained for spiked drinking water samples, demonstrating that the LLE method is suitable for the analysis of drinking water samples. Dichloroiodomethane, bromochloroiodomethane, and dibromoiodomethane were identified in drinking water collected from 70 places of water purification plants in Korea. The samples were classified by disinfection systems, regions, seasons, and water sources. The concentration of I-THMs in pre-/postchlorination facilities owing to excess chlorine usage was higher than in ozonization/postchlorination facilities. Moreover, the concentrations of I-THMs were high in the coastal region, because of the large amount of halide ions from the sea. There was no seasonal difference; however, the concentration of I-THMs in pre-/postchlorination facilities increased in spring and summer. The concentration of I-THMs in water sources was high in samples from the Geum River and the Yeongsan and Sumjin River. The concentration and detection frequency of I-THMs in Han River and Nakdong River were high in the coastal region, because of numerous pre-/postchlorination facilities and the abundance of halide ions from the ocean.