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
[1]   DETERMINATION OF SOME BETA-BLOCKERS AS DABSYL DERIVATIVES BY HPLC [J].
ALPERTUNGA, B ;
SUNGUR, S ;
ERSOY, L ;
MANAV, SY .
ARCHIV DER PHARMAZIE, 1990, 323 (09) :587-589
[2]  
[Anonymous], 1995, DISPOSITION TOXIC DR
[3]   SOLID-PHASE MICROEXTRACTION WITH THERMAL-DESORPTION USING FUSED-SILICA OPTICAL FIBERS [J].
ARTHUR, CL ;
PAWLISZYN, J .
ANALYTICAL CHEMISTRY, 1990, 62 (19) :2145-2148
[4]   Solid-phase extraction and derivatisation methods for beta-blockers in human post mortem whole blood, urine and equine urine [J].
Black, SB ;
Stenhouse, AM ;
Hansson, RC .
JOURNAL OF CHROMATOGRAPHY B-BIOMEDICAL APPLICATIONS, 1996, 685 (01) :67-80
[5]   Solid-phase microextraction coupled with high-performance liquid chromatography for the determination of alkylphenol ethoxylate surfactants in water [J].
BoydBoland, AA ;
Pawliszyn, JB .
ANALYTICAL CHEMISTRY, 1996, 68 (09) :1521-1529
[6]   The feasibility of the detection and quantitation of β-adrenergic blockers by solid-phase extraction and subsequent derivatization with methaneboronic acid [J].
Branum, GD ;
Sweeney, S ;
Palmeri, A ;
Haines, L ;
Huber, C .
JOURNAL OF ANALYTICAL TOXICOLOGY, 1998, 22 (02) :135-141
[7]  
Caldwell GW, 1998, J MASS SPECTROM, V33, P607, DOI 10.1002/(SICI)1096-9888(199807)33:7<607::AID-JMS672>3.0.CO
[8]  
2-O
[9]   SOLID-PHASE MICROEXTRACTION COUPLED TO HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY [J].
CHEN, J ;
PAWLISZYN, JB .
ANALYTICAL CHEMISTRY, 1995, 67 (15) :2530-2533
[10]  
Cruickshank J.M., 1988, BETA BLOCKERS CLIN P