scholarly journals Development and Validation of a Column High-Performance Liquid Chromatographic Method for Determination of Sibutramine in Capsules

2009 ◽  
Vol 92 (1) ◽  
pp. 148-151 ◽  
Author(s):  
Isabel Cristina Fração Diefenbach ◽  
Milene Friedrich ◽  
Marcos Roberto Dos Santos ◽  
Celso Figueiredo Bittencourt

Abstract The development and validation of a reversed-phase liquid chromatographic (LC) method for the determination of sibutramine hydrochloride monohydrate in capsules is described. An isocratic LC analysis was performed on a reversed-phase RP-18 column (250 4.6 mm id, 5 m particle size). The mobile phase consisted of methanolwatertriethylamine (80 + 20 + 0.5, v/v/v), with pH adjusted to 5.65 with 85 phosphoric acid, and was pumped at a constant flow rate of 1.0 mL/min. Measurements were made at a wavelength of 223 nm. The calibration curve was linear over the range of 1540 g/mL [correlation coefficient (r2) = 0.9998]. The relative standard deviation (RSD) value for intraday precision was 0.84. The RSD value for interday precision was 0.90. Recoveries ranged from 99.64 to 100.66. No interferences from the excipients were observed. Because of its simplicity and accuracy, the method is suitable for routine quality control analysis of sibutramine in capsules.

2005 ◽  
Vol 88 (2) ◽  
pp. 424-427 ◽  
Author(s):  
Lisiane Bajerski ◽  
Simone G Cardoso ◽  
Isabel Fraçao Diefenbach ◽  
Marcelo Donadel Malesuik ◽  
Silvia Helena Miollo Borgmann

Abstract The development and validation of a reversed-phase liquid chromatographic (LC) method for the determination of cetirizine dihydrochloride in oral formulations are described. An isocratic LC analysis was performed on a reversed-phase C18 column (250 × 4.6 mm id, 5 μm particle size). The mobile phase was 1% orthophosphoric acid solution, pH 3.0–acetonitrile (60 + 40, v/v), pumped at a constant flow rate of 1.0 mL/min. Measurements were made at a wavelength of 232 nm. The calibration curves were linear over the range of 10–30 μg/mL (r2 = 0.9999). The relative standard deviation (RSD) values for intraday precision were 0.94 and 1.43% for tablets and compounded capsules, respectively. The RSD values for interday precision were 0.13 and 0.82% for tablets and compounded capsules, respectively. Recoveries ranged from 97.7 to 101.8% for tablets and from 98.4 to 102% for compounded capsules. No interferences from the excipients were observed. Because of its simplicity and accuracy, the method is suitable for routine quality-control analysis for cetirizine in tablets and compounded capsules.


INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (07) ◽  
pp. 43-49
Author(s):  
B.P. Manjula ◽  
V. G Joshi ◽  
Siddamsetty Ramachandra Setty ◽  
M Geetha ◽  

Tea tree oil, an active ingredient of skin, hair and nail care cosmeceuticals, has claims for topical antimicrobial, analgesic and anti-inflammatory activity. Its complex composition is governed by ISO 4730:2017. Terpinene-4-ol is the principal constituent of the oil (35% - 48%) followed by γ-terpinene (14% -28%), α-terpinene (6%-12%) and 1,8-cineole (≤15%). A reversed-phase, isocratic high performance liquid chromatographic method has been developed and validated for routine determination of tea tree oil based on1,8-cineole content in bulk and commercially available cosmeceuticals using C18 column, methanol-water (70:30 v/v) as mobile phase and flow rate of 1mL/min. UV detection was done at 200 nm. Linearity of the method was established for 20-100μL/mL (R2 = 0.9992) with LOD, LOQ values of 0.5594 μL/mL and 5.5941μL/mL respectively. The % RSD values for robustness and precision were <1% and recovery ranged between 99.09-102.96%. The method was successfully applied for determination of 1,8-cineole content in cosmeceuticals.


2008 ◽  
Vol 91 (4) ◽  
pp. 739-743 ◽  
Author(s):  
Andréia de Haro Moreno ◽  
Hérida Regina Nunes Salgado

Abstract A rapid, accurate, and sensitive high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of ceftazidime in pharmaceuticals. The method validation parameters yielded good results and included range, linearity, precision, accuracy, specificity, and recovery. The excipients in the commercial powder for injection did not interfere with the assay. Reversed-phase chromatography was used for the HPLC separation on a Waters C18 (WAT 054275; Milford, MA) column with methanolwater (70 + 30, v/v) as the mobile phase pumped isocratically at a flow rate of 1.0 mL/min. The effluent was monitored at 245 nm. The calibration graph for ceftazidime was linear from 50.0 to 300.0 g/mL. The values for interday and intraday precision (relative standard deviation) were &lt;1. The results obtained by the HPLC method were calculated statistically by analysis of variance. We concluded that the HPLC method is satisfactory for the determination of ceftazidime in the raw material and pharmaceuticals.


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


2017 ◽  
Vol 1 (2) ◽  
pp. 1-8
Author(s):  
Milena Cristina Ribeiro Souza Magalhães ◽  
Alisson Samuel Portes Caldeira ◽  
Hanna De Sousa Rocha Almeida ◽  
Sílvia Ligório Fialho ◽  
Armando Da Silva Cunha Junior

A reversed-phase high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of encapsulation efficiency of zidovudine in nanoparticules. The method was carried out in isocratic mode using 0.040M sodium acetate: methanol: acetonitrile: glacial acetic acid (880:100:20:2) as mobile phase, a C8 column at 25ºC and UV detection at 240 nm. The method was linear (r2 ˃ 0.99) over the range of 25.0-150.0 μg/mL, precise (RSD ˂ 5%), accurate (recovery = 100.5%), robust and selective. The validated HPLC-UV method can be successfully applied to determine the rate of zidovudine in nanoparticules.


2009 ◽  
Vol 6 (2) ◽  
pp. 489-494 ◽  
Author(s):  
B. Prasanna Kumar Reddy ◽  
Y. Ramanjaneya Reddy ◽  
D. Ramachandran

A simple, sensitive and precise high performance liquid chromatographic method for the analysis of pantoprazole sodium and lansoprazole has been developed, validated and used for the determination of compounds in commercial pharmaceutical products. The compounds were well separated an isocratically on a C18column [Inertsil C18, 5μ, 150 mm x 4.6 mm] utilizing a mobile phase consisting of acetonitrile: phosphate buffer (60:40, v/v, pH 7.0) at a flow rate of 1.0 mL/min with UV detection at 230 nm. The retention time of pantoprazole sodium and lansoprazole was found to be 2.017 min and 2.538. The procedure was validated for linearity (Correlation coefficient=0.999). The study showed that reversed-phase liquid chromatography is sensitive and selective for the determination of pantoprazole sodium and lansoprazole using single mobile phase.


Author(s):  
Krishna Patel ◽  
Dipti Patel

A simple, specific and accurate reversed-phase high performance liquid chromatographic method was developed for the simultaneous determination of Capecitabine and Oxaliplatin, using a Hypersil BDS C18, 150x4.6 mm, 5μ column and a mobile phase composed of 10mM dipotassium hydrogen phosphate+0.1% TEA pH 5.0: Acetonitrile (50:50%v/v). The flow rate was 1.0 ml/min, and the detection wavelength was 245 nm. The injection volume was 20 μL. The retention times of Capecitabine and Oxaliplatin found 4.29 min and 5.52 min, respectively. Linearity was established for Capecitabine and Oxaliplatin in the range of 60-210μg/ml and 20-70 μg/ml, respectively. The percentage recoveries of Capecitabine and Oxaliplatin found to be in the range of 99.1-101.5% and 97.9-99.7 %, respectively. The proposed method validated for precision, accuracy, linearity range, and robustness. This method can successfully be employed for simultaneous quantitative analysis of Capecitabine and Oxaliplatin in the capsule.


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