Chiral selectors for enantioresolution and quantitation of the antidepressant drug fluoxetine in pharmaceutical formulations by 19F NMR spectroscopic method

Application of Fluorescence Spectrometry With Multivariate Calibration to the Enantiomeric Recognition of Fluoxetine in Pharmaceutical Preparations

“…14,15 Only a few studies have described the pharmaceutical analysis of FLX enantiomers using other than chromatographic methods, namely, capillary electrophoresis 16 and NMR. 17,18 The enantiomeric composition identification of biologically active chiral compounds poses special challenges to scientists in the areas of environmental and pharmaceutical research. The new strategies of enantiomer resolution include chiral analysis by nonchirooptical methods, such as molecular spectroscopy with chemometric evaluation of data.…”

Fluorine-19 nuclear magnetic resonance (19F NMR) as a powerful technique for the assay of anti-HIV drug efavirenz in human serum and pharmaceutical formulations

“…The inversion recovery pulse sequence method was employed to measure the longitudinal relaxation time (T 1 ) of efavirenz, using the T 1 cal BRUKER program, via fitting the data to the exponential equation I = I 0 + P exp(-/T 1 ) (Shamsipur et al, 2007a), where I is the intensity of efavirenz resonance at inversion delay times (= 0, 10, 0.25, 0.75, 1.00, 2.50, 5.00, 7.50, 10.00, 15.00 and 20.00 s) and I 0 is that at the equilibrium state and P is a constant.. The T 1 value thus obtained for efavirenz was 1.69 ± 0.01 s.…”

“…A number of previously published results revealed that 19 F NMR spectroscopy could be employed as a powerful selective tool to analyze different fluorinated drugs (Lenz et al, 2002;Malet-Martino et al, 2006;Martino et al, 2005;Shamsipur et al, 2003Shamsipur et al, , 2007aTalebpour et al, 2003a). In this work, the presence of three fluorine atoms in the efavirenz structure enabled us to use 19 F NMR for the selective and sensitive analysis of drug contents of human serum samples and pharmaceutical formulations.…”

Determination of enantiomeric composition of fluoxetine by synchronous fluorescence spectrometry coupled with multivariate calibration in biological samples

“…Chromatographic methods, as LC or GC with chiral columns or chiral additives into mobile phase are typical for the determination of the FLX enantiomers (Lerena et al, 2003;Li et al, 2004;Mifsud and Sqhendo, 2012;Yu et al, 2012;Ribeiro et al, 2013). Few studies of FLX chiral analysis using non-chromatography methods such as capillary electrophoresis were published (Asensi-Bernardi et al, 2013) and NMR (Ali et al, 2005;Shamsipur et al, 2007). Our research presents the feasibility of FLX chiral analysis by combination of synchronous fluorescence spectrometry and inverse MVC methods (PCR and PLS) which were compared to obtain the best resolution of the FLX enantiomers in complicate biological matrix such as urine.…”