scholarly journals FACILE AND SENSITIVE HPLC-UV METHOD FOR DETERMINATION OF NINTEDANIB IN RAT PLASMA

Author(s):  
Kohei Togami ◽  
Kenta Fukuda ◽  
Kotaro Yamaguchi ◽  
Sumio Chono ◽  
Hitoshi Tada

Objective: In this study, a facile and sensitive high-performance liquid chromatographic method for determination of nintedanib in rat plasma was developed and validated.Methods: After plasma protein was precipitated by addition of acetonitrile, the supernatant underwent centrifugation. An aliquot was then injected into a high-performance liquid chromatographic system with a Mightysil RP-18 GP II ODS column (250 × 3.0 mm, length by inner diameter, 5-μm particle size) maintained at 50 °C. A mobile phase mixture of 20 mmol phosphate buffer (pH 3.0) and acetonitrile (7:3, v/v) was used at a flow rate of 0.6 mL/min, with UV detection at a wavelength of 390 nm for isocratic separation and detection of nintedanib, its main metabolite (BIBF1202), and p-nitrophenol as an internal standard.Results: The quantitative range of nintedanib concentration in this method was 12.5–400 ng/ml, and the calibration curves were linear. The intra-and inter-day accuracy values (relative errors) were in the range of −3.65%–4.00% and −3.65%–3.64%, respectively. The intra-and inter-day precision values (relative standard deviations) were<5.9% and 8.36%, respectively. The method was successfully applied to a pharmacokinetic analysis of nintedanib in rats after intravenous administration.Conclusion: In this study, a rapid, sensitive, and simple HPLC-UV method for the quantitation of nintedanib in rat plasma was developed and validated. The method was shown to be accurate and precise and was successfully applied to a pharmacokinetic study.

2009 ◽  
Vol 92 (2) ◽  
pp. 404-409 ◽  
Author(s):  
Abdalla A Elshanawane ◽  
Samia M Mostafa ◽  
Mohamed S Elgawish

Abstract A high-performance liquid chromatographic method was developed for the simultaneous determination of 2 ternary mixtures containing amiloride hydrochloride, atenolol, hydrochlorothiazide, and chlorthalidone used in hypertension therapy. The use of cyanopropyl column results in satisfactory separation of both mixtures. The mobile phase consisted of 10 mM KH2PO4 buffer (pH 4.5) and methanol in a ratio of (75 25 v/v), at a flow rate of 1 mL/min. UV detector was operated at 275 nm. Calibration graphs were linear in the concentration ranges of 210, 20200, 10100, and 550 g/mL for amiloride hydrochloride, atenolol, hydrochlorothiazide, and chlorthalidone, respectively. Intraday and interday precision values (relative standard deviation) were &lt;1.13 for mixture I (amiloride hydrochloride, atenolol, chlorthalidone), and &lt;0.93 for mixture II (amiloride hydrochloride, atenolol, hydrochlorothiazide). The method was successfully applied for the determination of the 2 combinations in laboratory-prepared mixtures and commercial pharmaceutical formulation with high accuracy and precision. Statistical comparison of the results with those of the published methods showed excellent agreement and indicates no significant difference between them.


2009 ◽  
Vol 74 (12) ◽  
pp. 1455-1465 ◽  
Author(s):  
Valéria Guzsvány ◽  
Zsigmond Papp ◽  
Sanja Lazic ◽  
Ferenc Gaál ◽  
Luka Bjelica ◽  
...  

A simple first-order derivative spectrophotometric method was developed for the simultaneous determination of imidacloprid and 6-chloronicotinic acid (6-CNA). By using the zero-crossing approach, imidacloprid was determined at 249 nm and 6-CNA at 236 nm with detection limits of 0.32 and 0.17 ?g mL-1, respectively, and relative standard deviations not exceeding 1.2 % in the case of model systems. The proposed method was applied for the determination of imidacloprid and 6-CNA in commercial formulations. A conventional spectrophotometric method (at 270 nm) was also employed for the determination of the content of imidacloprid in the same commercial formulations. The results of the developed spectrophotometric methods were in good agreement with those obtained by the high-performance liquid chromatographic method.


2013 ◽  
Vol 9 (2) ◽  
pp. 26-29 ◽  
Author(s):  
AK Hemanth Kumar ◽  
V Sudha ◽  
Geetha Ramachandran

A high performance liquid chromatographic method for determination of rifabutin in human plasma was  developed. The method involved deproteinisation of the sample with acetonitrile and analysis of the  supernatant using a reversed-phase C18 column (250mm) and UV detection at a wavelength of 265nm.  The assay was specific for rifabutin and linear from 0.025 to 10.0μg/ml. The relative standard deviation  of intra- and inter-day assays was lower than 10%. The method was able to remove interfering materials  in plasma, yielding an average recovery of rifabutin from plasma of 101%. Due to its simplicity, the assay  can be used for pharmacokinetic studies of rifabutin. SAARC Journal of Tuberculosis, Lung Diseases & HIV/AIDS; 2012; IX(2) 26-29 DOI: http://dx.doi.org/10.3126/saarctb.v9i2.7975


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