Article

Simultaneous determination of barbiturates in human biological fluids by direct immersion solid-phase microextraction and gas chromatography-mass spectrometry.

Department of Legal Medicine, Aichi Medical University School of Medicine, Nagakute-cho, Aichi 480-1195, Japan.
Journal of Chromatography B (Impact Factor: 2.49). 07/2004; 806(1):65-73. DOI: 10.1016/j.jchromb.2004.03.016
Source: PubMed

ABSTRACT Simultaneous determination of seven barbiturates in human whole blood and urine by combining direct immersion solid-phase microextraction (DI-SPME) with gas chromatography-mass spectrometry (GC-MS) is presented. The main parameters affecting the DI-SPME process, such as SPME fibers, salt additives, pHs, extraction temperatures and immersion times were optimized for simultaneous determination of the drugs. The extraction efficiencies were 0.0180-0.988 and 0.0156-2.76% for whole blood and urine, respectively. The regression equations of the drugs showed excellent linearity for both samples; the correlation coefficients (r(2)) were 0.994-0.999. The detection limits for whole blood were 0.05-1 microg x ml(-1), and those for urine 0.01-0.6 microg x ml(-1). Actual quantitation could be made for pentobarbital in whole blood and urine obtained from volunteers, who had been orally administered a therapeutic dose of the drug. The DI-SPME/GC-MS procedure for barbiturates established in this study is simple and sensitive enough to be adopted in the fields of clinical and forensic toxicology.

0 Bookmarks
 · 
75 Views
  • [Show abstract] [Hide abstract]
    ABSTRACT: Sample preparation is important for isolating desired components from complex matrices and greatly influences their reliable and accurate analysis. Recent trends in sample preparation include miniaturization, automation, high-throughput performance, online coupling with analytical instruments, and low-cost operation through extremely low or no solvent consumption. Microextraction techniques, such as liquid-phase microextraction and solid-phase microextraction, have these advantages over the traditional approaches of liquid-liquid extraction and conventional solid-phase extraction. This review focuses primarily on these microextraction techniques developed over the last decade, and presents a summary of the characteristics of various approaches in drug analysis.
    Analytical and Bioanalytical Chemistry 10/2009; 396(1):339-64. · 3.66 Impact Factor
  • [Show abstract] [Hide abstract]
    ABSTRACT: A new, simple and rapid capillary electrophoresis method, using hexadimethrine bromide (HDB) as electro-osmotic flow modifier, has been developed for the identification and determination of nine barbiturates, barbital acid, barbital, phenobarbital, pentobarbital, amobarbital, thiobarbituric acid, butobarbital, N-methyl-5-phenyl-ethyl barbital acid and 5-cyclohexenyl-5-ethyl barbital acid in urine with UV detection at 200nm. The applied voltage was −25kV and the capillary temperature was kept constant at 25°C. The effects of buffer pH, the concentration of HDB and the concentration of α-cyclodextrin were studied systematically. Optimum separation was achieved with 20mM borate buffer at pH10.00 containing 0.04% (w/v) HDB and 2.06mM α-cyclodextrin. Regression equations revealed good linear relationship between the peak area of each compound and its concentration. The correlation coefficients were from 0.9990 to 0.9997. The relative standard deviations of migration times and peak areas were <3.84 and 5.45% (intra-day). The nine barbiturates in urine were successfully determined within 7min, without a prior preparation step and the method is useful for the investigation of intoxication.
    Chromatographia 01/2007; 65(9):611-615. · 1.44 Impact Factor
  • [Show abstract] [Hide abstract]
    ABSTRACT: Solid-phase microextraction (SPME) has undergone a surge in popularity within the field of analytical chemistry in the past two decades since its introduction. Owing to its nature of extraction, SPME has become widely known as a quick and cost-effective sample preparation technique. Although SPME has demonstrated extraordinary versatility in sampling capabilities, the technique continues to experience a tremendous growth in innovation. Presently, increasing efforts have been directed towards the engineering of novel sorbent material in order to expand the applicability of SPME for a wider range of analytes and matrices. This review highlights the application of ionic liquids (ILs) and polymeric ionic liquids (PILs) as innovative sorbent materials for SPME. Characterized by their unique physico-chemical properties, these compounds can be structurally-designed to selectively extract target analytes based on unique molecular interactions. To examine the advantages of IL and PIL-based sorbent coatings in SPME, the field is reviewed by gathering available experimental data and exploring the sensitivity, linear calibration range, as well as detection limits for a variety of target analytes in the methods that have been developed.
    Analytica chimica acta 06/2011; 695(1-2):18-43. · 4.31 Impact Factor