Simultaneous determination of barbiturates in human biological fluids by direct immersion solid-phase microextraction and gas chromatography-mass spectrometry
Department of Legal Medicine, Showa University, Shinagawa, Tōkyō, Japan Journal of Chromatography B
(Impact Factor: 2.73).
07/2004; 806(1):65-73. DOI: 10.1016/j.jchromb.2004.03.016
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.
Available from: Ravi Sheshala
- "al . , 2009 Hair HS - SPME PDMS ( 100 ) GC - MS Liu et al . , 2001 Nishida et al . , 2006 Saliva HS - SPME DI - SPME PDMS ( 30 ) GC - MS Fucci et al . , 2003 Barbiturates Whole blood DI - SPME PDMS ( 100 ) PDMS / DVB ( 65 ) GC - MS Iwai et al . , 2004 Urine DI - SPME PDMS ( 100 ) PDMS / DVB ( 65 ) PA ( 85 ) GC - MS Iwai et al . , 2004"
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ABSTRACT: This paper reviews the recent developments in bioanalysis sample preparation techniques and gives an update on basic principles, theory, applications and possibilities for automation, and a comparative discussion on the advantages and limitation of each technique. Conventional liquid-liquid extraction (LLE), protein precipitation (PP) and solid-phase extraction (SPE) techniques are now been considered as methods of the past. The last decade has witnessed a rapid development of novel sample preparation techniques in bioanalysis. Developments in SPE techniques such as selective sorbents and in the overall approach to SPE, such as hybrid SPE and molecularly imprinted polymer SPE, have been addressed. Considerable literature has been published in the area of solid-phase micro-extraction and its different versions, e.g. stir bar sorptive extraction, and their application in the development of selective and sensitive bioanalytical methods. Techniques such as dispersive solid-phase extraction, disposable pipette extraction and micro-extraction by packed sorbent offer a variety of extraction phases and provide unique advantages to bioanalytical methods. On-line SPE utilizing column-switching techniques is rapidly gaining acceptance in bioanalytical applications. PP sample preparation techniques such as PP filter plates/tubes offer many advantages like removal of phospholipids and proteins in plasma/serum. Newer approaches to conventional LLE techniques (salting-out LLE) are also covered in this review article.
Biomedical Chromatography 02/2011; 25(1-2):199-217. DOI:10.1002/bmc.1560 · 1.72 Impact Factor
Available from: Fernando Mauro Lancas
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ABSTRACT: A new solid phase microextraction (SPME) system, known as in-tube SPME, was recently developed using an open tubular fused-silica capilary column, instead of an SPME fiber, as the SPME device. On-line in-tube SPME is usually used in combination with high performance liquid chromatography. Drugs in biological samples are directly extracted and concentrated in the stationary phase of capillary columns by repeated draw/eject cycles of sample solution, and then directly transferred to the liquid chromatographic column. In-tube SPME is suitable for automation. Automated sample handling procedures not only shorten the total analysis time, but also usually provide better accuracy and precision relative to manual techniques. In-tube SPME has been demonstrated to be a very effective and highly sensitive technique to determine drugs in biological samples for various purposes such as therapeutic drug monitoring, clinical toxicology, bioavailability and pharmacokinetics.
Química Nova 01/2005; DOI:10.1590/S0100-40422005000500027 · 0.66 Impact Factor
Available from: Hiroyuki Kataoka
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ABSTRACT: Sample preparation is essential for isolating desired components from complex matrices and greatly influences their reliable and accurate analysis. Solid-phase microextraction (SPME) is a new and effective sample preparation technique. Fibers and capillary tubes coated with an appropriate stationary phase are usually used for SPME, but alternative microextraction techniques, including solid-phase dynamic extraction using an internal coated needle, microextraction in a packed syringe and stir-bar-sorptive extraction using a coated magnetic stir bar, have been developed recently. These techniques, in combination with gas chromatography (GC), GC-mass spectrometry (GC-MS), high performance liquid chromatography (HPLC), LC-MS or capillary electrophoresis, can be used for analysis for complex mixtures. These microextraction techniques save preparation time, as well as solvent purchase and disposal costs. This review summarizes recent advances in SPME and related microextraction techniques and their applications in pharmaceutical and biomedical analysis.
Current Pharmaceutical Analysis 01/2005; 1(1). DOI:10.2174/1573412052953373 · 0.72 Impact Factor
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