Simultaneous assay of sildenafil and desmethylsildenafil in human plasma using liquid chromatography-tandem mass spectrometry on silica column with aqueous-organic mobile phase

被引:65
作者
Eerkes, A [1 ]
Addison, T [1 ]
Weng, ND [1 ]
机构
[1] Covance Labs Inc, Madison, WI 53704 USA
来源
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES | 2002年 / 768卷 / 02期
关键词
sildenatil; desmethylsildenafil;
D O I
10.1016/S1570-0232(01)00602-X
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A liquid chromatography-tandem mass spectrometry method was developed for the analysis of sildenafil (SIL) and its metabolite desmethylsildenafil (DMS) in human plasma. Samples were accurately transferred to 96-well plates using a liquid handler (Multiprobe II). Solid-phase extraction was carried out on a 96-channel programmable liquid handling workstation (Quadra 96) using a C-8 and cation-exchange mixed-mode sorbent. The extract was injected onto a silica column with an aqueous-organic mobile phase, a combination that was novel for improving the method sensitivity. The low limit of quantitation was 1.0 ng/ml for both SIL and DMS. The method was validated to meet the criteria of current industrial guidance for quantitative bioanalytical methods. (C) 2002 Elsevier Science B.V. All rights reserved.
引用
收藏
页码:277 / 284
页数:8
相关论文
共 21 条
[1]  
Allanson JP, 1996, RAPID COMMUN MASS SP, V10, P811, DOI 10.1002/(SICI)1097-0231(199605)10:7<811::AID-RCM561>3.0.CO
[2]  
2-Q
[3]  
[Anonymous], 2001, Guidance for industry, bioanalytical method validation
[4]  
BHOIR IC, 2000, INDIAN DRUGS, V37, P319
[5]   Development of an assay for the simultaneous determination of sildenafil (Viagra) and its metabolite (UK-103,320) using automated sequential trace enrichment of dialysates and high-performance liquid chromatography [J].
Cooper, JDH ;
Muirhead, DC ;
Taylor, JE ;
Baker, PR .
JOURNAL OF CHROMATOGRAPHY B, 1997, 701 (01) :87-95
[6]   Determinaton of sildenafil citrate and related substances in the commercial products and tablet dosage form using HPLC [J].
Daraghmeh, N ;
Al-Omari, M ;
Badwan, AA ;
Jaber, AMY .
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS, 2001, 25 (3-4) :483-492
[7]   Automated solid-phase extraction workstations combined with quantitative bioanalytical LC/MS [J].
Huang, NH ;
Kagel, JR ;
Rossi, DT .
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS, 1999, 19 (3-4) :613-620
[8]  
Janiszewski J, 1997, RAPID COMMUN MASS SP, V11, P1033
[9]   Narrowbore high-performance liquid chromatography for the simultaneous determination of sildenafil and its metabolite UK-103,320 in human plasma using column switching [J].
Jeong, CK ;
Lee, HY ;
Jang, MS ;
Kim, WB ;
Lee, HS .
JOURNAL OF CHROMATOGRAPHY B, 2001, 752 (01) :141-147
[10]  
*MED EC CO, 2000, PHYS DESK REF, P2382