Stereoselective RP-HPLC determination of esmolol enantiomers in human plasma after pre-column derivatization

被引:17
作者
Tang, YH [1 ]
He, Y [1 ]
Yao, TW [1 ]
Zeng, S [1 ]
机构
[1] Zhejiang Univ, Coll Pharmaceut Sci, Dept Pharmaceut Anal & Drug Metab, Hangzhou 310031, Zhejiang, Peoples R China
来源
JOURNAL OF BIOCHEMICAL AND BIOPHYSICAL METHODS | 2004年 / 59卷 / 02期
基金
中国国家自然科学基金;
关键词
enantiomer separation; esmolol; PP-HPLC; diastereoselective chromatography;
D O I
10.1016/j.jbbm.2003.12.006
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A stereoselective reversed-phase HPLC assay to determine S-( -) and R-(+) enantiomers of esmolol in human plasma was developed. The method involved liquid-liquid extraction of esmolol from human plasma, using S-(-)-propranolol as the internal standard, and employed 2,3,4,6-tetra-O-acetyl-beta-D-glucopyranosyl isothiocyanate as a pre-column chiral derivatization reagent. The derivatized products were separated on a 5-mum reversed-phase C18 column with a mixture of acetonitrile/0.02 mol/L phosphate buffer (pH 4.5) (55:45, v/v) as mobile phase. The detection of esmolol derivatives was made at lambda = 224 nm with UV detector. The assay was linear from 0.035 to 12 mug/ml for each enantiomer. The analytical method afforded average recoveries of 94.8% and 95.5% for S-( -)- and R-(+)-esmolol, respectively. For each enantiomer, the limit of detection was 0.003 mug/ml and the limit of quantification for the method was 0.035 mug/ml (RSD < 14%). The reproducibility of the assay was satisfactory. (C) 2004 Elsevier B.V. All rights reserved.
引用
收藏
页码:159 / 166
页数:8
相关论文
共 12 条
[1]   Direct separation of labetalol stereoisomers in a high performance liquid chromatography system using helically self-assembled chelate as chiral selector in the mobile phase [J].
Bazylak, G ;
Aboul-Enein, HY .
JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES, 1999, 22 (08) :1171-1192
[2]  
Fornstedt T, 1997, CHIRALITY, V9, P329, DOI 10.1002/(SICI)1520-636X(1997)9:4<329::AID-CHIR3>3.0.CO
[3]  
2-8
[4]   Synthesis of new stable aliphatic isothiocyanate-based chiral derivatizing agent and application to indirect separation of chiral amino and thiol compounds [J].
Kleidernigg, OP ;
Lindner, W .
CHROMATOGRAPHIA, 1997, 44 (9-10) :465-472
[5]   Enantioselective analysis of (R)- and (S)-atenolol in urine samples by a high-perfomance liquid chromatography column-switching setup [J].
Lamprecht, G ;
Kraushofer, T ;
Stoschitzky, K ;
Lindner, W .
JOURNAL OF CHROMATOGRAPHY B, 2000, 740 (02) :219-226
[6]   Reversed-phase high-performance liquid chromatographic analysis of atenolol enantiomers in rat hepatic microsome after chiral derivatization with 2,3,4,6-tetra-O-acetyl-β-D-glycopyranosy isothiocyanate [J].
Li, X ;
Yao, TW ;
Zeng, S .
JOURNAL OF CHROMATOGRAPHY B, 2000, 742 (02) :433-439
[7]  
QUAN CY, 1988, DRUG METAB DISPOS, V16, P425
[8]   Analysis of enantiomers of chiral phenethylamine drugs by capillary gas chromatography/mass spectrometry/flame-ionization detection and pre-column chiral derivatization [J].
Tao, QF ;
Zeng, S .
JOURNAL OF BIOCHEMICAL AND BIOPHYSICAL METHODS, 2002, 54 (1-3) :103-113
[9]   ESMOLOL - A REVIEW OF ITS THERAPEUTIC EFFICACY AND PHARMACOKINETIC CHARACTERISTICS [J].
WIEST, D .
CLINICAL PHARMACOKINETICS, 1995, 28 (03) :190-202
[10]  
Xie GH, 1997, BIOMED CHROMATOGR, V11, P193, DOI 10.1002/(SICI)1099-0801(199707)11:4<193::AID-BMC672>3.0.CO