Optimized stationary phases for the high-performance liquid chromatography-electrospray ionization mass spectrometric analysis of basic pharmaceuticals

被引:55
作者
Needham, SR
Brown, PR
Duff, K
Bell, D
机构
[1] Pfizer Inc, Candidate Synth Enhancement & Evaluat Grp, Groton, CT 06340 USA
[2] Univ Rhode Isl, Dept Chem, Kingston, RI 02881 USA
[3] Restek Corp, Bellefonte, PA 16823 USA
关键词
stationary phases; LC; antidepressants; tricyclic; beta-blockers;
D O I
10.1016/S0021-9673(99)00986-3
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
Stationary phases were investigated for HPLC coupled with electrospray ionization mass spectrometry (ESI-MS) for the analysis of basic drugs. Tricyclic antidepressants (TCAs) and beta-blockers were used as model solutes. The functional groups, pentafluorophenyl (PFP), OH, CN or CH3 were attached to the silica via a propyl chain. The effects of these stationary phases as well as C-8 and C-18 phases on retention and peak shape of the basic drugs were studied. The CN and PFP phases adequately retained (t(R) of 2 to 6 min) the basic drugs when the mobile phase was composed of 90% acetonitrile, whereas with the C-4, C-8 and C-18 phases, less than 40% acetonitrile had to be used to provide adequate retention of the basic drugs. Because acetonitrile provides better desolvation in ESI than an aqueous solvent, it produces an increased MS signal. As an example of the HPLC-ESI-MS analysis of the beta-blocker, pindolol, on a CN phase, the use of 90% acetonitrile in the mobile phase increased the ESI-RIS signal by 790% when compared to a C-18 phase which could use only 5% acetonitrile in the mobile phase for retention of the solute. In addition, the CN and PFP phases provided better peak shape than the OH phase and the hydrophobic phases (C-4, C-8 and C-18) and ion-pairing or ion-suppressing agents were not required. The retention behavior of the TCAs and beta-blockers on each of the phases is described. (C) 2000 Elsevier Science B.V. All rights reserved.
引用
收藏
页码:159 / 170
页数:12
相关论文
共 36 条
[1]   Reversed-phase high-performance liquid chromatographic separations of tocopherols [J].
Abidi, SL ;
Mounts, TL .
JOURNAL OF CHROMATOGRAPHY A, 1997, 782 (01) :25-32
[2]   Solid phase extraction procedure of polar benzene- and naphthalenesulfonates in industrial effluents followed by unequivocal determination with ion pair chromatography/electrospray-mass spectrometry [J].
Alonso, MC ;
Castillo, M ;
Barceló, D .
ANALYTICAL CHEMISTRY, 1999, 71 (13) :2586-2593
[3]   Sensitive and rapid method for the simultaneous quantification of five antidepressants with their respective metabolites in plasma using high-performance liquid chromatography with diode-array detection [J].
Aymard, G ;
Livi, P ;
Pham, YT ;
Diquet, B .
JOURNAL OF CHROMATOGRAPHY B, 1997, 700 (1-2) :183-189
[4]   Quantitative determination of the β-blocker labetalol in pharmaceuticals and human urine by high-performance liquid chromatography with amperometric detection [J].
Ceniceros, C ;
Maguregui, MI ;
Jiménez, RM ;
Alonso, RM .
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES, 1998, 705 (01) :97-103
[5]   Validation of a high-performance liquid chromatographic method for the determination of norfloxacin and its application to stability studies (photo-stability study of norfloxacin) [J].
Cóordoba-Borrego, M ;
Cóordoba-Díaz, M ;
Cóordoba-Díaz, D .
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS, 1999, 18 (06) :919-926
[6]   PREPARATION AND COMPARISON OF A PENTAFLUOROPHENYL STATIONARY PHASE FOR REVERSED-PHASE LIQUID-CHROMATOGRAPHY [J].
CSATO, E ;
FULOP, N ;
SZABO, G .
JOURNAL OF CHROMATOGRAPHY, 1990, 511 :79-88
[7]   Determination of arylphenoxypropionic herbicides in water by liquid chromatography electrospray mass spectrometry [J].
D'Ascenzo, G ;
Gentili, A ;
Marchese, S ;
Perret, D .
JOURNAL OF CHROMATOGRAPHY A, 1998, 813 (02) :285-297
[8]  
Detaevernier M R, 1983, J Pharm Biomed Anal, V1, P331, DOI 10.1016/0731-7085(83)80045-4
[9]   FACTORS AFFECTING ELECTROSPRAY-IONIZATION OF EFFLUENTS CONTAINING TRIFLUOROACETIC-ACID FOR HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY/MASS SPECTROMETRY [J].
ESHRAGHI, J ;
CHOWDHURY, SK .
ANALYTICAL CHEMISTRY, 1993, 65 (23) :3528-3533
[10]  
Hutton KA, 1997, RAPID COMMUN MASS SP, V11, P735, DOI 10.1002/(SICI)1097-0231(19970422)11:7<735::AID-RCM918>3.0.CO