Micellar-Enhanced Spectrofluorimetric Method for Quantification of Diclofenac Potassium in Pure Form, in Pharmaceutical Preparations and Human Plasma

2021 ◽  
Vol 58 (6) ◽  
pp. 427-434
Author(s):  
Muhammad Naeem Khan ◽  
Irum ◽  
Saba Gul ◽  
Muslima ◽  
Muhammad Mursaleen
Keyword(s):  
Human Plasma ◽  
Limit Of Detection ◽  
Sodium Dodecyl ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Products ◽  
Pure Form ◽  
Fluorescence Signal ◽  
Spectrofluorimetric Method ◽  
Relative Standard

Abstract A rapid, simple and economical spectrofluorimetric method for the determination of diclofenac potassium in pure form, in pharmaceutical preparations and in human plasma has been developed. The method is based on the enhancement of the fluorescence signal of diclofenac potassium by the addition of sodium dodecyl sulphate in McIvaine buffer with a pH of 5. Different experimental conditions such as buffer type, pH, type and concentration of surfactants were investigated. The fluorescence intensity of the solution was recorded at 361 nm after excitation at 243 nm. The method shows linearity in the concentration range of 0.2 μg mL–1–10 μg mL–1 with a good correlation coefficient of 0.997. The relative standard deviation value was 3.62 (n = 7). The limit of detection and limit of quantification were calculated to be 2.84 × 10–3 μg mL–1 and 9.47 × 10–3 μg mL-1, respectively. The effect of excipients and co-administrated drugs was investigated and no interference was observed. The method was successfully applied for the determination of diclofenac potassium in pure form, in pharmaceutical products and in human plasma. The percentage recoveries obtained ranged from 100.25% to 102.16% for pure form and 97.50% to 102.00% for pharmaceutical products and from 98.50% to 101.67% for human plasma.

scholarly journals Solvolysis kinetic study and direct spectrofluorimetric analysis of the fungicide benomyl in natural waters

2014 ◽  
Vol 33 (2) ◽  
pp. 237 ◽  
Author(s):  
Diène Diègane Thiare ◽  
Abdourakhmane Khonté ◽  
Diegane Sarr ◽  
Cheikh Diop ◽  
Mame Diabou Gaye-Seye ◽  
...  
Keyword(s):  
Aqueous Solution ◽  
Aqueous Solutions ◽  
Natural Waters ◽  
Limit Of Detection ◽  
Sodium Dodecyl ◽  
Fluorescence Signal ◽  
Aqueous Solvent ◽  
Spectrofluorimetric Method ◽  
Relative Standard ◽  
Triton X

<p>A direct spectrofluorimetric method for the quantitative analysis of benomyl in natural waters is described. Benomyl is an instable, fluorescent fungicide that mainly decomposes into carbendazim and n-butyl-isocyanate in organic and aqueous solutions. The kinetics of benomyl solvolysis reactions were investigated in organic solvents (methanol and acetonitrile) and in aqueous solvent systems, including β–cyclodextrin (β-CD), sodium dodecyl sulfate (SDS), dodecyltrimethylammonium chloride (DTAC), cetyltrimethylammonium chloride (CTAC), cetyltrimethylammonium hydroxide (CTAOH), Brij-700, Triton X-100 and water, at different pH and/or NaOH concentrations. The benomyl fluorescence signal was found to be quasi-completely stable in 10<sup>-2</sup> M NaOH aqueous solution, various alkaline (10<sup>-2</sup> M NaOH) organized media, β-CD neutral solution and Triton X-100 aqueous solutions of different pH. Based on these results, a direct spectrofluorimetric analytical method was developed for the determination of benomyl in 10<sup>-2</sup> M NaOH aqueous solution and Triton X-100 solutions (pH7 and 10<sup>-2</sup> M NaOH), with wide linear dynamic range (LDR) values of two to three orders of magnitude, very low limit of detection (LOD) and limit of quantification (LOQ) values of, respectively, 0.002-0.5 ng/mL and 0.007-2.0 ng/mL, and small relative standard deviation (RSD) values of 0.2-1.7 %, according to the medium. This direct spectrofluorimetric method was applied to the evaluation of benomyl residues in natural waters, with satisfactory recovery values (87-94%).</p>

A fast spectrofluorimetric method for determination of carbinoxamine maleate in the nano-molar range. Application to pharmaceutical preparations, biological fluids and stability studies

2018 ◽  
Vol 10 (31) ◽  
pp. 3851-3858 ◽  
Author(s):  
Fatma Ahmed Aly ◽  
Nahed EL-Enany ◽  
Heba Elmansi ◽  
Amany Nabil
Keyword(s):  
Human Plasma ◽  
Biological Fluids ◽  
Pharmaceutical Preparations ◽  
Pure Form ◽  
Stability Studies ◽  
Spiked Human Plasma ◽  
Spectrofluorimetric Method

Carbinoxamine maleate (CBX), which is a common ingredient of cold and cough treatment preparations, is determined by a sensitive, simple and convenient spectrofluorimetric method in its pure form, pharmaceutical preparations and spiked human plasma.

Preconcentration and determination of ranitidine hydrochloride in real samples by using modified magnetic iron oxide nanoparticles

2016 ◽  
Vol 94 (1) ◽  
pp. 9-14 ◽  
Author(s):  
Elaheh Konoz ◽  
Amir H.M. Sarrafi ◽  
Hamed Sahebi
Keyword(s):  
Human Plasma ◽  
Ph Value ◽  
Limit Of Detection ◽  
Solid Phase ◽  
High Surface ◽  
Sodium Dodecyl ◽  
Magnetic Iron Oxide Nanoparticles ◽  
Ranitidine Hydrochloride ◽  
Relative Standard

This method shows a novel, fast, and simple magnetic solid-phase extraction (SPE) and spectrophotometric procedure for preconcentration and determination of ranitidine hydrochloride in human plasma and aquatic samples by using Fe3O4 nanoparticles (NPs) modified by sodium dodecyl sulfate (SDS) as an extractor. The unique properties of Fe3O4 NPs including high surface area and strong magnetism were utilized effectively in the magnetic SPE process. The determination method is based on the SDS-coated Fe3O4 NPs with extracted ranitidine-HCl, which was subsequently monitored spectrophotometrically at λmax = 320 nm. Effects of different parameters influencing the extraction efficiency of ranitidine-HCl including the pH value, amount of SDS, and Fe3O4 NPs, extraction time, desorption solvent, desorption time, and sample volume were optimized. Under optimized conditions, the method was successfully applied to the extraction of ranitidine-HCl from human plasma and aquatic samples. The extraction recovery in human plasma and different matrixes of waters were investigated and values of 89.0%–103.4% were obtained. The calibration graph for the determination of ranitidine-HCl was linear in the range of 0.025–1.50 μg mL−1 with R2 = 0.9946. The limit of detection of the proposed method was 7.5 × 10−3 μg mL−1. The repeatability and reproducibility (relative standard deviation) of the mentioned method were 0.83% and 1.22%, respectively. The experimental results showed that the proposed method was feasible for the analysis of ranitidine-HCl in environmental and biological samples.

scholarly journals Spectrophotometric Indirect Determination of Captopril through Redox Reaction with n-bromosuccinimide and RB dye in Pharmaceutical Products

2020 ◽  
Vol 8 (2) ◽  
pp. 8-14
Author(s):  
Dashne M. Kokhasmail ◽  
Tara F. Tahir ◽  
Kurdistan F. Azeez
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Reference Method ◽  
Pharmaceutical Products ◽  
Indirect Determination ◽  
Relative Standard ◽  
Experimental Parameters ◽  
Replicated Measurements ◽  
Student’S T

A simple, accurate, and sensitive method for the spectrophotometric determination of captopril in bulk and dosage forms is reported. The method is based on the bromination of captopril with excess solution of n-bromosuccinimide (NBS) in HCl acid medium. The excess NBS is pursued by the assessment of the residual NBS based on its ability to bleach the rhodamine B dye and measuring the absorbance at 555 nm. The amount of NBS reacted coincides to the drug content. The different experimental parameters influencing the development and stability of the color are precisely studied and optimized. Beer’s law is valid within a concentration range of 0.3–1.0 μg/mL with a correlation coefficient R2 = 0.991. The limit of detection 0.169 μg/mL is attained and relative standard deviation values for five replicated measurements of 0.3, 0.7, and 1.0 μg/mL captopril were between 0.53% and 2.03%. No interference is detected from prevalent additives found in pharmaceutical preparations. The proposed method is profitably put on to the determination of captopril in the tablet formulations with mean recoveries 98.91–101.27% and the results were statistically confronted with those of a reference method by applying Student’s t-and F-test.

scholarly journals Spectrophotometric determination of Phenylephrine hydrochloride and Salbutamol sulphate drugs in pharmaceutical preparations using diazotized Metoclopramide hydrochloride

2015 ◽  
Vol 12 (1) ◽  
pp. 167-177 ◽  
Author(s):  
Baghdad Science Journal
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Correlation Coefficients ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Salbutamol Sulphate ◽  
Phenylephrine Hydrochloride ◽  
Relative Standard ◽  
Metoclopramide Hydrochloride

A spectrophotometric method has been proposed for the determination of two drugs containing phenol group [phenylephrine hydrochloride (PHP) and salbutamol sulphate (SLB)] in pharmaceutical dosage forms. The method is based on the diazotization reaction of metoclopramide hydrochloride (MCP) and coupling of the diazotized reagent with drugs in alkaline medium to give intense orange colored product (?max at 470 nm for each of PHP and SLB). Variable parameters such as temperature, reaction time and concentration of the reactants have been analyzed and optimized. Under the proposed optimum condition, Beer’s law was obeyed in the concentration range of 1-32 and 1-14 ?g mL-1 for PHP and SLB, respectively. The limit of detection (LOD) and limit of quantification (LOQ) for each of PHP and SLB were 0.60, 0.52 ?g mL-1 and 2.02, 1.72 ?g mL-1, respectively. No interference was observed from common excipients present in pharmaceutical preparations. The good correlation coefficients and low relative standard deviation assert the applicability of this method. The suggested method was further applied for the determinations of drugs in commercial pharmaceutical preparations, which was compared statistically with reference methods by means of t- test and F- test and were found not to differ significantly at 95% confidence level. The procedure was characterized by its simplicity with accuracy and precision.

scholarly journals Spectrofluorometric Determination of Verapamil Hydrochloride in Pharmaceutical Preparations and Human Plasma Using Organized Media: Application to Stability Studies

2006 ◽  
Vol 89 (6) ◽  
pp. 1565-1572 ◽  
Author(s):  
Mohamed Walash ◽  
Fathalla Belal ◽  
Nahed El-Enany ◽  
Amina Abdelsalam
Keyword(s):  
Human Plasma ◽  
Biological Fluids ◽  
Sodium Dodecyl ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Official Method ◽  
Stability Studies ◽  
Verapamil Hydrochloride ◽  
Spiked Human Plasma

Abstract A highly sensitive spectrofluorometric method was developed for the determination of verapamil hydrochloride (VP HCl) in pharmaceutical formulations and biological fluids. The proposed method is based on investigation of the fluorescence spectral behavior of VP HCl in micellar systems, such as sodium dodecyl sulfate (SDS) and β-cyclodextrin (β-CD). In aqueous solutions of borate buffer of pH 9 and 8.5, VP HCl was well incorporated into SDS and β-CD, respectively, with enhancement of its native fluorescence. The fluorescence was measured at 318 nm after excitation at 231 nm. The fluorescence intensity enhancements were 183 and 107% in SDS and in β-CD, respectively. The fluorescence-concentration plots were rectilinear over the range of 0.020.2 and 0.020.25 μg/mL, with lower detection limits of 5.58 × 103 and 3.62 × 103 μg/mL in SDS and β-CD, respectively. The method was successfully applied to the analysis of commercial tablets and the results were in good agreement with those obtained with the official method. The method was further applied to the determination of VP HCl in real and spiked human plasma. The mean % recoveries in the case of spiked human plasma (n 4) was 92.59 3.11 and 88.35 2.55 using SDS and β-CD, respectively, while that in real human plasma (n 3) was 90.17 6.93 and 89.17 6.50 using SDS and β-CD, respectively. The application of the method was extended to the stability studies of VP HCl after exposureto ultraviolet radiation and upon oxidation with hydrogen peroxide.

scholarly journals Simultaneous Determination of Sitagliptin and Metformin in Pharmaceutical Preparations by Capillary Zone Electrophoresis and its Application to Human Plasma Analysis

2012 ◽  
Vol 7 ◽  
pp. ACI.S9940 ◽  
Author(s):  
Mohamed Salim ◽  
Nahed El-Enany ◽  
Fathallah Belal ◽  
Mohamed Walash ◽  
Gabor Patonay
Keyword(s):  
Simultaneous Determination ◽  
Human Plasma ◽  
Capillary Zone Electrophoresis ◽  
Pharmaceutical Preparations ◽  
Effective Length ◽  
Relative Standard ◽  
Significant Difference ◽  
Zone Electrophoresis ◽  
Capillary Zone

A novel, quick, reliable and simple capillary zone electrophoresis CZE method was developed and validated for the simultaneous determination of sitagliptin (SG) and metformin (MF) in pharmaceutical preparations. Separation was carried out in fused silica capillary (50.0 cm total length and 43.0 cm effective length, 49 μm i.d.) by applying a potential of 15 KV (positive polarity) and a running buffer containing 60 mM phosphate buffer at pH 4.0 with UV detection at 203 nm. The samples were injected hydrodynamically for 3 s at 0.5 psi and the temperature of the capillary cartridge was kept at 25 °C. Phenformin was used as internal standard (IS). The method was suitably validated with respect to specificity, linearity, limit of detection and quantitation, accuracy, precision, and robustness. The method showed good linearity in the ranges of 10-100 μg/mL and 50-500 μg/mL with limits of detection of 0.49, 2.11 μm/mL and limits of quantification of 1.48, 6.39 μg/mL for SG and MF, respectively. The proposed method was successfully applied for the analysis of the studied drugs in their synthetic mixtures and co-formulated tablets without interfering peaks due to the excipients present in the pharmaceutical tablets. The method was further extended to the in-vitro determination of the two drugs in spiked human plasma. The estimated amounts of SG/MF were almost identical with the certified values, and their percentage relative standard deviation values (% R.S.D.) were found to be ≤1.50% (n = 3). The results were compared to a reference method reported in the literature and no significant difference was found statistically.

scholarly journals Kinetic Spectrophotometric Determination of Gemifloxacin Mesylate and Moxifloxacin Hydrochloride in Pharmaceutical Preparations Using 4-Chloro-7-nitrobenzo-2-oxa-1,3-diazole

2014 ◽  
Vol 2014 ◽  
pp. 1-12 ◽  
Author(s):  
Mohammed G. Abdel Wahed ◽  
Ragaa El Sheikh ◽  
Ayman A. Gouda ◽  
Sayed Abou Taleb
Keyword(s):  
Limit Of Detection ◽  
Kinetic Method ◽  
Pharmaceutical Preparations ◽  
Fixed Time ◽  
Spectrophotometric Methods ◽  
Relative Standard ◽  
Significant Difference ◽  
Kinetic Spectrophotometric ◽  
Comparison Of The Results

Simple, sensitive, and accurate kinetic spectrophotometric method was proposed for the determination of gemifloxacin mesylate (GMF) and moxifloxacin hydrochloride (MOX) in pure forms and pharmaceutical preparations (tablets). The method is based on coupling the studied drugs with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) in the presence of alkaline borate buffer. Spectrophotometric measurement was achieved by recording the absorbance at 466 and 464 nm for GMF and MOX, respectively, after a fixed time of 20 and 15 min on a water bath adjusted at 70 ± 5°C for both drugs. The different experimental parameters affecting the development and stability of the color were carefully studied and optimized. The absorbance-concentration plots were linear over the ranges 0.5–8.0 and 2.0–12 μg mL−1for GMF and MOX, respectively. The limit of detection of the kinetic method was about 0.12 (2.47 × 10−7 M) and 0.36 (8.22 × 10−7 M) μg mL−1for GMF and MOX, respectively. The proposed methods have been applied and validated successfully with percentage relative standard deviation (RSD% ≤ 0.52) as precision and percentage relative error (RE% ≤ 1.33) as accuracy. The robustness of the proposed method was examined with recovery values that were 97.5–100.5 ± 1.3–1.9%. Statistical comparison of the results with the reference spectrophotometric methods shows excellent agreement and indicates no significant difference in accuracy or precision.

scholarly journals Microextraction by Packed Molecularly Imprinted Polymer Combined Ultra-High-Performance Liquid Chromatography for the Determination of Levofloxacin in Human Plasma

2019 ◽  
Vol 2019 ◽  
pp. 1-9 ◽  
Author(s):  
Jia Meng ◽  
Xu Wang
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
Bacterial Infections ◽  
High Performance ◽  
Limit Of Detection ◽  
Binding Capacity ◽  
Molecularly Imprinted ◽  
Relative Standard

Fluoroquinolones are considered as gold standard for the prevention of bacterial infections. To improve assessment of antibacterial efficacy, a novel method for determination of levofloxacin was developed and validated. Deep eutectic solvents (DESs) as only green solvent were used as a porogen for preparation of water-compatible molecularly imprinted polymers (MIPs) with a pseudotemplate. The DESs-MIPs were characterized in detail, including scanning electron microscope, nitrogen sorption porosimetry, and Fourier transform-infrared spectra. Clearly, the maximum binding capacity of levofloxacin on DESs-MIPs in water and methanol was 0.216 and 0.077 μmol g−1, respectively. The DESs-MIPs as adsorbing materials were applied in microextraction by packed sorbent (MEPS), and the DESs-MIPs-MEPS conditions were optimized. The DESs-MIPs-MEPS coupled with ultra-high-performance liquid chromatography (UHPLC) was used to determine levofloxacin in human plasma. The method was found linear over 0.05–10 μg mL−1 with coefficient of correlation equal to 0.9988. The limit of detection and limit of quantification were 0.012 and 0.04 μg mL−1, respectively. At three spiked levels, the precision of proposed method was between 95.3% and 99.7% with intraday and interday relative standard deviations ≤8.9%. Finally, the developed method was used to examine levofloxacin from human plasma of 20 hospitalized patients after transrectal ultrasound-guided prostate biopsy, and the average concentration (±SD) of levofloxacin was 2.35 ± 0.99 μg mL−1 in plasma.

Vortex-Assisted Dispersive Liquid–Liquid Microextraction Coupled with Deproteinization for Determination of Nateglinide in Human Plasma Using HPLC/UV

2020 ◽  
Author(s):  
Mohamed A Hammad ◽  
Amira H Kamal ◽  
Reham E Kannouma ◽  
Fotouh R Mansour
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Limit Of Detection ◽  
Signal To Noise Ratio ◽  
Cost Effective ◽  
Salt Addition ◽  
Relative Standard ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

Abstract A validated method for preconcentration and determination of nateglinide in plasma was developed using vortex-assisted dispersive liquid–liquid microextraction. Different variables that affect extraction efficiency were studied and optimized, including type and volume of extractant, type and volume of disperser, pH of diluent, salt addition effect, centrifugation and vortex time. Nateglinide was extracted using 30 μL of 1-octanol as an extractant and 200 μL of methanol as a disperser. The enrichment factor reached 330 under the optimum conditions. High-performance liquid chromatography/ultraviolet was used for detection using phosphate buffer (pH 2.5, 10 mM): acetonitrile (45:55, v/v) as a mobile phase at a flow rate of 1 mL/min. The method was linear over the range of 50–20,000 ng/mL with a limit of detection of 15 ng/mL (signal-to-noise ratio = 3). Intra- and inter-day precision had %relative standard deviation &lt;6% (n = 3) and the %recoveries were found to be between 102.5 and 105.9%. The proposed method is simple, sensitive, eco-friendly, cost-effective and powerful for microextraction of nateglinide from human plasma samples.

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