A novel, rapid, and sensitive liquid chromatography-tandem mass spectrometric method was developed and validated for the simultaneous quantification of tenofovir, emtricitabine, and efavirenz in human plasma. Nevirapine was used as an internal standard. The analytes and the internal standard were extracted from human plasma sample by solid-phase extraction technique (SPE). The reconstituted samples were chromatographed on a Chromolith ROD C18 column (50 × 4.6 mm; 5 μ) by gradient elution using a mixture of ammonium acetate buffer (5 mM) and 0.1% formic acid in acetonitrile as the mobile phase at a flow rate of 1.0 mL min−1. The calibration curve obtained was linear (r2 ≥ 0.9990) over the concentration range of 2.5–650 ng mL−1 for tenofovir and 10–4000 ng mL−1 for emtricitabine and efavirenz. The results of the intra- and inter-day precision and accuracy studies were well within the acceptable limits. A run time of 2.5 min for each sample made it possible to analyze more than 300 plasma samples per day. The proposed method was found to be applicable to clinical studies, and the authenticity in the measurement of clinical data is demonstrated through incurred samples reanalysis (ISR).
US Department of Health and Human Services, 2008
C.C.J. Carpenter, M.A. Fischl, and S.M. Hammer, J. Am. Med. Assoc., 277, 962 (1997)
R.K. Nirogi, B. Gopinadh, K. Vishwottam, M. Koteshwara, K. Prashanth, A. Raghupathi, and K. Mukkanti, Biomed. Chromatogr., 23, 371 (2009)
Mukkanti K., '' (2009) 23Biomed. Chromatogr.: 371-.
Mukkanti K.Biomed. Chromatogr.200923371)| false
US DHHS, FDA, CDER. Guidance for Industry: Bioanalytical Method validation. U.S. Department of Health and Human Services, Food and Drug Administration, Center for Drug Evaluation and Research (CDER), Center for Veterinary Medicine (CV), 2001. Available at: http://www/fda.gov/cder/guidance/index.htm.
'', in Guidance for Industry: Bioanalytical Method validation, (2001) -.
Guidance for Industry: Bioanalytical Method validation2001)| false
D.M. Fast, M. Kelley, and C.T. Viswanathan, AAPS. J., 11, 238 (2007)
Viswanathan C.T., '' (2007) 11AAPS. J.: 238-.
Viswanathan C.T.AAPS. J.200711238)| false
N.M. Hiren, G.J. Arvind, P. Ashutosh, G. Noel, S. Mallika, and S. Pranav, J. Chromatgr., B., 853, 320 (2007)
Pranav S., '' (2007) 853J. Chromatgr., B.: 320-.
Pranav S.J. Chromatgr., B.2007853320)| false
A.M. Anita, H. John, M. Mark, H. James, K. Sanjeev, and P.K. Brian, J. Acquired Immune Defic. Syndr., 46, 167 (2007)
Brian P.K., '' (2007) 46J. Acquired Immune Defic. Syndr.: 167-.
Brian P.K.J. Acquired Immune Defic. Syndr.200746167)| false
B.T. De and J. Wieling, Bioanalysis, 3, 983 (2011)
Editors(s) Danica Agbaba (University of Belgrade, Belgrade, Serbia);
Ivana Stanimirova-Daszykowska (University of Silesia, Katowice, Poland),
Monika Waksmundzka-Hajnos (Medical University of Lublin, Lublin, Poland)
R. Bhushan (The Indian Institute of Technology, Roorkee, India)
J. Bojarski (Jagiellonian University, Kraków, Poland)
B. Chankvetadze (State University of Tbilisi, Tbilisi, Georgia)
M. Daszykowski (University of Silesia, Katowice, Poland)
T.H. Dzido (Medical University of Lublin, Lublin, Poland)
A. Felinger (University of Pécs, Pécs, Hungary)
K. Glowniak (Medical University of Lublin, Lublin, Poland)
B. Glód (Siedlce University of Natural Sciences and Humanities, Siedlce, Poland)
K. Kaczmarski (Rzeszow University of Technology, Rzeszów, Poland)
H. Kalász (Semmelweis University, Budapest, Hungary)
I. Klebovich (Semmelweis University, Budapest, Hungary)
A. Koch (Private Pharmacy, Hamburg, Germany)
Ł. Komsta (Medical University of Lublin, Lublin, Poland)
P. Kus (Univerity of Silesia, Katowice, Poland)
D. Mangelings (Free University of Brussels, Brussels, Belgium)
E. Mincsovics (Corvinus University of Budapest, Budapest, Hungary)
G. Morlock (Giessen University, Giessen, Germany)
J. Sherma (Lafayette College, Easton, PA, USA)
R. Skibiński (Medical University of Lublin, Lublin, Poland)
B. Spangenberg (Offenburg University of Applied Sciences, Germany)
T. Tuzimski (Medical University of Lublin, Lublin, Poland)
Y. Vander Heyden (Free University of Brussels, Brussels, Belgium)
A. Voelkel (Poznań University of Technology, Poznań, Poland)
B. Walczak (University of Silesia, Katowice, Poland)
W. Wasiak (Adam Mickiewicz University, Poznań, Poland)