A simple method for the quantification of tipranavir, a new non-peptidic protease-inhibitor, was developed. An internal standard, prazepam, was added to 100 microl of plasma before a liquid-liquid extraction by 3 ml of tert-butyl methyl ether. The extracts were evaporated to dryness and reconstituted with 100 microl of mobile phase before being injected in the chromatographic system. The separation was made on a C8 column using sodium acetate buffer (pH 5):methanol:acetonitrile (35:30:35, v/v/v) as mobile phase. The detection was performed at a wavelength of 260 nm. The method was linear and has been validated over a concentration range of 2-80 mg/l. The mean precision and accuracy of the method were respectively, 10.5 and -9.1%. The mean recovery was 70.8%.
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http://dx.doi.org/10.1016/j.jchromb.2005.10.024 | DOI Listing |
J Pharm Anal
December 2016
Clinical Pharmacology Unit, CNR Institute of Neuroscience, Department of Biomedical and Clinical Sciences, L. Sacco University Hospital, Università di Milano, 20157 Milan, Italy.
A new method using high-performance liquid chromatography coupled with ultra violet detection (HPLC-UV) was developed and validated for the simultaneous quantification of atazanavir, dolutegravir, darunavir, efavirenz, etravirine lopinavir, raltegravir, rilpivirine and tipranavir in human plasma. For the first time we reported here the development and validation of an HPLC-UV assay to quantify the frequently administered 9 antiretroviral compounds including dolutegravir and rilpivirine. A simple solid phase extraction procedure was applied to 500 µL aliquots of plasma.
View Article and Find Full Text PDFJ Pharm Biomed Anal
March 2011
Laboratory of Clinical Pharmacology and Pharmacogenetics, Department of Infectious Diseases, University of Torino, Amedeo di Savoia Hospital, Corso Svizzera 164, Turin, Italy.
A sensitive and accurate high performance liquid chromatography-mass spectrometric (HPLC-MS) method for the intracellular determination of 14 antiretroviral drugs in peripheral blood mononuclear cells (PBMCs) for HIV+ patients was validated. PBMCs are isolated by Ficoll density gradient centrifugation and cells count and the relative mean volume is performed with a Coulter(®) instrument. Extraction of drugs from PBMCs pellets was obtained with methanol:water (70:30, v/v), with quinoxaline added as internal standard, after a sonication step.
View Article and Find Full Text PDFClin Chem Lab Med
August 2010
Department of Pharmacy and Pharmacology, Slotervaart Hospital, Amsterdam, The Netherlands.
Background: We previously developed a method for the simultaneous determination of the human immunodeficiency protease inhibitors: amprenavir, atazanavir, darunavir, indinavir, lopinavir, nelfinavir, ritonavir, saquinavir and tipranavir, the active nelfinavir metabolite M8 the non-nucleoside reverse transcriptase inhibitors efavirenz, nevirapine and etravirine and the internal standards dibenzepine, (13)C(6)-efavirenz, D5-saquinavir and D6-indinavir in plasma using liquid chromatography coupled with tandem mass spectrometry with a Sciex API3000 triple quadrupole mass spectrometer and an analytical run time of only 10 min. We report the transfer of this method from the API3000 to a supposedly less sensitive Sciex API365 mass spectrometer.
Methods: We describe the steps that were undertaken to optimize the sensitivity and validation of the method that we transferred.
Clin Pharmacol Ther
June 2010
Division of Pharmacotherapy and Experimental Therapeutics, School of Pharmacy, University of North Carolina at Chapel Hill, Chapel Hill, North Carolina, USA.
The effects of tipranavir/ritonavir (TPV/r) on hepatic and intestinal P-glycoprotein (P-gp) and cytochrome P450 (CYP) enzyme activity were evaluated in 23 volunteers. The subjects received oral (p.o.
View Article and Find Full Text PDFTher Drug Monit
December 2009
Laboratoire de Pharmacocinétique et Toxicologie, Hôpital de la Timone, Marseille, France.
Background: Raltegravir is the first human immunodeficiency virus-1 (HIV-1) integrase inhibitor used in treatment-experienced patients who have evidence of viral replication and HIV-1 strains resistance to multiple antiretroviral regimens. Etravirine is a novel NNRTI, active against HIV-1 strains harboring multiple NNRTI mutations. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the quantification of raltegravir, etravirine, and 9 other antiretroviral agents (amprenavir, atazanavir, darunavir, efavirenz, indinavir, lopinavir, ritonavir, saquinavir, and tipranavir) in plasma at the concentrations associated with therapy.
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