Development of an LC-MS Method for Measuring TNF in Human Vaginal Tissue

被引:11
作者
Choi, S. O.
Rezk, N. [1 ]
Kim, J. S. [1 ]
Kashuba, A. D. M. [1 ]
机构
[1] Univ N Carolina, Ctr AIDS Res, Chapel Hill, NC 27515 USA
关键词
PERFORMANCE LIQUID-CHROMATOGRAPHY; HUMAN PLASMA; TENOFOVIR; ASSAY;
D O I
10.1093/chromsci/48.3.219
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A sensitive, accurate, and precise liquid chromatography-mass spectrometry assay for the determination of tenofovir (TNF) in human vaginal tissue was developed and validated. After homogenization of the tissue, solid-phase extraction on Varian Bond Elut-C-18 column was used for sample clean up. Chromatographic separation of TNF and the internal standard (tolbutamide) was achieved with a Varian Polaris 3C(18)-A reversed-phase analytical column (1150 mm x 2 mm). A gradient method using 0.1% formic acid in water and 0.1% formic acid in acetonitrile was employed. Detection of TNF and tolbutamide was achieved by electrospray ionization mass spectrometry in the positive ion mode using 288.05 and 271.00 m/z, respectively. Linear TNF calibration curves were obtained between 1-1,000 ng/mL with a correlation coefficient (r(2)) greater than 0.999. Intra- and inter-day accuracy for TNF ranged from 89.7% and 109.4% and from 97.3% and 104.9%, and precision ranged from 1.3% and 10.9% and 2.6% and 9.0%, respectively. This is the first validated method developed to quantitate TNF in human tissues.
引用
收藏
页码:219 / 223
页数:5
相关论文
共 12 条
[1]  
[Anonymous], 2001, GUID IND BIOAN METH
[2]   Key elements of bioanalytical method validation for small molecules [J].
Bansal, Surendra ;
DeStefano, Anthony .
AAPS JOURNAL, 2007, 9 (01) :E109-E114
[3]   Simultaneous analysis of several antiretroviral nucleosides in rat-plasma by high-performance liquid chromatography with UV using acetic acid/hydroxylamine buffer - Test of this new volatile medium-pH for HPLC-ESI-MS/MS [J].
Bezy, V ;
Morin, P ;
Couerbe, P ;
Leleu, G ;
Agrofoglio, L .
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES, 2005, 821 (02) :132-143
[4]   Sensitive assay for determining plasma tenofovir concentrations by LC/MS/MS [J].
Delahunty, T ;
Bushman, L ;
Fletcher, CV .
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES, 2006, 830 (01) :6-12
[5]   Relevance of a combined UV and single mass spectrometry detection for the determination of tenofovir in human plasma by HPLC in therapeutic drug monitoring [J].
El Barkil, Mirna ;
Gagnieu, Marie-Claude ;
Guitton, Jerome .
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES, 2007, 854 (1-2) :192-197
[6]   Determination of tenofovir in human plasma by high-performance liquid chromatography with spectrofluorimetric detection [J].
Jullien, V ;
Tréluyer, JM ;
Pons, G ;
Rey, E .
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES, 2003, 785 (02) :377-381
[7]   Liquid chromatography-tandem mass spectrometric determination of tenofovir-diphosphate in human peripheral blood mononuclear cells [J].
King, Tracy ;
Bushman, Lane ;
Kiser, Jennifer ;
Anderson, Peter L. ;
Ray, Michelle ;
Delahunty, Thomas ;
Fletcher, Courtney V. .
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES, 2006, 843 (02) :147-156
[8]   Safety and tolerability of tenofovir vaginal gel in abstinent and sexually active HIV-infected and uninfected women [J].
Mayer, KH ;
Maslankowski, LA ;
Gai, F ;
El-Sadr, WM ;
Justman, J ;
Kwiecien, A ;
Mâsse, B ;
Eshleman, SH ;
Hendrix, C ;
Morrow, K ;
Rooney, JF ;
Soto-Torres, L .
AIDS, 2006, 20 (04) :543-551
[9]  
PORSHE DJ, 2002, J ASSOC NURSE AIDS C, V13, P100
[10]   Simultaneous quantification of emtricitabine and tenofovir in human plasma using high-performance liquid chromatography after solid phase extraction [J].
Rezk, NL ;
Crutchley, RD ;
Kashuba, ADM .
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES, 2005, 822 (1-2) :201-208