scholarly journals HPLC-fluorescence detection for assay of tramadol binary mixtures with ibuprofen or chlorzoxazone in tablets and plasma: Analytical Eco-Scale and GAPI tools for green assessment

2021 ◽  
Author(s):  
Mohamed M.A. Hamdy ◽  
Mona M. Abdel Moneim
Keyword(s):  
Binary Mixtures ◽  
Fluorescence Detection ◽  
Analytical Procedure ◽  
Gradient Elution ◽  
Dosage Forms ◽  
Hplc Method ◽  
Sample Treatment ◽  
Spiked Plasma ◽  
Water Ph ◽  
Higher Sensitivity

AbstractTramadol, a strong pain killer known for its addictive problems is either co-administrated or co-formulated with other analgesics or muscle relaxants. The power of fluorescence detection in HPLC is tested to resolve such mixtures in plasma matrix to reach the required sensitivity with simple sample treatment using just protein precipitation. The aim of this work was to develop an eco-friendly and sensitive HPLC method with fluorimetric detection for analysis of Tramadol in its two binary mixtures with Ibuprofen (mixture 1) and Chlorzoxazone (mixture 2) in two combined dosage forms and spiked plasma. Separation was done using a C18 column with mobile phase of acetonitrile and water (pH 3.5) in gradient elution and 1 mL/min flow rate. Detection was carried out with λ excitation/λ emission of 220 and 307 nm, respectively. The method was applied to detect the two binary mixtures in real plasma samples after invivo application to rats, to assure that the drugs’ metabolites do not affect the sensitivity or selectivity of the assay. Evaluation of greenness of the proposed method was done using semi-quantitative Eco‐Scale and new Green Analytical Procedure Index which showed that this method can be a greener alternative with higher sensitivity for analysis of both mixtures. The method (15 min-assay) was linear over concentrations of 0.1–10 μg/mL and 0.1–33 μg/mL in plasma. In addition, the proposed method was validated per ICH as well as FDA bioanalytical methods’ validation guidelines.

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;

Analytical and bioanalytical HPLC method for simultaneous estimation of 5-fluorouracil and sonidegib

Bioanalysis ◽  
2021 ◽  
Author(s):  
Bharath S Padya ◽  
Aswathi R Hegde ◽  
Sadhana P Mutalik ◽  
Swati Biswas ◽  
Srinivas Mutalik
Keyword(s):  
Analytical Procedure ◽  
Gradient Elution ◽  
Rat Plasma ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Simultaneous Quantification ◽  
Liquid Liquid Extraction ◽  
Rp Hplc ◽  
Dose Oral ◽  
Methods Analytical

Aim: To develop a new sensitive RP-HPLC method for simultaneous estimation of 5-fluorouracil (5-FU) and sonidegib (SDG). Materials & methods: Analytical and bioanalytical methods for simultaneous quantification of 5-FU and SDG in bulk, nanoformulations and in rat plasma were developed and validated using a gradient elution technique. Results: Separation of the analytes was effected on a Luna® C18 LC column using a mobile mixture comprising acetonitrile and acidified water. 5-FU and SDG were extracted from plasma matrix using liquid–liquid extraction. The applicability of the method was verified through single-dose oral pharmacokinetic study in Wistar rats. Conclusion: The developed methods allow a specific, sensitive and steady analytical procedure for the simultaneous estimation of 5-FU and SDG in nanoformulations and biological matrix.

A New HPLC Method with Fluorescence Detection for the Determination of Memantine in Human Plasma

2013 ◽  
Vol 96 (1) ◽  
pp. 52-55 ◽  
Author(s):  
Serife Evrim Kepekci Tekkeli ◽  
Sidika Erturk Toker
Keyword(s):  
Human Plasma ◽  
Fluorescence Detection ◽  
Pharmacokinetic Study ◽  
Mobile Phase ◽  
Orthophosphoric Acid ◽  
Gradient Elution ◽  
Hplc Method ◽  
Fluorometric Detection ◽  
Fluorescent Derivative

Abstract A sensitive and selective HPLC method with fluorometric detection was developed for the determination of memantine in human plasma and applied to a pharmacokinetic study. Memantine was precolumn derivatized with 9-fluorenylmethyl chloroformate, and the fluorescent derivative was separated on an RP C18 column using a mobile phase composed of acetonitrile–10 mM orthophosphoric acid containing 1 mL/L triethylamine with gradient elution. The method was based on the measurement of the derivative using fluorescence detection at 310 nm with excitation at 260 nm. The calibration curve was linear over the range 1.0–50.0 ng/mL. LOD and LOQ were found to be 0.3 and 1.0 ng/mL, respectively. Intraday and interday RSD values were less than 3.39%.

scholarly journals Development and Validation of a Rapid RP HPLC Method for the Determination of Cinitapride Hydrogen Tartarate in Solid Oral Dosage Forms

2011 ◽  
Vol 8 (3) ◽  
pp. 1424-1429
Author(s):  
Syeda Humaira ◽  
Akalanka Dey ◽  
S.Appala Raju ◽  
Syed Sanaullah
Keyword(s):  
Pharmaceutical Formulations ◽  
Gradient Elution ◽  
Dosage Forms ◽  
Hplc Method ◽  
Oral Dosage ◽  
Control Analysis ◽  
Pharmaceutical Dosage Forms ◽  
Solid Dosage ◽  
Oral Dosage Forms ◽  
Development And Validation

In the present study a simple, sensitive rapid and accurate HPLC method with UV detection for the analysis of cinitapride hydrogen tartarate was developed and validated in solid dosage forms. The method utilized gradient elution technique with C18 column (150×4.6 mm I.D, 5 μm particle size) with mobile phase consisting of 0.1% formic acid in water and acetonitrile The detection wavelength was at 268 nm, with flow rate of 0.5 mL/min and injection volume of 10 μL for separation of cinitapride in bulk drugs and pharmaceutical formulations. The gradient elution was developed for better and optimized results. The developed method was validated for precision which includes system precision and method precision, accuracy and linearity studies in the concentration range of 5-100 μg/mL with correlation coefficient of 0.9987. The accuracy (recovery) was between 97.32 and 100.82%. The proposed method is simple, fast, accurate, precise and reproducible, hence can be applied for routine quality control analysis of cinitapride in pure and pharmaceutical dosage forms.

Simultaneous Estimation of Ilaprazole and Domperidone in Pharmaceutical Dosage Form

2016 ◽  
Vol 9 (6) ◽  
pp. 3549-3555
Author(s):  
Gopi Patel ◽  
Kiral M Prajapati ◽  
Bhavesh Prajapati ◽  
Samir K Shah
Keyword(s):  
Dosage Form ◽  
Ammonia Solution ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Control Analysis ◽  
Linear Calibration ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Water Ph ◽  
Alkali Hydrolysis

A simple, accurate and precise stability-indicating RP-HPLC method was developed and subsequently validated for simultaneous determination of ilaprazole and domperidone in bulk and pharmaceutical dosage form. The proposed HPLC method utilizes  C18  (250 mm × 4.6 mm × 5 µm) column with mobile phase comprising of 0.5 % glacial acetic acid in water pH 5.5 adjusted with ammonia solution: methanol in the ratio 45:55 v/v at a flow rate of 1.0 ml/min. Quantitation was achieved with UV detection at 286 nm based on peak area with linear calibration curves at concentration  ranges 80-120µg/ml for ilaprazole and 240-360 µg/ml for domperidone  with correlation coefficient of 0.999.The retention times of ilaprazole and domperidone  were found to be 3.0 min, 5.4 min respectively. The mean recoveries obtained for ilaprazole and domperidone were found to be 99.76 ± 0.6463 % and 100.7 ± 0.2424 % respectively. Stress testing which covered acid, alkali hydrolysis, and peroxide, photolytic, thermal degradation was performed to prove the specificity of the proposed method and degradation was achieved. The proposed method was successfully applied for the stability indicating simultaneous estimation of ilaprazole and domperidone in routine quality control analysis in bulk and pharmaceutical formulation.

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