Quantitative determination of residual active pharmaceutical ingredients and intermediates on equipment surfaces by ion mobility spectrometry

2010 ◽  
Vol 51 (1) ◽  
pp. 107-113 ◽  
Author(s):  
C. Qin ◽  
A. Granger ◽  
V. Papov ◽  
J. McCaffrey ◽  
D.L. Norwood
Keyword(s):  
Quantitative Determination ◽  
Ion Mobility Spectrometry ◽  
Ion Mobility ◽  
Active Pharmaceutical Ingredients ◽  
Pharmaceutical Ingredients

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.

scholarly journals Ion Mobility–Mass Spectrometry for Bioanalysis

Separations ◽  
2021 ◽  
Vol 8 (3) ◽  
pp. 33
Author(s):  
Xavier Garcia ◽  
Maria del Mar Sabaté ◽  
Jorge Aubets ◽  
Josep Maria Jansat ◽  
Sonia Sentellas
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Ion Mobility Spectrometry ◽  
Ion Mobility ◽  
Biological Samples ◽  
Ion Mobility Mass Spectrometry ◽  
Exogenous Compounds ◽  
Analytical Separation

This paper aims to cover the main strategies based on ion mobility spectrometry (IMS) for the analysis of biological samples. The determination of endogenous and exogenous compounds in such samples is important for the understanding of the health status of individuals. For this reason, the development of new approaches that can be complementary to the ones already established (mainly based on liquid chromatography coupled to mass spectrometry) is welcomed. In this regard, ion mobility spectrometry has appeared in the analytical scenario as a powerful technique for the separation and characterization of compounds based on their mobility. IMS has been used in several areas taking advantage of its orthogonality with other analytical separation techniques, such as liquid chromatography, gas chromatography, capillary electrophoresis, or supercritical fluid chromatography. Bioanalysis is not one of the areas where IMS has been more extensively applied. However, over the last years, the interest in using this approach for the analysis of biological samples has clearly increased. This paper introduces the reader to the principles controlling the separation in IMS and reviews recent applications using this technique in the field of bioanalysis.

scholarly journals Rapid determination of N-methylpyrrolidine in cefepime by combining direct infusion electrospray ionisation-time-of-flight mass spectrometry with field asymmetric waveform ion mobility spectrometry

2015 ◽  
Vol 7 (1) ◽  
pp. 34-39 ◽  
Author(s):  
Robert W. Smith ◽  
Lisa B. Cox ◽  
Aswandi Yudin ◽  
James C. Reynolds ◽  
Mark Powell ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Ion Mobility Spectrometry ◽  
Ion Mobility ◽  
Rapid Determination ◽  
Time Of Flight ◽  
Asymmetric Waveform ◽  
Direct Infusion ◽  
Electrospray Ionisation ◽  
Flight Mass Spectrometry

FAIMS separation prior to mass spectrometry enables selective transmission of NMP in cefepime without interference from NMP formed by in-source CID.

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.

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