scholarly journals Method Development for 4-Hydroxy-2-Methyl-N- (5-Methyl-2-Thiazolyl)-2H-1,2-Benzothiazine-3-Carboxamide-1,1-Dioxide by Reverse Phase HPLC: New Analytical Technique

Author(s):  
Husnul Maab ◽  
Hammad Yousaf ◽  
Syed Saeed ul Hassan ◽  
Umar Farooq

Purpose: In this study, development of a new analytical method for the evaluation of 4-Hydroxy-2-methyl-N-(5-methyl-2-thiazolyl)-2H-1,2-benzothiazine-3-carboxamide-1,1-dioxide (Meloxicam) by reverse phase HPLC was carried out. The basic aim of this research was to develop and validate a simple, precise, accurate and sensitive method for qualitative and quantitative analysis of Meloxicam in pharmaceutical raw material and its dosage forms. The existing reported method (BP) for the analysis of Meloxicam is potentiometric method which is an old, lengthy and tedious method. Methods: In the new method of reverse phase HPLC, C18 column was used while the mobile phase was acetonitrile and methanol (70:30). The flow rate of mobile phase was 0.6 ml/min and retention time was found to be 1.5min. Separately equal volume of standard solution and sample solutions in HPLC vials were injected in auto sampler compartment of HPLC in six replicates. Chromatogram and peak areas of Meloxicam in standard and sample solutions of different concentrations were recorded. Results: This method was later validated in different ways by which the calibration curve proved to be linear with linearity coefficient of 0.999 over the range of 100 to 600ppm. The precision was equivalent to 0.0003%. The LOD and LOQ were 0.0003ug/ml and 0.001ug/ml respectively. The system also showed accuracy over the range of 95 to 99%. Conclusion: Hence, this method proved to be an alternative to the existing reported method of potentiometric titration because the new method showed accuracy, reproducibility and sensitivity.

Drug Research ◽  
2017 ◽  
Vol 68 (05) ◽  
pp. 296-300
Author(s):  
Anupreet Kaur ◽  
Jaspreet Kaur ◽  
Ranju Bansal

AbstractThe present work describes a rapid and green microwave mediated method for the synthesis and a simple and precise isocratic reverse phase HPLC method for the estimation of the biologically significant dihydropyridines. The conventional synthesis of these dihydropyridines has been previously reported from our lab. The analysis of a standard solution (1 mg/ml) was accomplished on a symmetry (4.6 mm I.D x 250 mm) C-18 column using mobile phase acetonitrile:water:triethylamine (TEA) (70:30:0.1 v/v/v) at a flow rate of 0.7 ml/min. Detection was monitored at 354 nm. The retention time for all the compounds was accomplished as less than 10 min. The compounds showed the linear response over the concentration range 10–100 µg/ml. The study is aimed to develop a rapid method for the quantification of these potent molecules. Various parameters like linearity (10–100 µg/ml), USP tailing and plate count were found to be satisfactory. The investigated parameters were studied with the freshly prepared solutions.


2006 ◽  
Vol 3 (1) ◽  
pp. 60-64 ◽  
Author(s):  
P. Venkata Reddy ◽  
B. Sudha Rani ◽  
G. Srinu Babu ◽  
J. V. L. N. Seshagiri Rao

A reverse phase HPLC method is developed for the determination of Raloxifene in pharmaceutical dosage forms. Chromatography was carried out on an inertsil C18 column using a mixture of acetonitrile and phosphate buffer (30:70 v/v) as the mobile phase at a flow rate of 1 mL/min. Detection was carried out at 290 nm .The retention time of the drug was 10.609 min. The method produced linear responses in the concentration range of 0.5-200 µg/mL of Raloxifene. The method was found to be applicable for determination of the drug in tablets.


Author(s):  
Devi Ramesh ◽  
Mohammad Habibuddin

Objective: The objective of the present study is to develop and validate a simple, rapid, sensitive reverse phase HPLC method for the determination of Armodafinil present in bulk and its pharmaceutical formulations.Methods: The chromatographic separation was achieved by using Hypersil ODS C-18 (150 x 4.6 mm, 5µ) in an isocratic mode with mobile phase methanol: phosphate buffer 3.0 (60:40 %v/v) was used. The flow rate was 1 ml/min and effluent was monitored at 225 nm. The method was validated for validation parameters i.e. linearity, accuracy, precision and robustness according to ICH guidelines.Results: The retention time of Armodafinil was 4.2 min and the linearity range of the method was 500-20000ng/ml with regression (r2) coefficient 0.9998. The method was validated for precision, accuracy, robustness and which were found to be within the acceptable limits according to the ICH guidelines. Also, the method was successfully applied for the estimation of Armodafinil in the marketed formulation of Nuvigil and the recovery was found to be>98%.Conclusion: The developed method possess good selectivity, specificity, there is no interference found in the blank at a retention time of ARM and good correlation between the peak area and concentration of the drugs under prescribed conditions. Hence, the method can be applied for routine analysis of Armodafinil. 


2020 ◽  
Vol 2020 ◽  
pp. 1-7
Author(s):  
Murad Abualhasan ◽  
Nihaya Wasif Odeh ◽  
Ghadeer Naser Younis ◽  
Oyoun Fadel Zeidan

Background. Sodium valproate has anticonvulsant activity and is structurally different to conventional antiepileptic drugs. The problem with valproic acid is the lack of a chromophore, which means that gas chromatography is the sole assay methodology. The introduction of benzoyl and phenyl groups to the molecule is a useful derivatisation, which enables the creation of detectable chromophores for HPLC analysis for pharmaceutical dosages as well as biological systems. Methodology. Sodium valproate was derivatised by the addition of a chromophore to its structure by introducing a methyl benzoyl or a phenyl group. Trichlorophenol and 2-hydroxyacetophenone were used to introduce phenyl and benzoyl groups to valproic acid, respectively. The reaction used was estrification reaction using coupling agents. An analytical method was then developed and validated using reverse-phase HPLC. The method was validated for parameters like linearity, range, accuracy precision, and robustness. Results. The developed method was easy and feasible and can be applied to both routine analysis and bioanalysis. The method was very sensitive and could quantify valproic acid at a very low concentration of 0.75 × 10−5 mg/ml. The developed method was found to be linear (R2 = 0.997), accurate, precise, and robust. Conclusion. The proposed chemical derivatisation and the developed analytical method are novel. The developed analytical procedure is the first of its kind; it is easy and feasible and can be used to quantify and detect sodium valproate at very low concentrations compared to other available methods in the literature.


2013 ◽  
Vol 2013 ◽  
pp. 1-5
Author(s):  
Laura D. Simionato ◽  
Leonardo Ferello ◽  
Sebastián Stamer ◽  
Patricia D. Zubata ◽  
Adriana I. Segall

Simple, sensitive, and economical simultaneous volumetric and HPLC methods for the determination of pridinol mesylate in raw material have been developed. The volumetric method is based on the reaction of pridinol with sodium lauryl sulphate in diluted sulphuric acid. Dimethyl yellow was used as indicator to detect the end point of the titration in aqueous/organic layer. The HPLC method for the determination of pridinol mesylate employs a reverse phase C18 column at ambient temperature with a mobile phase consisting of acetonitrile: 0.05 M potassium dihydrogen phosphate, pH adjusted to 5.0 (1 : 2, v/v). The flow rate was 0.8 mL/min. Quantitation was achieved with UV detection at 258 nm based on peak area. Both methods were found to be suitable for the quality control of pridinol mesylate in raw material.


2020 ◽  
Vol 11 (1) ◽  
pp. 775-780 ◽  
Author(s):  
Sri Rama Krishna Surapureddi ◽  
Kunta Ravindhranath ◽  
Saritha Anthireddy

D-Psicose/allulose, a rare sugar, is an essential raw material in the pharmaceutical and food industries. It is scantly found in nature and to meet its demand in industries, D-Psicose is generated enzymatically using D-fructose as a substrate.  In these conversations, it is important to monitor D-Psicose,  in order to control the process, impurities, optimize the reaction time and reduce the process cost The available analytical methods have their limitations in quantifying D-psicose and D-fructose mixtures. Hence there is a need for the development of a routine, sensitive, quick and precise analytical method for D-psicose production on-line monitoring of reaction mixer. In the present work, a simplified reverse phase HPLC technique is developed and validated for the quick reaction monitoring of D-psicose from D-fructose, during enzymatic conversation procedures. The analysis is conducted at different concentrations ranging from 0.05 % to 0.5 % of the standard solutions of the D-psicose and D-fructose, by using water and Acetonitrile (at a ratio of 20:80) as eluent with a flow rate of 1.0 mL/min on isocratic HPLC-RID system with an aminopropyl silane stationary phase [ZORBAX SIL 4.6 x 150 mm, 5 µm particle size column (USP-L8)]. The applicability of this method is illustrated in reaction monitoring, where D-fructose (substrate) is converted to D-psicose (product) in the presence of the enzyme:  D-Tagotose 3- epimerase. Separation of D-psicose and D-fructose is achieved within 8 minutes with a resolution ≥ 4 which is the key advantage for reaction monitoring and linearity is established with regression of ≥ 0.99.  Additionally, the current method uses a simple mobile phase, without any buffers. It can be used routinely for reaction monitoring.


2013 ◽  
Vol 25 (13) ◽  
pp. 7481-7484
Author(s):  
Syed Saeed-Ul-Hassan ◽  
Ahsan-Ul-Haq Ather ◽  
Muhammad Tayyab Ansari ◽  
Imran Tariq ◽  
Sabiha Karim

1998 ◽  
Vol 31 (14) ◽  
pp. 2513-2535 ◽  
Author(s):  
J. J. Berzas-Nevado ◽  
C. Guiberteau-Cabanillas ◽  
A. M. Contento-Salcedo

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