Preconcentration and Detection of Gefitinib Anti-Cancer Drug Traces from Water and Human Plasma Samples by Means of Magnetic Nanoparticles

Along of widespread application of anti-cancer drug Gefitinib (GEF), it appears in human body fluids as well as clinical wastewater. Consequently, a reliable and easy-to-adapt detection technique is of essential importance to quantify the drug in different media. The extraction and quantitative detection of anti-cancer drug Gefinitib (GEF) is demonstrated based on a straightforward and efficient magnetic nanoparticle-assisted preconcentration route from water and human plasma samples. Iron oxide magnetic nanoparticles (Fe3O4) have been prepared with an average particle size of 15 nm and utilized as extractible adsorbents for the magnetic solid-phase extraction (MSPE) of GEF in aqueous media. The method is based on MSPE and preconcentration of GEF followed by High-Performance Liquid Chromatography-Ultraviolet Detection (HPLC-UV). The yield of GEF extraction under the optimum MSPE conditions were 94% and 87% for water and plasma samples, respectively. The chromatographic separation was carried out isocratically at 25 °C on a Phenomenex C8 reversed phase column (150 mm × 4.6 mm, with 5 µm particle size). The proposed method was linear over concentration ranges of 15.0–300.0 and 80.0–600.0 ng/mL for water and plasma samples with limits of detection of 4.6 and 25.0 ng/mL in a respective order. Relative standard deviations (%RSD) for intra-day and inter-day were 0.75 and 0.94 for water samples and 1.26 and 1.70 for plasma samples, respectively. Using the magnetic nanoparticles (MNPs) as loaded drug-extractors made the detection of the anti-cancer drug environmentally friendly and simple and has great potential to be used for different drug-containing systems

Development and validation of stability indicating method for determination of sertraline following ICH guidlines and its determination in pharmaceuticals and biological fluids

<p>Abstract</p> <p>Background</p> <p>Sertraline is a well known antidepressant drug which belongs to a class called selective serotonin reuptake inhibitor. Most published methods do not enable studying the stability of this drug in different stress conditions.</p> <p>Results</p> <p>Two new methods were developed for the determination of sertraline (SER). Both methods are based on coupling with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) in borate buffer of pH 7.8 and measuring the reaction product spectrophotometrically at 395 nm (Method I) or spectrofluorimetrically at 530 nm upon excitation at 480 nm (Method II). The response-concentration plots were rectilinear over the range 2-24 μg/mL and 0.25-5 μg/mL for methods I and II respectively with LOD of 0.18 μg/mL and 0.07 μg/mL, and LOQ of 0.56 μg/mL and 0.21 μg/mL for methods I and II, respectively.</p> <p>Conclusion</p> <p>Both methods were applied to the analysis of commercial tablets and the results were in good agreement with those obtained using a reference method. The fluorimetric method was further applied to the in vivo determination of SER in human plasma. A proposal of the reaction pathway was presented. The spectrophotometric method was extended to stability study of SER. The drug was exposed to alkaline, acidic, oxidative and photolytic degradation according to ICH guidelines. Moreover, the method was utilized to investigate the kinetics of oxidative degradation of the drug. The apparent first order rate constant and t_1/2of the degradation reaction were determined.</p

Studying the quenching resulted from the formation of an association complex between olsalazine or sulfasalazine with acriflavine

We report the detection and quantification of important ulcerative colitis drugs olsalazine (OLS) and sulfasalazine (SUL) by the spectrofluorometric method. The proposed method was optimized and validated by using the quenching effect on the acriflavine fluorescence. The method was applied on the detection and quantification of OLS and SUL under optimized conditions showing the calibration curves were linear (range: 1.0–10.0 µg ml−1), with correlation coefficients R2 of 0.9999 for both drugs. The limits of detection (LOD) and quantification (LOQ) were 53 and 104 ng ml−1 for the OLS and 160 and 315 ng ml−1 for the SUL. This method permitted the analysis of OLS and SUL in their pure and pharmaceutical forms. The proposed spectrofluorimetric method was also evaluated against ‘green’ criteria and all the experimental results make it an eco-friendly and safe method for the detection of OLS and SUL

Full validation corrected_TEB

Calibration data for TE

Spectroscopic strategies for quantitation of varenicline in pharmaceutical preparations and content uniformity testing

Herein, two new facile methods were examined for varenicline determination using erythrosine. The latter is a food additive that has been recently investigated as a fluorescent dye for the determination of drugs. In the first method, the fluorescence of erythrosine B was quenched quantitatively by increasing the concentration of varenicline through ion-pair complex formation. This linear response was a basis for the spectrofluorimetric method used for varenicline quantitation in pure and dosage forms. The quenching is correlated with the concentration linearly over the range of 0.4–4.0 µg ml−1 at 550 nm after excitation at 528 nm with a correlation coefficient of 0.9993. Different parameters were investigated to reach the optimal conditions with the highest sensitivity and repeatability. The second method is depending on measuring the formed complex by spectrophotometry at 550 nm over the range of 1.0–10.0 µg ml−1 with an excellent correlation coefficient of 0.9999. The suggested methods were validated consistently with ICH guidelines, with acceptable results. The procedures were used to test the uniformity of content of Champix tablets. By comparing with the previous spectroscopic method, there was no significant difference as revealed from the calculated Student t-test and variance ratio F-test values

Full validation_BAM

Calibration data for BA

synthetic mixequal conc 3.2 micro

First derivative synchronous spectra of TEB, BAM and their synthetic mixture (concentration of each 3.2 microgram/mL

Data from: Synchronous fluorescence as a green and selective tool for simultaneous determination of bambuterol and its main degradation product, terbutaline

A green, sensitive and cost-effective method is introduced in this research for the determination of bambuterol and its main degradation product; terbutaline simultaneously relied on the synchronous spectrofluorimetric technique. First derivative synchronous spectrofluorimetric amplitude is measured at Δλ=20 nm, so bambuterol can be quantitated at 260 nm, and terbutaline can be measured at 290 nm, each at the zero crossing point of the other. The amplitude-concentration plots were linear over the concentration ranges of 0.2-6.0 g/mL and 0.2-4.0 g/mL for both bambuterol and terbutaline, respectively. Official guidelines were followed to calculate the validation parameters of the proposed method. The low values of LODs 0.023, 0.056 g/mL and LOQs 0.071, 0.169 g/mL for bambuterol and terbutaline, respectively point out to the sensitivity of the method. Bambuterol is a prodrug for terbutaline, and the latter is considered its degradation product so the established method could be regarded as a stability-indicating one. Moreover, the proposed method is utilized for the analysis of BAM and TEB in their single ingredient preparations and the results revealed statistical agreement with the reference method. The suggested method, being simple and low cost procedure, is superior to the previously published methods which need more sophisticated techniques, longer analysis time and highly toxic solvents and reagents. It could be considered as an ecofriendly analytical procedure

Simultaneous determination of cetirizine, phenyl propanolamine and nimesulide using third derivative spectrophotometry and high performance liquid chromatography in pharmaceutical preparations

Abstract Background The combination between cetirizine (CET), phenylpropanolamine (PPA) and nimesulide (NMS) under trade name Nemeriv Cp tablet is prescribed for nasal congestion, cold, sneezing, and allergy. Among all published methods for the three drugs; there is no reported method concerning estimation of CTZ, PPA and NMS simultaneously and this motivates us to develop new and simple methods for their assay in pure form and tablet preparations. Results Two new methodologies were described for the simultaneous quantification of cetirizine (CTZ), PPA and NMS. Spectrophotometric procedures relies on measuring the amplitudes of the third derivative curves at 238 nm for CTZ, 218 nm for PPA and 305 nm for NMS. The calibration graphs were rectilinear over the ranges of 8–90 µg/mL for CTZ, 20–100 µg/mL for PPA and 20–200 µg/mL for NMS respectively. Regarding the HPLC method; monolithic column (100 mm × 4.6 mm i.d) was used for the separation. The used mobile phase composed of 0.1 M phosphate buffer and methanol in the ratio of 40:60, v/v at pH 7.0. The analysis was performed using UV detector at 215 nm. Calibration curves showed the linearity over concentration ranges of 5–40, 10–100 and 10–120 µg/mL for CTZ, PPA and NMS. Conclusion Application of the proposed methods to the laboratory prepared tablets was carried out successfully. The results were compared with those obtained from previously published methods and they were satisfactory. Graphical abstract Graphical abstract represents the chemical structures, representative chromatogram for the HPLC separation of a PPA, b NMS and c CTZ and third derivative absorption spectra of a PPA, b NMS and c CTZ for the spectrophotometric method