scholarly journals New potentiometric sensors for methylphenidate detection based on host–guest interaction

BMC Chemistry ◽  
2019 ◽  
Vol 13 (1) ◽  
Author(s):  
Haitham AlRabiah ◽  
Mohammed Abounassif ◽  
Haya I. Aljohar ◽  
Gamal Abdel-Hafiz Mostafa
Keyword(s):  
Dosage Form ◽  
Fast Response ◽  
High Accuracy ◽  
Hplc Method ◽  
Dioctyl Phthalate ◽  
Potentiometric Sensors ◽  
Routine Laboratory ◽  
Electroactive Materials ◽  
Ph Range

Abstract The study aims to develop simple, sensitive, and selective methods for detecting methylphenidate in its bulk, dosage form and human urine. Sensing materials include β-cyclodextrin (β-CD), γ-cyclodextrin (γ-CD), and 4-tertbutylcalix[8]arene as ionophores or electroactive materials have been used for construction of sensors 1, 2, and 3, respectively; Potassium tetrakis (4-chlorophenyl)borate (KTpClPB) as an ion additive was used and dioctyl phthalate as a plasticizer. The sensors displayed a fast, stable response over a wide concentration range of methylphenidate (8 × 10−6 M to 1 × 10−3 M) with 10−6 M detection limit over the pH range of 4–8. The developed sensors displayed a Near-Nernstian cationic response for methylphenidate at 59.5, 51.37, and 56.5 mV/decade for sensors β-CD, γ-CD, or 4-tertbutylcalix[8]arene respectively. Validation of the proposed sensors is supported by high accuracy, precision, stability, fast response, and long lifetimes, as well as selectivity for methylphenidate in the presence of different species. Sensitive and practical sensors for the determination of methylphenidate in bulk, in pharmaceutical forms and urine were developed and validated for routine laboratory use. The results were comparable to those obtained by HPLC method.

NEW VALIDATED RP-HPLC METHOD FOR THE DETERMINATION OF RIZATRIPTAN BENZOATE IN BULK AND PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2014 ◽  
Vol 51 (12) ◽  
pp. 32-36
Author(s):  
T. Vishalakhi ◽  
◽  
S. K Kumar ◽  
K Sujana ◽  
P Rani
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Hplc Method ◽  
Detector Response ◽  
Mobile Phase Flow Rate ◽  
Pharmaceutical Dosage Form ◽  
Rizatriptan Benzoate ◽  
Rp Hplc ◽  
Bulk Drug

A simple validated RP HPLC method for the estimation of rizatriptan benzoate in pharmaceutical dosage form and bulk was developed for routine analysis. This method was developed by selecting Agilent TC C18 (250 x 4.6 mm, 5 μ) column as stationary phase and acrylonibrile:water (45:55), pH adjusted to 3, as mobile phase. Flow rate of mobile phase was maintained at 4: 1 mL/min at ambient temperature throughout the experiment. Quantification was achieved with ultraviolet (DAD) detection at 220 nm. The retention time obtained for rizatriptan was 2.8 min. The detector response was linear in the concentration range of 2-25μg/mL. This method was validated and shown to be specific, sensitive, precise, linear, accurate, rugged and robust. Hence, this method can be applied for routine quality control of rizatriptan benzoate in dosage forms as well as in bulk drug.

HPLC METHOD DEVELOPMENT FOR ESTIMATION OF RAMELTEON IN TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (06) ◽  
pp. 20-23
Author(s):  
S Sahoo ◽  
◽  
P. K. Panda ◽  
S. K. Mishra
Keyword(s):  
Flow Rate ◽  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Ich Guidelines ◽  
Hplc Method Development ◽  
Tablet Dosage ◽  
Good Agreement

A simple, fast, accurate and precise reverse phase HPLC method is developed and described for the determination of ramelteon in tablet dosage form. Chromatography was carried on an ODS column using a mixture of acetonitrile and phosphate buffer pH 7.0 (35:65 V/V) as the mobile phase at a flow rate of 1.0 mL/min with detection at 286 nm. The retention time of the drug was 7.7 min. The procedure was validated for linearity, precision, accuracy, and robustness. The developed method was validated for linearity from 50 to 150% which shows the method is quite linear with a correlation coefficient of 0.999, for precision which includes system precision, method precision, intraday and by another analyst on another day, and accuracy. The %RSD for system precision was observed to be 1.1, whereas the method precision was observed to be 0.2. The % recovery from ‘accuracy’ studies yielded the recovery of 99.7-101.5% which indicates the capability of the method, and finally for robustness that includes studies w.r.t. change in flow rate, the percentage of organic modifier and pH. As per ICH guidelines, method validation results are in good agreement. The proposed method was simple, sensitive, precise and accurate.

A Development and Validation of RP-HPLC Method for the Determination of Degradation Impurities in Anagrelide Dosage Form

2021 ◽  
Vol 11 (5) ◽  
pp. 708-718
Author(s):  
Ravindra Mallavarapu ◽  
Kommera Pavithra ◽  
Naresh Kumar Katari ◽  
Thirupathi Dongala
Keyword(s):  
Dosage Form ◽  
Hplc Method ◽  
Rp Hplc ◽  
Development And Validation

REVERSE PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR DETERMINATION OF REGORAFENIB IN TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (06) ◽  
pp. 63-68
Author(s):  
R. Raut ◽  
◽  
A. Patil ◽  
V. K Munipalli ◽  
M. Patel ◽  
...  
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Control Analysis ◽  
Reverse Phase ◽  
Ich Guidelines ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple precise and rapid Reverse Phase High Performance Liquid Chromatographic (RP-HPLC) method has been developed for quantitative determination of Regorafenib in tablet dosage form. In this method Hypersil Gold (C18, 150mm× 4.6mm id, 3μ) column with mobile phase consisting of Trifluoroacetic acid (0.2% v/v) and Acetonitrile in the ratio of (50: 50 v/v) at 400C in an isocratic mode was used. The detection was carried out at 260 nm and 20μL injection volume was selected with the flow rate 1mL/min. The linearity range of Regorafenib shows concentration between 5-200 μg/mL. The regression coefficient obtained was 0.999. Retention time of Regorafenib was found to be 6.49 minutes. Acetonitrile and Water in the ratio of (3:1) was used as a diluent. The method was validated as per ICH guidelines and is simple, fast, accurate, precise and can be applied for routine quality control analysis of Regorafenib in tablet dosage form.

Simultaneous determination of Sulphadoxine and Pyrimethamine by taking Tolterodine as an internal standard in Pharmaceutical dosage form by RP-HPLC

2021 ◽  
pp. 145-150
Author(s):  
Sushil D. Patil ◽  
Pravin B. Shelke ◽  
Priti Aher ◽  
Maswood Ahmed Hafizur Rahman
Keyword(s):  
Simultaneous Determination ◽  
Dosage Form ◽  
Internal Standard ◽  
Hplc Method ◽  
Control Analysis ◽  
Pharmaceutical Dosage Form ◽  
Quality Control Analysis ◽  
Rp Hplc ◽  
Sulphadoxine Pyrimethamine

A simple, rapid, economic, sensitive and precise HPLC method has been developed for the simultaneous determination of Sulphadoxine and Pyrimethamine in pharmaceutical dosage form by taking Tolterodine as an internal standard. The method was carried out using Phenomenex C18 (4.6ID × 250mm; 5µm) column and mobile phase comprised of methanol and Phosphate Buffer in proportion of ratio 60:40 v/v. The flow rate was 1.0mL/min and detection was carried out at 276nm. The retention time of Sulphadoxine, Pyrimethamine and Tolterodine were found to be 2.967, 4.058 and 6.908 respectively. Linearity of Sulphadoxine and Pyrimethamine in the range of 2 to 12μg/mL and 4 to 24μg/mL respectively. The % recoveries of Sulphadoxine and Pyrimethamine were found to be in between 99.93% to 99. 96 % respectively. The proposed method is suitable for the routine quality control analysis for simultaneous determination of Sulphadoxine and Pyrimethamine was in bulk and pharmaceutical dosage form.

scholarly journals Validation of a Stability-Indicating RP-HPLC Method for the Determination of Entecavir in Tablet Dosage Form

2010 ◽  
Vol 93 (2) ◽  
pp. 523-530 ◽  
Author(s):  
Sérgio Luiz Dalmora ◽  
Maximiliano da Silva Sangoi ◽  
Daniele Rubert Nogueira ◽  
Lucélia Magalhães da Silva
Keyword(s):  
Dosage Form ◽  
Potassium Phosphate ◽  
Hplc Method ◽  
Forced Degradation ◽  
Photodiode Array Detection ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Tablet Dosage

Abstract An RP-HPLC method was validated for the determination of entecavir in tablet dosage form. The HPLC method was carried out on a Gemini C18 column (150 4.6 mm id) maintained at 30C. The mobile phase consisted of acetonitrilewater (95 + 5, v/v)/potassium phosphate buffer (0.01 M, pH 4; 9 + 91, v/v) pumped at a flow rate of 1.0 mL/min. Photodiode array detection was at 253 nm. The chromatographic separation was obtained with a retention time of 4.18 min, and the method was linear in the range of 0.5200 g/mL (r2 0.9998). The specificity and stability-indicating capability of the method was proven through forced degradation studies, which also showed that there was no interference of the excipients and an increase of the cytotoxicity only by the basic condition. The accuracy was 101.19, with bias lower than 1.81. The LOD and LOQ were 0.39 and 0.5 g/mL, respectively. Method validation demonstrated acceptable results for precision and robustness. The proposed method was applied for the analysis of tablet formulations, to improve QC and assure therapeutic efficacy.

scholarly journals Polymeric Matrix Membrane Sensors for Stability-Indicating Potentiometric Determination of Oxybutynin Hydrochloride and Flavoxate Hydrochloride Urogenital System Drugs

2008 ◽  
Vol 91 (6) ◽  
pp. 1318-1330 ◽  
Author(s):  
Mohamed Heba ◽  
Nesrin Ramadan ◽  
Moustafa El-Laithy
Keyword(s):  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Official Method ◽  
Urogenital System ◽  
Electroactive Materials ◽  
Significant Difference ◽  
Ph Range ◽  
Oxybutynin Hydrochloride ◽  
Flavoxate Hydrochloride

Abstract Four polyvinyl chloride (PVC) matrix membrane electrodes responsive to 2 drugs affecting the urogenital systemoxybutynin hydrochloride (OX) and flavoxate hydrochloride (FX)were developed, described, and characterized. A precipitation-based technique with tungstophosphate (TP) and ammonium reineckate (R) anions as electroactive materials in a PVC matrix with an OX cation was used for electrode 1 and 2 fabrication, respectively. Electrode 3 and 4 fabrication was based on use of the precipitation technique of FX cation with tetrakis (4-chlorophenyl) borate and R anions as electroactive materials. Fast and stable Nernstian responses in the range 1 1021 106 M for the 2 drugs over the pH range 58 revealed the performance characteristics of these electrodes, which were evaluated according to International Union of Pure and Applied Chemistry recommendations. The method was applied to FX and OX in their pharmaceutical formulations and in human plasma samples. The 4 proposed sensors were found to be specific for the drugs in the presence of up to 60 of their degradation products. Validation of the method according to the quality assurance standards showed suitability of the proposed electrodes for use in the quality control assessment of these drugs. The recoveries for determination of the drugs by the 4 proposed selective electrodes were 99.5 0.5, 100.0 0.4, 99.9 0.4, and 100.1 0.4 for sensors 14, respectively. Statistical comparison between the results obtained by this method and the official method of the drugs was done, and no significant difference found.

Development and Validation of Two Robust Stability-Indicating Chromatographic Methods for Determination of Metolazone in Drug Substance and Pharmaceutical Dosage Form in the Presence of Its Degradation Products and Characterization of Main Degradation Products Based on LC-MS

2019 ◽  
Vol 58 (3) ◽  
pp. 251-261
Author(s):  
Hala E Zaazaa ◽  
Rasha Abdel-Ghany ◽  
M Abdelkawy ◽  
Mahmoud Sayed
Keyword(s):  
Dosage Form ◽  
Degradation Products ◽  
Hplc Method ◽  
Drug Substance ◽  
Design Parameters ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Chromatographic Methods ◽  
Hptlc Method

Abstract Two robust and selective stability-indicating chromatographic methods were developed and validated for the determination of metolazone in drug substance and pharmaceutical dosage form in the presence of its degradation products. The HPLC method employed a Kromasil C18 (250 × 4.6,5 μm) column and a mobile phase of acetonitrile: 0.2% orthophosphoric acid (32:68 v/v) at a flow rate 2 mL/min and detection at 238 nm. The separation was performed in HPLC isocratic mode. The robustness of the suggested method was assessed using the Plackett–Burman design, parameters affecting system suitability were established and non-significant intervals for the significant parameters were considered. The HPTLC method employed Nano-SIL-20 UV254 HPTLC plates as adsorbent, ethyl acetate: toluene: acetic acid solution (4:4:0.5, v/v/v), as a developing solvent system and densitometric detection at 238 nm. Metolazone was exposed to different stress conditions, including acid and alkaline hydrolysis and oxidative and photolytic degradation. The main degradation products obtained have been characterized and interpreted based on LC-MS. The linearity of the suggested methods was proved in the concentration range of 20–75 μg/mL for the HPLC method and 100–900 ng/spot for the HPTLC method. The suggested methods were validated according to international conference on harmonization guidelines. These methods were successfully dedicated for the estimation of metolazone in drug substance and pharmaceutical dosage form in the presence of its degradation products. The results of the suggested methods were evaluated and compared statistically with results obtained by an official method without finding any significant difference.

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