Ibuprofen In Urine Research Articles

Deep eutectic solvent-based ultrasound-assisted liquid–liquid microextraction of ibuprofen prior to HPLC-UV determination

ABSTRACT In this study, accurate and sensitive determination of ibuprofen in blood, urine, pharmaceutical tablet, syrup, and water samples was accomplished with the combination use of deep eutectic solvent-based ultrasound-assisted liquid–liquid microextraction (DES-UA-LLME) and high-performance liquid chromatography-ultraviolet visible detection system. The most important advantage of this method is that it can be used in the determination of ibuprofen without affecting the matrix environment of a wide range of samples. Ibuprofen in the sample phase was extracted to 500 µL of deep eutectic solvents phase (ChCl:Ph at 1:4 molar ratios) at pH 3.0. The influence of analytical parameters, such as pH of sample solution, the molar ratio of deep eutectic solvents components, tetrahydrofuran volume, and volume of DESs, were optimised in details. The preconcentration factor (PF), the detection limit (DL), intraday, and interday relative standard deviations (RSD, %) for the developed DES-UA-LLME/HPLC procedure were found as 30, 0.4 µg L−1, 1.74%, and 4.68%, respectively. The developed DES-UA-LLME was successfully used for the determination of ibuprofen in urine, blood, pharmaceutical tablet, syrup, and water samples.

Enhanced fluorescence of CdTe quantum dots capped with a novel nonionic alginate for selective optosensing of ibuprofen

In this work, we report the development of highly fluorescent materials for the selective and sensitive detection of ibuprofen (IBP). Novel nonionic alginate polymers and their CdTe quantum dots (QDs) were synthesized and characterized using FT-IR, 1H NMR, TEM, UV–vis, and EDAX techniques. The nonionic alginate-capped CdTe QDs show tremendously enhanced fluorescence intensity (∼30 times), increased quantum yields up to 49% (∼10 times), and improved biocompatibility (IC50=1414μgmL−1) compared with that of pristine CdTe QDs. The synthesized CdTe QD-Al-PEG2000(SH)2 was successfully used as an optical sensor to detect IBP based on multiple hydrogen bonding interactions between the sensor and IBP. The quenching effect on the fluorescence intensity of the sensor showed very good linearity in the range 1.0–30μmolL−1 (R2=0.9959) and a remarkably low detection limit of 0.004μmolL−1, (S/N=3). The sensor was highly selective to IBP in the presence of other potentially competing compounds and was successfully applied for the detection of IBP in urine and human serum samples with good recoveries. This reported method is expected to open new possibilities for the cost-effective, non-toxic, selective, and highly sensitive optosensing of IBP.

Estimation of ibuprofen in urine and tablet formulations by transmission Fourier Transform Infrared spectroscopy by partial least square

A rapid, reliable and cost effective analytical procedure for the estimation of ibuprofen in pharmaceutical formulations and human urine samples was developed using transmission Fourier Transform Infrared (FT-IR) spectroscopy. For the determination of ibuprofen, a KBr window with 500μm spacer was used to acquire the FT-IR spectra of standards, pharmaceuticals as well as urine samples. Partial least square (PLS) calibration model was developed based on region from 1807 to 1461cm−1 using ibuprofen standards ranging from 10 to 100μgml−1. The developed model was evaluated by cross-validation to determine standard error of the models such as root mean square error of calibration (RMSEC), root mean square error of cross validation (RMSECV) and root mean square error of prediction (RMSEP). The coefficient of determination (R2) achieved was 0.998 with minimum errors in RMSEC, RMSECV and RMSEP with the value of 1.89%, 1.63% and 4.07%, respectively. The method was successfully applied to urine and pharmaceutical samples and obtained good recovery (98–102%).

Highly sensitive chiral analysis in capillary electrophoresis with large-volume sample stacking with an electroosmotic flow pump

To improve the sensitivity in chiral analysis by capillary electrophoresis without loss of optical resolution, application of large-volume sample stacking with an electroosmotic flow pump (LVSEP) was investigated. Effects of the addition of cyclodextrin (CD) into a running solution on the LVSEP preconcentration was theoretically studied, where the preconcentration efficiency and effective separation length would be slightly increased if the effective electrophoretic velocity (vep,eff,BGS) of the analytes was decreased by interacting with CD. In LVSEP-CD-modified capillary zone electrophoresis (CDCZE) and LVSEP-CD electrokinetic chromatography with reduced vep,eff,BGS, up to 1000-fold sensitivity increases were achieved with almost no loss of resolution. In LVSEP-CD-modified micellar electrokinetic chromatography of amino acids with increased vep,eff,BGS, a 1300-fold sensitivity increase was achieved without much loss of resolution, indicating the versatile applicability of LVSEP to many separation modes. An enantio-excess (EE) assay was also carried out in LVSEP-CDCZE, resulting in successful analyses of up to 99.6% EE. Finally, we analyzed ibuprofen in urine by desalting with a C18 solid-phase extraction column. As a typical result, 250ppb ibuprofen was well concentrated and optically resolved with 84.0–86.6% recovery in LVSEP-CDCZE, indicating the applicability of LVSEP to real samples containing a large amount of unnecessary background salts.

Solid-phase microextraction and chiral HPLC analysis of ibuprofen in urine

A simple and rapid solid-phase microextraction method was developed for the enantioselective analysis of ibuprofen in urine. The sampling was made with a polydimethylsiloxane-divinylbenzene coated fiber immersed in the liquid sample. After desorptioning from the fiber, ibuprofen enantiomers were analyzed by HPLC using a Chiralpak AD-RH column and UV detection. The mobile phase was made of methanol–pH 3.0 phosphoric acid solution (75:25, v/v), at a flow rate of 0.45 mL/min. The mean recoveries of SPME were 19.8 and 19.1% for (−)- R-ibuprofen and (+)-( S)-ibuprofen, respectively. The method was linear at the range of 0.25–25 μg/mL. Within-day and between-day assay precision and accuracy were below 15% for both ibuprofen enantiomers at concentrations of 0.75, 7.5 and 20 μg/mL. The method was tested with urine quality control samples and human urine fractions after administration of 200 mg rac-ibuprofen.

Pharmacokinetics of Ibuprofen Enantiomers in Children with Cystic Fibrosis

Chiral inversion of R(-)- to S(+)-ibuprofen in children with cystic fibrosis was investigated. Children with cystic fibrosis (n = 38, ages 2-13 years) were administered a single oral dose of racemic ibuprofen (20 mg/kg), and the pharmacokinetics of ibuprofen was found to be stereoselective. Mean Cmax, AUC, apparent CL/F, and Varea/F of S-ibuprofen were significantly different from those of R-ibuprofen. The enantiomeric ratio of plasma AUC (S:R = 2.09:1) and of free and conjugated ibuprofen in urine (S:R = 13.9:1) of children with cystic fibrosis was not different from reported values for healthy children and adults. No significant gender difference was observed for any of the pharmacokinetic parameters determined. However, there was an inverse linear relationship between the CL/F of R-ibuprofen and age in children with cystic fibrosis. Apparent CL/F was higher in children with cystic fibrosis than previously reported for healthy children; therefore, higher doses of ibuprofen would be necessary for children with cystic fibrosis.

Stereospecific analysis of the major metabolites of ibuprofen in urine by sequential achiral-chiral high-performance liquid chromatography

A sequential achiral-chiral HPLC method has been developed for the stereospecific analysis of the two major urinary metabolites of ibuprofen, namely hydroxyibuprofen and carboxyibuprofen. Achiral analysis was carried out using a Partisil column (250×4.6 mm, 5 μm) and a mobile phase of hexane:ethanol (98.2:1.8, v/v) containing trifluoroacetic acid (TFA; 0.05%, v/v) at a flow-rate of 2.0 ml/min. The HPLC eluate containing the two metabolites was separately collected, evaporated under nitrogen and the residue dissolved in the mobile phase used for chiral chromatography. Chiral-phase analysis was carried out using a Chiralpak AD CSP (250×4.6 mm, 10 μm) with a mobile phase of hexane:ethanol (92:8, v/v) containing TFA (0.05%, v/v) at a flow-rate of 1.0 ml/min. In both assays the analytes were quantified by ultraviolet detection at a wavelength of 220 nm. Modification of the mobile-phase composition allowed the resolution of all six analytes in a single chromatographic run but with an increase in run time and consequent band broadening. The analytical method described allows the direct quantitation of the stereoisomers of both metabolites of ibuprofen in urine following the administration of therapeutic doses of the racemic drug to man.