scholarly journals Experimental and computational evaluation of kolliphor RH 40 as a new fluorescence enhancer in development of a micellar-based spectrofluorimetric method for determination of lapatinib in tablets and urine

PLoS ONE ◽  
2020 ◽  
Vol 15 (12) ◽  
pp. e0239918
Author(s):  
Hany W. Darwish ◽  
Ahmed H. Bakheit ◽  
Nasser S. Al-shakliah ◽  
A. F. M. Motiur Rahman ◽  
Ibrahim A. Darwish
Keyword(s):  
Kinase Inhibitor ◽  
Ph Value ◽  
Limit Of Detection ◽  
Accurate Determination ◽  
Content Uniformity ◽  
Pharmaceutical Tablets ◽  
Computational Evaluation ◽  
Green Approach ◽  
Spectrofluorimetric Method

This study describes, for the first time, the experimental and computational investigations for evaluation of kolliphor RH 40 as a fluorescence enhancer surfactant in development of a spectrofluorimetric method for determination of lapatinib (LAP), a tyrosine kinase-inhibitor drug approved for targeted therapy of breast cancer. The investigations involved the ability of kolliphor RH 40 to form micelles with LAP and its enhancing effect on the weak native fluorescence of LAP at 420 nm after its excitation at 292 nm. Different variables were experimentally investigated: types of organized media, diluting solvent, buffer type and its pH value. The optimum values of the most influencing variables on the interaction of kolliphor RH 40 with LAP were refined by the computational response surface methodology (RSM). Under the optimized conditions, it was found that kolliphor RH 40 forms micelles with LAP, and its fluorescence enhancing ability was higher than other surfactants tested by ~ 10-folds. This micellar-enhanced effect of kolliphor RH 40 was employed in the development of a new sensitive spectrofluorimetric method for the accurate determination of LAP. The method was validated according to the guidelines of the International Conference on Harmonization (ICH) for validation of analytical procedures. The relative fluorescence intensity (RFI) was in excellent linear relationship (correlation coefficient was 0.998) with the LAP concentrations in the range of 50–1000 ng/mL. The method limit of detection (LOD) was 27.31 ng/mL and its accuracy was ≥ 99.82%. The method was successfully applied to the determination of LAP in its pharmaceutical tablets, tablets dissolution testing and content uniformity. The method application was extended to the determination of LAP in urine samples with an accuracy of 99.82 ± 3.45%. The method is considered as an eco-friendly green approach and more efficient alternative method to the existing analytical methodologies for determination of LAP.

scholarly journals Spectrofluorimetric method for atenolol determination based on gold nanoparticles

2018 ◽  
Vol 68 (2) ◽  
pp. 243-250 ◽  
Author(s):  
Esam Bakir ◽  
Mohamed Gouda ◽  
Ahmed Alnajjar ◽  
Waleed E. Boraie
Keyword(s):  
Gold Nanoparticles ◽  
Linear Correlation ◽  
Ph Value ◽  
Limit Of Detection ◽  
Coefficient Of Determination ◽  
Quenching Effect ◽  
Ich Guidelines ◽  
Spectrofluorimetric Method ◽  
Limit Of Quantitation

Abstract A simple and sensitive spectrofluorimetric method for determination of atenolol (ATE) using gold nanoparticles (AuNPs) was developed. The method is based on the quenching effect of atenolol on photoluminescence of AuNPs at λem = 705 nm. Variables affecting luminescence of gold nanoparticles such as the solvent, pH value and surfactant were studied and optimized. The method was preliminarily validated according to ICH guidelines. A linear correlation was recorded within the range of 1.0–10 mg mL−1 ATE with the coefficient of determination R2 of 0.999. The limit of detection and limit of quantitation for atenolol were found to be 0.87 and 2.64 mg mL−1, resp. Good recoveries in the range of 98.7–100.0 % were obtained for spiked samples. The proposed method was applied successfully to assaying atenolol in pharmaceuticals formulations.

scholarly journals New Spectrofluorimetric Method with Enhanced Sensitivity for Determination of Paroxetine in Dosage Forms and Plasma

2008 ◽  
Vol 3 ◽  
pp. ACI.S1053 ◽  
Author(s):  
Ibrahim A. Darwish ◽  
Sawsan M. Amer ◽  
Heba H. Abdine ◽  
Lama I. Al-Rayes
Keyword(s):  
High Sensitivity ◽  
Dosage Forms ◽  
Official Method ◽  
Factors Affecting ◽  
Pharmaceutical Tablets ◽  
Enhanced Sensitivity ◽  
Spectrofluorimetric Method ◽  
Relative Standard ◽  
Optimized Conditions

New simple spectrofluorimetric method with enhanced sensitivity has been developed and validated for the determination of the antidepressant paroxetine (PXT) in its dosage forms and plasma. The method was based on nucleophilic substitution reaction of PXT with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole in an alkaline medium (pH 8) to form a highly fluorescent derivative that was measured at 545 nm after excitation at 490 nm. The factors affecting the reaction was carefully studied and optimized. The kinetics of the reaction was investigated, and the reaction mechanism was presented. Under the optimized conditions, linear relationship with good correlation coefficient (0.9993) was found between the fluorescence intensity and PXT concentration in the range of 80-800 ng ml-1. The limits of detection and quantitation for the method were 25 and 77 ng ml-1, respectively. The precision of the method was satisfactory; the values of relative standard deviations did not exceed 3%. The proposed method was successfully applied to the determination of PXT in its pharmaceutical tablets with good accuracy; the recovery values were 100.2 ± 1.61%. The results obtained by the proposed method were comparable with those obtained by the official method. The proposed method is superior to the previously reported spectrofluorimetric method for determination of PXT in terms of its higher sensitivity and wider linear range. The high sensitivity of the method allowed its successful application to the analysis of PXT in spiked human plasma. The proposed method is practical and valuable for its routine application in quality control and clinical laboratories for analysis of PXT.

scholarly journals Development and validation of a new spectrofluorimetric method for the determination of some beta-blockers through fluorescence quenching of eosin Y. Application to content uniformity test

2016 ◽  
Vol 14 (1) ◽  
pp. 258-266 ◽  
Author(s):  
Sayed M Derayea ◽  
Mahmoud A Omar ◽  
Mohamed Aboel-Kasem Abdel-Lateef ◽  
Ahmed I. Hassan
Keyword(s):  
Fluorescence Quenching ◽  
Beta Blockers ◽  
Dosage Forms ◽  
Ion Pair ◽  
Content Uniformity ◽  
Eosin Y ◽  
Pharmaceutical Dosage Forms ◽  
Quenching Effect ◽  
Spectrofluorimetric Method

AbstractA simple, rapid, sensitive and economic spectrofluorimetric method has been developed and validated for determination of some β-adrenergic blocking agents namely; betaxolol hydrochloride (BTX), carvedilol (CAR), labetalol hydrochloride (LBT), nebivolol hydrochloride (NEB) and propranolol hydrochloride (PRO). The method is based on the quenching effect of the cited drugs on the fluorescence intensity of eosin Y at pH 3.4 (acetate buffer). The fluorescence quenching is due to the formation of an ion-pair complex and was measured without extraction at 545 nm (λex. 301.5 nm). The factors affecting the formation of the ion-pair complex were carefully studied and optimized. Under the optimal conditions, the linear ranges for the relationship between the fluorescence quenching value and the concentration of the investigated drugs were 100-2500, 150-2500 and 50-2250 ng mL-1 for (BTX, CAR), (LBT, NEB) and (PRO) respectively. The method was validated according to ICH guidelines and was applied for determination of the cited drugs in pharmaceutical dosage forms with excellent recoveries. In addition, content uniformity testing of some commercial dosage forms was checked by the proposed method.

scholarly journals Determination of Atenolol and Trimetazidine in Pharmaceutical Tablets and Human Urine Using a High Performance Liquid Chromatography-Photo Diode Array Detection Method

2019 ◽  
Vol 2019 ◽  
pp. 1-8 ◽  
Author(s):  
Walaa El-Alfy ◽  
Omnia A. Ismaiel ◽  
Magda Y. El-Mammli ◽  
Abdalla Shalaby
Keyword(s):  
Human Urine ◽  
Limit Of Detection ◽  
Pure Form ◽  
Urine Samples ◽  
Dihydrogen Phosphate ◽  
Simple Liquid ◽  
Pharmaceutical Tablets ◽  
Limit Of Quantitation ◽  
Precision And Accuracy

A simple RP-HPLC-PDA method for determination of atenolol (ATN) and trimetazidine (TMZ) in human urine and tablets has been developed. Analytes were separated on a Caltrex BI column (125× 4.0 mm, 5 μm) with 25mM potassium dihydrogen phosphate pH 3.3, methanol, and acetonitrile mobile phases. The PDA detector was operated at 210 nm for TMZ and 225 nm for ATN and the flow rate was 1.0 mL/ min. Linearity was obtained over a concentration range of (1.0-100 μg/mL) for both analytes in standard solutions and the method was successfully applied for determination of target analytes in their pharmaceutical tablets. Excellent linearity was also obtained over concentration ranges of (0.25-25 μg/mL) and (0.5-25 μg/mL) in human urine for TMZ and ATN, respectively. A simple liquid-liquid extraction was applied for urine sample clean-up and a gradient method was used for chromatographic separation. The lower limit of quantitation (LOQ) was 0.99 and 0.60 μg/mL for ATN and TMZ, respectively. The limit of detection (LOD) was 0.30 and 0.18 μg/mL for ATN and TMZ, respectively. Inter- and intraday precision and accuracy for ATN were within ±1.89% in pure form and within ±2.85% in urine samples. Inter- and intraday precision and accuracy for TMZ were within ± 3.99% in pure form and within ± 3.19% in urine samples.

scholarly journals Determination of Methadone and Tramadol in Vitreous Humor Specimens Using Dispersive LiquidLiquidMicroextractionandUltraHighPerformance Liquid Chromatography

2021 ◽  
Vol 11 (1) ◽  
pp. 31530.1-31530.9
Author(s):  
Maryam Akhgari ◽  
Keyword(s):  
Liquid Chromatography ◽  
Ph Value ◽  
Limit Of Detection ◽  
Vitreous Humor ◽  
Point Of View ◽  
Limit Of Quantification ◽  
Ultrahigh Performance Liquid Chromatography ◽  
Abused Drugs ◽  
Dispersive Liquid Liquid Microextraction

Background: Drug abuse is spreading rapidly all over the world. Methadone and tramadol are among not only the most abused opioids but also important from the forensic point of view. Therefore, we need to devise a simple and sensitive method for the sample preparation and identification of abused drugs in postmortem specimens. Methods: A simple and rapid Dispersive Liquid-Liquid Microextraction (DLLME) technique coupled with Ultrahigh Performance Liquid Chromatography (UHPLC) was developed for the extraction and analysis of methadone and tramadol from postmortem vitreous humor samples. Different parameters affecting the extraction recovery, such as the type and volume of extraction and dispersion solvents, pH value, sensitivity, and specificity, were optimized and studied. Results: Under optimized conditions, the recovery ranges were 82.3%-89.6% and 85.4%-87.1% for methadone and tramadol, respectively. The linear range was 25-100 ng/mL for both methadone and tramadol with a correlation coefficient (R2) of more than 0.98. Limit of Detection (LoD) and Limit of Quantification (LoQ) were 3 and 8 ng/mL for methadone and 6 and 16 ng/mL for tramadol. The accuracy level of the methods for methadone and tramadol detection were 99.4%-100% and 99.7%-99.9%, respectively. The method was specific enough for the qualitative and quantitative determination of methadone and tramadol. Conclusion: The obtained results showed that DLLME combined with UHPLC is a fast and straightforward method for determining methadone and tramadol in postmortem vitreous humor specimens.

scholarly journals Determination of fumonisins B1 and B2 in beer

2011 ◽  
Vol 23 (No. 1) ◽  
pp. 20-26 ◽  
Author(s):  
Ľ. Daško ◽  
D. Rauová ◽  
E. Belajová ◽  
M. Kováč
Keyword(s):  
Fluorescence Detection ◽  
Phosphate Buffer ◽  
Analytical Procedure ◽  
Ph Value ◽  
Limit Of Detection ◽  
Gradient Elution ◽  
Cleaning Procedure ◽  
Peak Splitting

The aim of this study was to investigate the contamination of beer of Slovak origin with fumonisins. A suitable analytical procedure was suggested &ndash; the limit of detection at the level close to 1 &micro;g/l was achieved for both fumonisins B<sub>1</sub> and B<sub>2</sub>. The recovery was determined at 93% for fumonisin B<sub>1 </sub>and at 78% for fumonisin B<sub>2</sub>. Fluorescence detection was used after derivatisation with a mixture of o-phthaldialdehyde and 2-mercaptoethanol. Phosphate buffer usually applied resulted in a poor separation of derivatised fumonisins. Peak splitting was observed depending on the pH of the eluent. The pH value of 2.6 was found suitable for the peak splitting elimination. A convenient gradient elution metod was suggested avoiding the possible interference in fumonisin contents determination. For the preparation of samples, immunoaffinity cleaning procedure was applied. Beer samples from all domestic producers were analysed. The content of fumonisins determined was under the limit of detection in all cases. All the beers tested were produced from the barley grown in 2003. &nbsp;

scholarly journals Highly Sensitive Micellar Enhanced Spectrofluorimetric Method for Determination of Mirtazapine in Tablets and Human Urine: Application to In Vitro Drug Release and Content Uniformity Test

2016 ◽  
Vol 2016 ◽  
pp. 1-8 ◽  
Author(s):  
Hany W. Darwish ◽  
Ahmed H. Bakheit ◽  
Raed M. Alharbi
Keyword(s):  
Drug Release ◽  
Human Urine ◽  
Dosage Form ◽  
Content Uniformity ◽  
In Vitro Drug Release ◽  
Spectrofluorimetric Method ◽  
Highly Sensitive ◽  
Spiked Human Urine

A highly sensitive and simple micelle enhanced spectrofluorimetric method was developed for assaying mirtazapine (MRZ) in REMERON® tablets and spiked human urine directly without the need of derivatizing agent. The basis of the current procedure is the examination of the relative fluorescence intensity (RFI) of MRZ in sodium lauryl sulphate (SLS) micellar medium. The RFI of MRZ in water was enhanced markedly on addition of SLS. The RFI was measured at 403 nm after excitation at 320 nm. The fluorescence-concentration relationship was linear over the range 1–500 ng/mL, with lower detection limit of 0.399 ng/mL. The proposed method was successfully applied to the determination of MRZ in dosage form and spiked human urine. Recovery percentages of MRZ utilizing the current method were99.05±1.83,98.37±1.96, and100.41±2.61% for pure powder, pharmaceutical dosage form, and spiked human urine, respectively. The application of the proposed method was extended to test content uniformity and the in vitro drug release of REMERON tablets, according to USP guidelines.

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