Direct and fast capillary zone electrophoretic method for the determination of Gleevec and its main metabolite in human urine.

A capillary zone electrophoretic (CZE) method was investigated for the determination of Gleevec and its main metabolite (N-demethylated piperazine derivative) in human urine using a fused-silica capillary (75 microm I.D.x60 cm total length, 10 cm effective length). The separation was performed with an hydrodynamic injection time of 10 s (0.5 p.s.i.) a voltage of -25 kV, a capillary temperature of 25 degrees C and a 100 mM phosphoric acid adjusted to pH 2 with the addition of triethanolamine. Under these conditions, the analysis takes about 5 min. A linear response over the 0.4-30.0 mg l(-1) concentration range was investigated for two compounds. A dilution of the sample was the only step necessary before the electrophoresis analysis. Detection limits of 0.1 mg l(-1) for Gleevec and its metabolite (S/N=3) were obtained. The developed method is easy, rapid and sensitive and has been applied to determine Gleevec and its main metabolite in clinical urine samples.

Micellar electrokinetic capillary chromatography as an alternative method for the determination of ethinylestradiol and levo-norgestrel.

A method for quantifying of ethinylestradiol (ETE) and levo-norgestrel (LEV) in pharmaceutical products by micellar electrokinetic chromatography (MEKC) is described. The separation was carried out at 25 degrees C and 25 kV, using a 20 mM borate buffer (pH 9.2), 15 mM sodium dodecylsulfate (SDS) in 30% acetonitrile/water (v/v). Under these conditions the analysis takes about 7 min. The method has been applied for quantifying both compounds in six different commercial contraceptives and the proposed method gave good results when compared with a reference liquid chromatographic (LC) method.

Voltammetric determination of Imatinib (Gleevec) and its main metabolite using square-wave and adsorptive stripping square-wave techniques in urine samples.

The voltammetric behaviour of Imatinib (STI 571) and its main metabolite (N-demethylated piperazine derivative) were studied by square-wave techniques, resulting in to two methods for their determination in aqueous and urine samples at pH 2. The application of the square-wave (SW) without the adsorptive accumulation and voltammetric stripping (AdSV) exhibit a peak at a reduction potential of -0.70V for an accumulation potential of -0.45V. The sensitivity was higher for the stripping technique because a signal four times higher than that provided by the square-wave method without the previous accumulation was obtained. Due to the fact that Imatinib and its metabolite show the same voltammetric reduction process, some experiments were performed in order to compare the voltammetric response of Imatinib and its main metabolite in a similar ratio than that of the therapeutic concentration. The calibration curve for Imatinib in urine was linear in the range from 1.9x10(-8) to 1.9x10(-6)M in stripping mode with an accumulation time (t(acc)) of 10s. The relative standard deviations obtained for concentration levels of Imatinib as low as 2.0x10(-7)M for square-wave was 2.17% (n=9) and for stripping square-wave was 2.65% (n=9) in the same day. The limits of detection for square-wave and stripping square-wave were 5.55x10(-9) and 5.19x10(-9)M, respectively. Thus, the presented method are straightforward, rapid and sensitive and has been applied to the determination of Imatinib and its main metabolite altogether in urine samples from real patients.

Simultaneous determination of ethinylestradiol and levonorgestrel in oral contraceptives by derivative spectrophotometry.

A method for determining ethinylestradiol (ETE) and levonorgestrel (LEV) in mixtures by first-derivative spectrophotometry is described. The procedure does not require any separation step. Measurements are made at the zero-crossing wavelengths and the calibration graphs are linear up to 26 and 33 micrograms ml-1 of ETE and LEV, respectively. The method was applied to the determination of both compounds in five different Spanish commercial low-dose oral contraceptives. Similar results were obtained by an HPLC method.

Determination of Clobazam, Clorazepate, Flurazepam and Flunitrazepam in pharmaceutical preparations.

The separation of four benzodiazepines (Flurazepam, Flunitrazepam, Clobazam and Clorazepate) in pharmaceutical products by micellar electrokinetic chromatography (MEKC) is described. It was carried out at 25 degrees C and 25 kV by using a 57 cm (50 cm to the detector)x75 mum i.d. fused silica capillary and a 15 mM borate buffer (pH 9.2), 35 mM sodium dodecylsulfate (SDS) and 35 mM sodium deoxycholate water solution. Under these conditions, the analysis was performed in 8 min with acceptable limits of quantification (between 3 and 5 mg l(-1)). The method has been applied for quantifying these benzodiazepines in serum and different commercial formulations with recoveries near 100%.

Cyclodextrin enhanced spectrofluorimetric determination of fluoxetine in pharmaceuticals and biological fluids.

The characteristics of host-guest complexation between methyl-beta-cyclodextrin and fluoxetine were investigated by fluorescence spectrometry. A 1:1 stoichiometry of the complex was established and association constant of 4.35x10(-3) M(-1) at 20 degrees C was calculated. A spectrofluorimetric method for the determination of fluoxetine, with a range of application between 40 and 1000 mug l(-1) was developed. Overall least squares regression was used to find the straight line that fitted the experimental data. The detection limit, according to the error propagation theory, was 9.6 mug l(-1) and the detection limit proposed by Clayton was 15.8 mug l(-1). Repeatability and relative standard deviation were also determined according to this theory, with satisfactory results. The method was successfully applied to the determination of fluoxetine in pharmaceuticals and biological fluids.

Determination of sildenafil citrate (viagra) and its metabolite (UK-103,320) by square-wave and adsorptive stripping square-wave voltammetry. Total determination in biological samples.

The voltammetric behaviour of Sildenafil citrate (SC) and its main metabolite UK-103,320 (UK) was studied by square wave techniques, leading to two methods for its total determination in biological samples (urine and human serum). The application of the square wave (SW), without the adsorptive accumulation, shows a maximum response at -0.950V. The effect of experimental parameters that affect this determination are discussed. The stripping technique, proved to be more sensitive, yielding signals three times larger than those obtained by applying a square wave scan without the previous accumulation. Two calibration graphs to determine total SC and UK concentration were established. Calibration graph in urine sample was linear in the range 4.4x10(-8) to 4.8x10(-7)M by the stripping mode with an accumulation time of 10s. In the same conditions but in serum sample regression line was linear in the range 3.4x10(-8) to 9.7x10(-7)M. The two proposed methods (SW and square-wave adsorptive stripping voltammetry (SWAdSV)) were applied to the total concentration analysis in eight different biological samples by the standard addition method with satisfactory results in the four different serum samples by the SW and in the four urines by SWAdSV.