Development and Validation of a Sensitive GC-MS Method for the Determination of Alkylating Agent, 4-Chloro-1-butanol, in Active Pharmaceutical Ingredients

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.

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Fast and Accurate Quantitative Determination of Prednisolone and Chlorpheniramine in Active Pharmaceutical Ingredients and Parenteral Dosage Forms

10.26538/tjnpr/v5i11.5 ◽

2021 ◽

Vol 5 (11) ◽

pp. 1922-1926

Keyword(s):

Quantitative Determination ◽

Dosage Forms ◽

Active Pharmaceutical Ingredients ◽

Pharmaceutical Ingredients

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

Asian Journal of Research in Chemistry ◽

10.52711/0974-4150.2021.00070 ◽

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.

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Stability Indicating RP-HPLC Method Development and Validation for the Determination of Solifenacin Succinate in Bulk and its Pharmaceutical Formulation

Research Journal of Pharmacy and Technology ◽

10.52711/0974-360x.2021.00608 ◽

2021 ◽

pp. 3509-3514

Author(s):

A. Tanuja ◽

S. Ganapaty ◽

Varanasi S N Murthy

Keyword(s):

Method Development ◽

Current Method ◽

Hplc Method ◽

Pharmaceutical Ingredients ◽

Solifenacin Succinate ◽

Ich Guidelines ◽

Degradation Studies ◽

Hplc Method Development ◽

Development And Validation

The current work aims to establish a novel and advanced reverse phase isocratic liquid chromatography system followed by validation and to conduct stability analysis in active pharmaceutical ingredients and formulations for the quantification of Solifenacin Succinate. The optimized elution was achieved with column Sunfire C8 (4.6 x 150mm, 5µm), using the mobile phase of Buffer: Methanol: Acetonitrile in the composition ratio of 45:45:10 v/v. The wavelength of detection was selected as 220nm with 1.0ml/ min flow rate and 30μl injection volume. The retention time of Solifenacin Succinate was found 2.94 min respectively. The method developed has been validated for various analytical parameters according to ICH guidelines. The Linearity was attained at 20 to100 μg/ml of concentration range. The established method was proved as reproducible. The Assay was obtained as 100.40%. The degradation studies were carried out at all degradative conditions and the results of degradation studies denote that the current method was specific, reliable, and economical. Hence, the developed method can be applied for the qualitative and quantitative determination of the selected drug and its commercial formulations.

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