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Titolo:
Development of automated in-tube SPME/LC/MS method for drug analysis
Autore:
Kataoka, H; Lord, HL; Yamamoto, S; Narimatsu, S; Pawliszyn, J;
Indirizzi:
Univ Waterloo, Dept Chem, Waterloo, ON N2L 3G1, Canada Univ Waterloo Waterloo ON Canada N2L 3G1 em, Waterloo, ON N2L 3G1, Canada Okayama Univ, Fac Pharmaceut Sci, Okayama 7008530, Japan Okayama Univ Okayama Japan 7008530 harmaceut Sci, Okayama 7008530, Japan
Titolo Testata:
JOURNAL OF MICROCOLUMN SEPARATIONS
fascicolo: 9, volume: 12, anno: 2000,
pagine: 493 - 500
SICI:
1040-7685(2000)12:9<493:DOAISM>2.0.ZU;2-7
Fonte:
ISI
Lingua:
ENG
Soggetto:
SOLID-PHASE MICROEXTRACTION; PERFORMANCE LIQUID-CHROMATOGRAPHY; MASS-SPECTROMETRY; HUMAN URINE; WATER; FIBERS; HPLC; GAS;
Keywords:
in-tube solid-phase microextraction; liquid chromatography/mass spectrometry; automated sample preparation; drug analysis; stimulants; beta-blockers;
Tipo documento:
Article
Natura:
Periodico
Settore Disciplinare:
Physical, Chemical & Earth Sciences
Citazioni:
27
Recensione:
Indirizzi per estratti:
Indirizzo: Kataoka, H Univ Waterloo, Dept Chem, Waterloo, ON N2L 3G1, Canada Univ Waterloo Waterloo ON Canada N2L 3G1 o, ON N2L 3G1, Canada
Citazione:
H. Kataoka et al., "Development of automated in-tube SPME/LC/MS method for drug analysis", J MICROCOL, 12(9), 2000, pp. 493-500

Abstract

The technique of automated in-tube solid-phase microextraction (SPME) coupled with liquid chromatography/electrospray ionization mass spectrometry (LC/ESI-MS) was developed for the determination of stimulants and beta -blockers in biological samples. In-tube SPME is an extraction technique for organic compounds in aqueous samples, in which analytes are extracted from the sample directly into an open tubular capillary column by repeated draw/eject cycles of sample solution. LC/MS analyses of stimulants and beta -blockers were initially performed by liquid injection onto a LC column. Five stimulants and nine beta -blockers tested in this study gave very simple ESI mass spectra, and strong signals corresponding to [M + H](+) were observed foran drugs. The stimulants were separated with a Supelcosil LC-CN column using acetonitrile/50 mM ammonium acetate (15:85) as a mobile phase. The beta -blockers were separated with a HyperSil BDS C-18 column using acetonitrile/methanol/water/acetic acid (15:15:70:1) as a mobile phase. In order to optimize the extraction of these drugs, several in-tube SPME parameters were examined. The optimum extraction conditions were 15 draw/eject cycles of 30-35 muL Of Sample in 50-100 mM Tris-HCl (pH 8.5) at a flow rate of 100 muL/min using Omegawax 250 capillary column (Supelco, Bellefonte, PA). The drugsextracted on the capillary column were easily desorbed by mobile phase flow, and carryover of drugs was not observed. Using in-tube SPME/LC/ESI-MS with selected ion monitoring, the calibration curves of drugs were linear in the range of 2-100 ng/mL with correlation coefficients above 0.9982 (n = 18), and detection limits (S/N = 3) of 0.1-1.2 ng/mL. This technique was successfully applied to the analysis of biological samples, such as urine and serum, without interference peaks. The recoveries of drugs spiked into humanurine and serum samples were above 81 and 71%, respectively. (C) 2000 JohnWiley & Sons, Inc.

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Documento generato il 14/07/20 alle ore 06:29:47