scholarly journals DEVELOPMENT AND VALIDATION OF METHODS FOR QUANTITATIVE DETERMINATION OF ACTIVE PHARMACEUTICAL SUBSTANCES IN NASAL SPRAY

2021 ◽  
Vol 9 (4) ◽  
pp. 266-277
Author(s):  
M. V. Larskiy ◽  
A. E. Pozdnyakova ◽  
Z. D. Khadzhieva ◽  
D. I. Pozdnyakov
Keyword(s):  
Quantitative Determination ◽  
Nasal Spray ◽  
High Performance ◽  
Potassium Dihydrogen Phosphate ◽  
Dihydrogen Phosphate ◽  
Active Pharmaceutical Ingredients ◽  
Potassium Dihydrogen ◽  
Pharmaceutical Ingredients ◽  
Development And Validation

Intranasal administration of H1-histamine receptor blockers may be a promising approach to the treatment of allergic rhinitis. Earlier, an original composition of a nasal spray containing fexofenadine hydrochloride and ammonium glycyrrhizinate and demonstrating a high level of therapeutic efficacy, was developed.The aim of the study was to develop and validate a method of the quantitative determination of active pharmaceutical ingredients fexofenadine hydrochloride and ammonium glycyrrhizinate in a spray for intranasal administration.Materials and methods. During the development and validation of the method of the fexofenadine hydrochloride and ammonium glycyrrhizinate quantitative determination in a nasal spray, the method of high performance liquid chromatography was used: a Dionex Ultimate 3000 UV chromatograph with a Luna C18 column (2) containing octadecylsilicagel with a 5 μm grain size as a sorbent. The analysis and validation procedures were performed in accordance with the requirements of the State Pharmacopoeia of the Russian Federation, the XIVth edition.Results. The study showed that for the simultaneous quantitative determination of fexofenadine hydrochloride and ammonium glycyrrhizinate, the optimal elution regime is a gradient mode with a mobile phase containing 50 mmol/L potassium dihydrogen phosphate solution with methanol (45:55), which ensured the separation of the components in the 20 minutes interval. The validation procedures showed that the developed methodology correspond to all the criteria of validity in terms of the following indicators: correctness, precision, specificity and linearity in the analytical area.Conclusion. The obtained results indicate the possibility of using the method of high-performance liquid chromatography in a gradient elution mode with a mobile phase of the composition of a 50 mmol/L solution of potassium dihydrogen phosphate with methanol (45:55) for the simultaneous quantitative determination of active pharmaceutical ingredients – fexofenadine hydrochloride and ammonium glycyrrhizinate as parts of a promising nasal spray for the allergic rhinitis treatment.

DEVELOPMENT AND VALIDATION OF A RP-UFLC ANALYTICAL METHOD FOR THE DETERMINATION OF OPIPRAMOL IN TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (11) ◽  
pp. 24-28
Author(s):  
S.B Rohith ◽  
◽  
B.M Gurupadayya ◽  
R.S Chandan
Keyword(s):  
Analytical Method ◽  
Potassium Dihydrogen Phosphate ◽  
Dihydrogen Phosphate ◽  
Control Analysis ◽  
Potassium Dihydrogen ◽  
Ich Guidelines ◽  
Fast Liquid Chromatography ◽  
Development And Validation ◽  
Tablet Dosage

A novel ultra-fast liquid chromatography (RP- UFLC) analytical method has been developed to quantify opipramol in tablet formulations. The determination was carried out by means of a Phenomenex Luna C8 Column (250×4.60mm, 5μ); potassium dihydrogen phosphate buffer of pH 2.4 and acetonitrile was used as a mobile phase in the ratio of 60:40 V/V with a flow rate of 1.00 mL/min. The photo diode array (PDA) detector was operated at wavelength of 253nm. The retention time for opipramol was found to be 2.72min. The validation studies were carried out according to ICH guidelines with a specific aim to establish that the new analytical method developed complied with the validation guidelines. The main parameters for validation study are specificity, linearity, accuracy, precision, LOD, LOQ and robustness. This method can be used for quality control analysis of opipramol in pure and marketed formulation.

scholarly journals Development and validation of a reversed-phase HPLC method for determination of assay content of Teriflunomide by the aid of BOMD simulations

2021 ◽  
pp. 281-294 ◽  
Author(s):  
Abolghasem Beheshti ◽  
Zahra Kamalzadeha ◽  
Monireh Haj-Maleka ◽  
Meghdad Payaba ◽  
Mohammad Amin Rezvanfar ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Potassium Dihydrogen Phosphate ◽  
Active Pharmaceutical Ingredient ◽  
Reversed Phase ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Td Dft ◽  
High Level ◽  
Development And Validation

Due to the new hopes for treatment of multiple sclerosis (MS) diseases by Teriflunomide (TFN), in this project, a cheap, robust, and fully validated method has been developed both for determination of assay content in API (active pharmaceutical ingredient), and for related impurities analysis (RIA). To operate the method, a common C18, end-capped (250 × 4.6) mm, 5µm liquid chromatography column, was applied. The mobile phase A was prepared by dissolving 2.74 g (20mM) of PDP (potassium dihydrogen phosphate) and 3.72 g (50mM) of PC (potassium chloride) in water (1000 mL). Then, pH was adjusted to 3.0 by adding OPA (ortho-phosphoric acid) 85%; while, the mobile phase B was acetonitrile (ACN) (100%). In order to confirm the experimental data about the λmax of TFN, we have used the Born-Oppenheimer molecular dynamics (BOMD) simulations, quantum mechanics (QM), and TD-DFT calculations. According to the results, the method showed a high level of suitability, specificity, linearity, accuracy, precision, repeatability, robustness, and reliable detection limit.

Simultaneous Determination of Emtricitabine and Tenofovir disoproxil fumarate in Pharmaceutical Dosage by Reverse Phase High Performance Liquid Chromatography

2021 ◽  
pp. 412-416
Author(s):  
Rajan V. Rele ◽  
Sandip P. Patil
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Tenofovir Disoproxil Fumarate ◽  
High Performance ◽  
Phosphoric Acid Solution ◽  
Active Pharmaceutical Ingredients ◽  
Chromatography Method ◽  
Pharmaceutical Ingredients

A simple, rapid and accurate high performance liquid chromatography method is described for simultaneous determination of emtricitabine and tenofovir disoproxil fumarate from active pharmaceutical ingredients. The separation of drug was achieved on Hypersil BDS C18 (150 x 4.6 mm i.d.) with 5 µ particle size column showed most favorable chromatographic pattern over the other columns. The mobile phase consisted of a mixture of buffer and methanol (85:15 % v/v). The buffer was mixtures of 0.1 % (v/v) ortho-phosphoric acid solution adjusted the pH 3.5 with tri-ethyl amine. The detection was carried out at wavelength 260 nm. The mixture of buffer of pH 3.5 and methanol (85:15% v/v) was used as a diluent. The method was validated for system suitability, linearity, accuracy, precision, robustness, stability of sample solution. The method has been successfully used to analyze emtricitabine and tenofovir disoproxil fumarate from active pharmaceutical ingredients.

DEVELOPMENT OF LIQUID CHROMATOGRAPHIC METHOD FOR SIMULTANEOUS DETERMINATION OF BROMHEXINE HYDROCHLORIDE AND ENROFLOXACIN IN FORMULATIONS

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (02) ◽  
pp. 44-49
Author(s):  
P Choksi ◽  
◽  
F. Shaikh ◽  
D. A. Shah ◽  
K. Agarwal ◽  
...  
Keyword(s):  
Potassium Dihydrogen Phosphate ◽  
Fixed Dose ◽  
Dihydrogen Phosphate ◽  
Potassium Dihydrogen ◽  
Liquid Chromatographic Method ◽  
Dose Combination ◽  
Reproducible Method ◽  
Liquid Chromatographic ◽  
Isocratic Mode

A simple, specific, accurate, precise and reproducible method has been developed and validated for the estimation of bromhexine hydrochloride and enrofloxacin in fixed dose combination using RP-HPLC. The separation was achieved using stationary phase ODS Hypersil C18 column (250 mm× 4.6 mm i.d.) in isocratic mode, with mobile phase containing 0.05 M potassium dihydrogen phosphate buffer (pH 4 by o-phosphoric acid) : methanol: acetonitrile : triethylamine (40:20:40:01), at a flow rate of 1.0mL/min and eluents were monitored at 256 nm. The retention time of enrofloxacin and bromhexine HCl were found to be 3.00 min and 5.1 min respectively. The linearity for bromhexine HCl and enrofloxacin was in the range of 2-15 μg/mL and 20-150 μg/mL, respectively. The method was validated as per ICH guideline. The recoveries of bromhexine HCl and enrofloxacin were found in the range of 99.61-101.65% and 99.52-100.13 %, respectively. The method was successfully applied for the determination of both the drugs in combined dosage form.

Validated HPLC and Ultra-HPLC Methods for Determination of Dronedarone and Amiodarone Application for Counterfeit Drug Analysis

2015 ◽  
Vol 98 (6) ◽  
pp. 1496-1502 ◽  
Author(s):  
Ramzia I El-Bagary ◽  
Ehab F Elkady ◽  
Shereen Mowaka ◽  
Maria Attallah
Keyword(s):  
Flow Rate ◽  
Chromatographic Separation ◽  
Phosphate Buffer ◽  
Potassium Dihydrogen Phosphate ◽  
Pharmaceutical Preparations ◽  
Uv Detection ◽  
Dihydrogen Phosphate ◽  
Isocratic Elution ◽  
Potassium Dihydrogen

Abstract Two simple, accurate, and precise chromatographic methods have been developed and validated for the determination of dronedarone (DRO) HCl and amiodarone (AMI) HCl either alone or in binary mixtures due to the possibility of using AMI as a counterfeit of DRO because of its lower price. First, an RP-HPLC method is described for the simultaneous determination of DRO and AMI. Chromatographic separation was achieved on a BDS Hypersil C18 column (150 × 4.6 mm, 5 μm). Isocratic elution based on potassium dihydrogen phosphate buffer with 0.1% triethylamine pH 6–methanol (10 + 90, v/v) at a flow rate of 2 mL/min with UV detection at 254 nm was performed. The second method is RP ultra-HPLC in which the chromatographic separation was achieved on an AcclaimTM RSLC 120 C18 column (100 × 2.1 mm, 2.2 μm) using isocratic elution with potassium dihydrogen phosphate buffer with 0.1% triethylamine pH 6–methanol (5 + 95, v/v) at a flow rate of 1 mL/min with UV detection at 254 nm. Linearity, accuracy, and precision of the two methods were found to be acceptable over the concentration ranges of 5–80 μg/mL for both DRO and AMI. The results were statistically compared using one-way analysis of variance. The optimized methods were validated and proved to be specific, robust, precise, and accurate for the QC of the drugs in their pharmaceutical preparations.

scholarly journals High-Performance Liquid Chromatographic Determination of Dihydroergocristine in a Pharmaceutical Formulation with Fluorescence Detection

2010 ◽  
Vol 93 (1) ◽  
pp. 97-101
Author(s):  
Michal Douša ◽  
Michaela Dubovská
Keyword(s):  
Fluorescence Detection ◽  
Mobile Phase ◽  
High Performance ◽  
Pharmaceutical Preparation ◽  
Potassium Dihydrogen Phosphate ◽  
Sample Pretreatment ◽  
Chromatographic Determination ◽  
Hplc Determination ◽  
Dihydrogen Phosphate

Abstract A rapid procedure based on a direct extraction and HPLC determination of dihydroergocristine in a pharmaceutical preparation with fluorescence detection has been developed and validated. The optimized chromatographic conditions included a Purospher RP18e column, 5 µm particle size, 250 4.0 mm, and 25 mM potassium dihydrogen phosphate buffer (pH 2.8)acetonitrile (60 + 40, v/v) mobile phase at a flow rate of 1 mL/min. The separation was carried out at 50C, and the injection volume was 5 L. Fluorescence detection was performed at an excitation and emission wavelength of 224 and 344 nm, respectively. The mobile phase parameters such as organic solvent composition, temperature, and pH were studied. The proposed method has the advantages of a very simple sample pretreatment and fast HPLC determination.

scholarly journals Stability-Indicating Method for Determination of Oxyphenonium Bromide and Its Degradation Product by High-Performance Liquid Chromatography

2007 ◽  
Vol 90 (5) ◽  
pp. 1250-1257 ◽  
Author(s):  
Alaa EL-Gindy ◽  
Samy Emara ◽  
Heba Shaaban
Keyword(s):  
Degradation Product ◽  
High Performance ◽  
Potassium Dihydrogen Phosphate ◽  
Order Rate Constant ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Stability Indicating Method ◽  
Oxyphenonium Bromide

Abstract A high-performance liquid chromatographic (HPLC) method was developed for determination of oxyphenonium bromide (OX) and its degradation product. The method was based on the HPLC separation of OX from its degradation product, using a cyanopropyl column at ambient temperature with mobile phase of acetonitrile25 mM potassium dihydrogen phosphate, pH 3.4 (50 + 50, v/v). UV detection at 222 nm was used for quantitation based on peak area. The method was applied to the determination of OX and its degradation product in tablets. The proposed method was also used to investigate the kinetics of the acidic and alkaline degradation of OX at different temperatures, and the apparent pseudo first-order rate constant, half-life, and activation energy were calculated. The pH-rate profile of the degradation of OX in Britton-Robinson buffer solutions within the pH range 212 was studied.

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