scholarly journals New benzimidazole derivatives with potential cytotoxic activity--study of their stability by RP-HPLC.

2012 ◽  
Vol 59 (2) ◽  
Author(s):  
Katarzyna Błaszczak-Świątkiewicz ◽  
Marek Mirowski ◽  
Katarzyna Kaplińska ◽  
Rafał Kruszyński ◽  
Agata Trzęsowska-Kruszyńska ◽  
...  

Obtained benzimidazole derivatives, our next synthesized heterocyclic compounds, belong to a new group of chemical bondings with potential anticancer properties (Błaszczak-Świątkiewicz & Mikiciuk-Olasik, 2006, J Liguid Chrom Rel Tech 29: 2367-2385; Błaszczak-Świątkiewicz & Mikiciuk-Olasik, 2008, Wiad Chem 62: 11-12, in Polish; Błaszczak-Świątkiewicz & Mikiciuk-Olasik, 2011, J Liguid Chrom Rel Tech 34: 1901-1912). We used HPLC analysis to determine stability of these compounds in 0.2% DMSO (dimethyl sulfoxide). Optimisation of the chromatographic system and validation of the established analytical method were performed. Reversed phases (RP-18) and a 1:1 mixture of acetate buffer (pH 4.5) and acetonitrile as a mobile phase were used for all the analysed compounds at a flow rate 1.0 mL/min. The eluted compounds were monitored using a UV detector, the wavelength was specific for compounds 6 and 9 and compounds 7 and 10. The retention time was specific for all four compounds. The used method was found to have linearity in the concentration range of (0.1 mg/mL-0.1 μg/mL) with a correlation coefficient not less than r(2)=0.9995. Statistical validation of the method proved it to be a simple, highly precise and accurate way to determine the stability of benzimidazole derivatives in 0.2% DMSO. The recoveries of all four compounds examined were in the range 99.24-100.00%. The developed HPLC analysis revealed that the compounds studied remain homogeneous in 0.2% DMSO for up to 96 h and that the analysed N-oxide benzimidazole derivatives do not disintegrate into their analogues - benzimidazole derivatives. Compounds 8, 6 and 9 exhibit the best cytotoxic properties under normoxic conditions when tested against cells of human malignant melanoma WM 115.


Author(s):  
Vaishali Mistry ◽  
Rohan Mishra

Objective: This study describes the stability-indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for simultaneous estimation of betahistine dihydrochloride and domperidone in pharmaceutical dosage forms.Methods: The proposed RP-HPLC method was developed using Shimadzu Prominence-i LC-2030 HPLC system equipped with UV detector and chromatographic operation was carried on Shim-pack C18 (250 mm×4.6 mm, 5 μ) column at a flow rate of 1 ml/min and the run time was 10 min. The mobile phase consisted of methanol and water in the ratio of 80:20% v/v and eluents were scanned using a UV detector at 244 nm.Results: The retention time of betahistine dihydrochloride and domperidone was found to be 2.3 and 3.6 min, respectively. A linearity response was observed in the concentration range of 9.6 μg/ml–22.4 μg/ml for betahistine dihydrochloride and 6–14 μg/ml for domperidone, respectively. Limit of detection and limit of quantification for betahistine dihydrochloride were 0.52 μg/ml and 1.58 μg/ml and for domperidone are 0.64 μg/ml and 1.94 μg/ml, respectively.Conclusion: The stability-indicating method was developed by subjecting drugs to stress conditions such as acid and base hydrolysis, oxidation, photo and thermal degradation, and degraded products formed were resolved successfully from samples.



Author(s):  
Vaishali Mistry ◽  
Akshay Yelwe ◽  
Amey Deshpande

Objective: The present study describes the stability indicating reversed-phase high-performance liquid chromatography (RP-HPLC) method for simultaneous estimation of 5-fluorouracil and tegafur in pharmaceutical dosage forms.Method: 5-fluorouracil and tegafur the propose RP-HPLC method were developed by using Shimadzu Prominence-i LC-2030 HPLC system equipped with UV detector and chromatographic separation was carried on shim-pack gist c18 (250 × 4.6 mm, 5 μ) column at a flow rate of 1 ml/min and the run time was 10 min. The mobile phase consisted of methanol and water in the ratio of 50:50% v/v and elements were scanned using a UV detector at 271 nm.Result: The retention time of 5-fluorouracil and tegafur was found to be 2.74 and 3.66 min, respectively. A linearity response was observed in the concentration range of 13.4 μg/ml–31.3 μg/ml for 5-fluorouracil and 6 μg/ml–14 μg/ml for tegafur, respectively. Limit of detection and limit of quantification of 5-fluorouracil were 10.97 μg/ml and 33.26 μg/ml and for tegafur are 4.89 μg/ml and 14.83 μg/ml, respectively.Conclusion: The stability indicating that the method was developed by subjecting drugs to stress conditions such as acid and base hydrolysis, oxidation, photo and thermal degradation, and degraded products formed were resolved successfully from samples.



Author(s):  
Nutan Rao ◽  
Kajal D Gawde

Objective: The present study describes the stability indicating reversed-phase high-performance liquid chromatography (RP-HPLC) method for simultaneous estimation of salbutamol sulfate (SAL), etofylline (ETO), and bromhexine hydrochloride (BROM) in pharmaceutical dosage forms.Methods: The proposed RP-HPLC method was developed using Shimadzu prominence-i LC-2030 HPLC system equipped with ultraviolet (UV) detector and chromatographic separation was achieved isocratically using Shim-pack C18 (250 mm×4.6mm, 5 μ) column at a flow rate of 1 ml/min and the run time was 13 min. The mobile phase consisted of acetonitrile: 0.1M potassium dihydrogen phosphate buffer (35:65) with pH adjusted to 3.0 and eluents were scanned using UV detector at 225 nm.Result: The retention time of SAL, ETO, and BROM was found to be 2.319 min, 2.698 min, and 10.329 min, respectively. The calibration curve was linear over the concentration ranges of 1.6–3.2 μg/ml, 160–320 μg/ml, and 6.4–12.8 μg/ml for SAL, ETO, and BROM, respectively.Conclusion: The stability indicating method was developed by subjecting the drugs to stress conditions such as acid and base hydrolysis, oxidation, humidity, and photo- and thermal degradation and the degraded products formed were resolved successfully from the samples. Therefore, the proposed method can be used as a more convenient and efficient option for the simultaneous estimation of all the three drugs in bulk and combined



Author(s):  
Javed S Shaik ◽  
Nutan N Rao

Objective: The present study describes the stability indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for simultaneous estimation of amiloride hydrochloride and furosemide in pharmaceutical dosage forms.Methods: The proposed RP-HPLC method was developed using Shimadzu LC-2030 HPLC system equipped with UV detector, and chromatographic separation was carried on Shim-pack C18 (250 mm×4.6 mm, 5 μ) column at a flow rate of 1 ml/min and the runtime was 4min. The mobile phase consisted of water and acetonitrile in the ratio of 35:65, and elements were scanned using a UV detector at 281 nm.Results: The retention time of amiloride hydrochloride and furosemide was found to be 1.92 min and 3.14min, respectively. Linearity was found to be 12–28 ppm for amiloride hydrochloride and 96–224 ppm for furosemide, respectively. Limit of detection and limit of quantification for amiloride hydrochloride were 0.381 ppm and 1.156 ppm and for furosemide were 2.00 ppm and 6.068 ppm, respectively.Conclusion: The stability indicating method was developed by subjecting the drugs to stress conditions such as acid and base hydrolysis, oxidation, humidity, photolytic, and thermal degradation, and the degraded products formed were resolved successfully from the samples.



2010 ◽  
Vol 22 (3) ◽  
pp. 473-480 ◽  
Author(s):  
N. W. Ali ◽  
S. Abouzid ◽  
A. Nasib ◽  
S. Khan ◽  
J. Qureshi ◽  
...  


2013 ◽  
Vol 12 (2) ◽  
pp. 219-225
Author(s):  
Carmen Roba ◽  
Cristina Rosu ◽  
Iulia Neamtiu ◽  
Eugen Gurzau


2020 ◽  
Vol 27 (35) ◽  
pp. 5970-6014 ◽  
Author(s):  
Md. Jawaid Akhtar ◽  
Mohammad Shahar Yar ◽  
Vinod Kumar Sharma ◽  
Ahsan Ahmed Khan ◽  
Zulphikar Ali ◽  
...  

This review presents the detailed account of factors leading to cancer and design strategy for the synthesis of benzimidazole derivatives as anticancer agents. The recent survey for cancer treatment in Cancer facts and figures 2017 American Chemical Society has shown progressive development in fighting cancer. Researchers all over the world in both developed and developing countries are in a continuous effort to tackle this serious concern. Benzimidazole and its derivatives showed a broad range of biological activities due to their resemblance with naturally occurring nitrogenous base i.e. purine. The review discussed benzimidazole derivatives showing anticancer properties through a different mechanism viz. intercalation, alkylating agents, topoisomerases, DHFR enzymes, and tubulin inhibitors. Benzimidazole derivatives act through a different mechanism and the substituents reported from the earlier and recent research articles are prerequisites for the synthesis of targeted based benzimidazole derivatives as anticancer agents. The review focuses on an easy comparison of the substituent essential for potency and selectivity through SAR presented in figures. This will further provide a better outlook or fulfills the challenges faced in the development of novel benzimidazole derivatives as anticancer.



2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Amol S. Jagdale ◽  
Nilesh S. Pendbhaje ◽  
Rupali V. Nirmal ◽  
Poonam M. Bachhav ◽  
Dayandeo B. Sumbre

Abstract Background A new, sensitive, suitable, clear, accurate, and robust reversed-phase high-performance liquid chromatography (RP-HPLC) method for the determination of brexpiprazole in bulk drug and tablet formulation was developed and validated in this research. Surface methodology was used to optimize the data, with a three-level Box-Behnken design. Methanol concentration in the mobile phase, flow rate, and pH were chosen as the three variables. The separation was performed using an HPLC method with a UV detector and Openlab EZchrom program, as well as a Water spherisorb C18 column (100 mm × 4.6; 5m). Acetonitrile was pumped at a flow rate of 1.0 mL/min with a 10 mM phosphate buffer balanced to a pH of 2.50.05 by diluted OPA (65:35% v/v) and detected at 216 nm. Result The developed RP-HPLC method yielded a suitable retention time for brexpiprazole of 4.22 min, which was optimized using the Design Expert-12 software. The linearity of the established method was verified with a correlation coefficient (r2) of 0.999 over the concentration range of 5.05–75.75 g/mL. For API and formulation, the percent assay was 99.46% and 100.91%, respectively. The percentage RSD for the method’s precision was found to be less than 2.0%. The percentage recoveries were discovered to be between 99.38 and 101.07%. 0.64 μg/mL and 1.95 μg/mL were found to be the LOD and LOQ, respectively. Conclusion The developed and validated RP-HPLC system takes less time and can be used in the industry for routine quality control/analysis of bulk drug and marketed brexpiprazole products. Graphical abstract



Author(s):  
Mehmet Emin Şeker ◽  
Ali Çelik ◽  
Kenan Dost ◽  
Ayşegül Erdoğan

Abstract Investigation of phenolic content from different pine bark species grown in Turkey was performed using a reversed-phase high pressure liquid chromatography with ultraviolet (RP-HPLC-UV) method. All phenolic constituents were separated in <26 min on reversed-phase C18 column with gradient mobile phase that consists of orthophosphoric acid, methanol and acetonitrile. Detections were made on an UV detector at 280 nm and at a flow rate of 1 mL/min. Samples were prepared according to Masqueller’s conventional sample preparation method with slight modifications. To avoid the reduction in extraction efficiency the sample preparation step was carried out under argon atmosphere. The linearity of the method was between 0.9994 and 0.9999. The detection limits for the five phenolic constituents ranged from 0122 to 0.324 mg/L. Catechin and taxifolin were found in all pine barks at a concentration of 0.065 ± 0.002–1.454 ± 0.004 and 0.015 ± 0.001–23.164 ± 0.322 mg/g, respectively. Epicatechin was determined in four pine barks between 0.027 ± 0.001 and 0.076 ± 0.002 mg/g, ferulic acid in two pine barks between 0.010 ± 0.001 and 0.022 ± 0.001 mg/g and epicatechin gallate in only one of the pine barks at 0.025 ± 0.001 mg/g. Finally, the total amount of phenolic compounds and antioxidant capacities of the pine barks were found to be very high.



INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (09) ◽  
pp. 40-47
Author(s):  
B. N Nalluri ◽  
◽  
B. Mrudula ◽  
K Chitralatha ◽  
S. A Sultana ◽  
...  

The present paper describes a sensitive and simple RP-HPLC-PDA method for the simultaneous estimation of Naproxen Sodium (NPX) and Diphenhydramine Hydrochloride (DPH) in the presence of their degradants. The drugs were subjected to stress conditions (forced degradation) to show the stability-indicating power of the method. The separation was achieved on Inertsil ODS C18 column (250×4.6mm, 5μ). The optimized liquid chromatographic conditions were found to be a mobile phase of 15mM ammonium acetate buffer: acetonitrile (60:40V/V) combination at a flow rate of 1.0 mL/min in isocratic mode with an injection volume of 10µL. The proposed method provided retention times of 4.6 and 10.8min, with linear responses over a range of 60-140μg/mL and 10-30μg/mL and regression coefficient (R2) of 0.999 and 0.996 respectively for NPX and DPH. No interference from other components of pharmaceutical dosage form and degradants was observed. The method was validated as per ICH guidelines and was successfully applied for the simultaneous estimation of both the drugs in bulk and tablet preparations.



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