Automated in tube solid-phase microextraction coupled with liquid chromatography/electrospray ionization mass spectrometry for the determination of β-blockers and metabolites in urine and serum samples

被引:164
作者
Kataoka', H
Narimatsu, S
Lord, HL
Pawliszyn, J [1 ]
机构
[1] Univ Waterloo, Dept Chem, Waterloo, ON N2L 3G1, Canada
[2] Okayama Univ, Fac Pharmaceut Sci, Okayama 7008530, Japan
关键词
D O I
10.1021/ac990356x
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
The technique of automated in-tube solid-phase microextraction (SPME) coupled with liquid chromatography/electrospray ionization mass spectrometry (LC/ESI-MS) was evaluated for the determination of beta-blockers in urine and serum 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 by repeated draw/eject cycles of sample solution. LC/MS analyses of beta-blockers were initially performed by liquid injection onto a LC column. Nine beta-blockers tested in this study gave very simple ESI mass spectra, and strong signals corresponding to [M + H](+) were observed for all beta-blockers. 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. To optimize the extraction of beta-blockers, several in-tube SPME parameters were examined. The optimum extraction conditions were 15 draw/eject cycles of 30 mu L of sample in 100 mM Tris-HCl (pH 8.5) at a now rate of 100 mu L/min using an Omegawax 250 capillary (Supelco, Bellefonte, PA). The beta-blockers extracted by the capillary were easily desorbed by mobile-phase now, and carryover of beta-blockers was not observed. Using in-tube SPME/LC/ESI-MS with selected ion monitoring, the calibration curves of beta-blockers were linear in the range from 2 to 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 method was successfully applied to the analysis of biological samples without interference peaks. The recoveries of beta-blockers spiked into human urine and serum samples were above 84 and 71%, respectively. A serum sample from a patient administrated propranolol was analyzed using this method and both propranolol and its metabolites were detected.
引用
收藏
页码:4237 / 4244
页数:8
相关论文
共 45 条
[31]   RING-HYDROXYLATED PROPRANOLOL - SYNTHESIS AND BETA-RECEPTOR ANTAGONIST AND VASODILATING ACTIVITIES OF THE 7 ISOMERS [J].
OATIS, JE ;
RUSSELL, MP ;
KNAPP, DR ;
WALLE, T .
JOURNAL OF MEDICINAL CHEMISTRY, 1981, 24 (03) :309-314
[32]   Selective extraction of beta-blockers from biological fluids by column-switching high-performance liquid chromatography using an internal-surface phenylboronic acid precolumn [J].
Ohta, T ;
Niida, S ;
Nakamura, H .
JOURNAL OF CHROMATOGRAPHY B-BIOMEDICAL APPLICATIONS, 1996, 675 (01) :168-173
[33]  
Pawliszyn J., 1997, SOLID PHASE MICROEXT
[34]   Performance of micellar mobile phases in reversed-phase chromatography for the analysis of pharmaceuticals containing beta-blockers and other antihypertensive drugs [J].
RapadoMartinez, I ;
GarciaAlvarezCoque, MC ;
VillanuevaCamanas, RM .
ANALYST, 1996, 121 (11) :1677-1682
[35]   SCREENING AND DETERMINATION OF BETA-BLOCKERS, NARCOTIC ANALGESICS AND STIMULANTS IN URINE BY HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY WITH COLUMN-SWITCHING [J].
SAARINEN, MT ;
SIREN, H ;
RIEKKOLA, ML .
JOURNAL OF CHROMATOGRAPHY B-BIOMEDICAL APPLICATIONS, 1995, 664 (02) :341-346
[36]   SCREENING OF BETA-BLOCKERS IN HUMAN SERUM BY ION-PAIR CHROMATOGRAPHY AND THEIR IDENTIFICATION AS METHYL OR ACETYL DERIVATIVES BY GAS-CHROMATOGRAPHY MASS-SPECTROMETRY [J].
SIREN, H ;
SAARINEN, M ;
HAINARI, S ;
LUKKARI, P ;
RIEKKOLA, ML .
JOURNAL OF CHROMATOGRAPHY, 1993, 632 (1-2) :215-227
[38]   Rapid SPME/LC/MS/MS analysis of N-methylcarbamate pesticides in water [J].
Volmer, DA ;
Hui, JPM .
ARCHIVES OF ENVIRONMENTAL CONTAMINATION AND TOXICOLOGY, 1998, 35 (01) :1-7
[39]  
Volmer DA, 1998, RAPID COMMUN MASS SP, V12, P123, DOI 10.1002/(SICI)1097-0231(19980214)12:3<123::AID-RCM126>3.0.CO
[40]  
2-4