-
[show abstract]
[hide abstract]
ABSTRACT: Low-temperature and ambient-temperature nonaqueous stacking techniques in capillary electrophoresis (CE) are described for the first time. A low-temperature bath was used to control the temperature from ambient to subzero degrees, by which a novel hyphenated method, low-temperature bath-nonaqueous capillary electrophoresis stacking (LTB-NACE stacking) is demonstrated. 3,4-Methylenedioxymethamphetamine (3,4-MDMA) was determined at a concentration of 4.7 x 10(-6) M (at a 92.1% confidence level) by normal nonaqueous capillary zone electrophoresis (NACZE) and this was improved to 2.6 x 10(-8) M and 5.0 x 10(-9) M, respectively, when the NACZE stacking and LTB-NACZE stacking techniques were applied. The content of 3,4-MDMA in an illicit drug and a suspect urine sample was readily detected. Upon application of the LTB to the separation of isomers the resolution (R) for the separation of 2,3-/3,4-MDMA was improved from 0.6 (LTB, 22 degrees C) to 1.6 (LTB, -55 degrees C) and for (+)3,4-MDMA/(-)3,4-MDMA, from 0.4 (LTB, 25 degrees C) to 1.0 (LTB, -10 degrees C).
Electrophoresis 07/2004; 25(10-11):1601-6. · 3.30 Impact Factor
-
[show abstract]
[hide abstract]
ABSTRACT: The separation and on-line concentration of lysergic acid diethylamide (LSD) in mouse blood was achieved by means of capillary electrophoresis/fluorescence spectroscopy using sodium dodecyl sulfate (SDS) as the surfactant. Techniques involving on-line sample concentration, including sweeping micellar electrokinetic chromatography (sweeping-MEKC) and cation-selective exhaustive injection-sweep-micellar electrokinetic chromatography (CSEI-sweep-MEKC) were applied; the optimum on-line concentration and separation conditions were determined. In the analysis of an actual sample, LSD was found in a blood sample from a test mouse (0.1 mg LSD fed to a 20 g mouse; approximately 1/10 to the value of LD(50)). As a result, 120 and 30 ng/mL of LSD was detected at 20 and 60 min, respectively, after ingestion of the doses.
Electrophoresis 04/2003; 24(6):1031-7. · 3.30 Impact Factor
-
[show abstract]
[hide abstract]
ABSTRACT: This work describes a novel method for the accurate determination of lysergic acid diethylamide (LSD) in tablets. A technique involving sweeping-micellar electrokinetic chromatography (MEKC) was used for the initial on-line concentration and separation, after which a cryogenic molecular fluorescence experiment was performed at 77 K. Using this approach, not only the separation of LSD from the tablet extract was achieved, but on-line spectra were readily distinguishable and could be unambiguously assigned. The results are in agreement with analyses by gas chromatography-mass spectrometry (GC-MS). Thus, this method, which was found to be accurate, sensitive and rapid, has the potential for use as a reliable complementary method to GC-MS in such analyses.
Electrophoresis 04/2003; 24(6):1025-30. · 3.30 Impact Factor
-
[show abstract]
[hide abstract]
ABSTRACT: The principal advantage of the use of Shopl'skii effect (low temperature spectrum) is that spectral sharpening occurs both in absorption and emission. However, thus far using the technique of capillary electrophoresis/low temperature fluorescence spectroscopy (CE/LTFS) either at 77 or 4.2 K remains difficult to obtain an on-line spectrum, if the analyte is present at low concentration. This paper examines the feasibility of combining the techniques of online concentration and CE/LTFS to identify LSD and related compounds in urine at 77 K. To improve sensitivity, sweeping-micellar electrokinetic chromatography (sweeping-MEKC) and cation-selective exhaustive injection-sweep-micellar electrokinetic chromatography (CSEI-sweep-MEKC) were used for on-line concentration which resulted in detection limits of approximately 20 approximately 60 ppt, respectively.
Talanta 11/2002; 58(4):691-9. · 3.79 Impact Factor
-
[show abstract]
[hide abstract]
ABSTRACT: The separation and on-line concentrations of lysergic acid diethylamide (LSD), iso-lysergic acid diethylamide (iso-LSD) and lysergic acid N,N-methylpropylamide (LAMPA) in human urine were investigated by capillary electrophoresis-fluorescence spectroscopy using sodium dodecyl sulfate (SDS) as an anionic surfactant. A number of parameters such as buffer pH, SDS concentration, Brij-30 concentration and the content of organic solvent used in separation, were optimized. The techniques of sweeping-micellar electrokinetic chromatography (sweeping-MEKC) and cation-selective exhaustive injection-sweep-micellar electrokinetic chromatography (CSEI-sweep-MEKC) were used for determining on-line concentrations. The advantages and disadvantages of this procedure with respect to sensitivity, precision and simplicity are discussed and compared.
Journal of Chromatography B 08/2002; 775(1):37-47. · 2.89 Impact Factor
-
[show abstract]
[hide abstract]
ABSTRACT: Because of the increasing use of 3,4-methylenedioxymethamphetamine (3,4-MDMA), a rapid and sensitive analytical technique is required for its detection and determination. Using nonaqueous capillary electrophoresis/fluorescence spectroscopy (NACE/FS) detection, it is possible to determine this drug at the level 0.5 ppm without any pre-treatment in less than 5 min. After liquid-liquid extraction, the sample can be condensed and a detection limit of 3,4-MDMA in urine of 50 ppb (S/N = 3) can be achieved. The precision of the method was evaluated by measuring the repeatability and intermediate precision of migration time and the corrected peak height by comparison with a 3,4-MDMA-D5 internal standard. With the conventional GC/MS method, it is necessary to derivatize the 3,4-MDMA before injection and the GC migration time also is in excess of 20 min. Therefore, NACE/FS represents a good complementary method to GC/MS for use in forensic analysis.
Forensic Science International 03/2002; 125(2-3):142-8. · 2.30 Impact Factor
