scholarly journals SEPARATION AND ANALYSIS OF AMLODIPINE/BENAZEPRIL COMBINATION IN CAPSULES BY A NOVEL ION PAIR LIQUID CHROMATOGRAPHY

Author(s):  
Saleh Trefi ◽  
Yaser Bitar

Objective: The objective of this study was to develop and validate a novel ion-pair liquid chromatography method, in order to separate and assay of amlodipine/benazepril combination in capsules. This method was a fast, practical and additional choice in quality control laboratories.Methods: The chromatographic conditions comprised of a classical C18-type stationary phase (250 × 4.6 mm, 5μ), with a mobile phase consisting of: 45% of 10-3 M of cetrimide and 55% acetonitrile. The flow rate was 1 ml/min; the detection wavelength was at 242 nm, under ambient temperature.Results: The method was validated for linearity with correlation coefficients very close to one, the accuracy with mean recovery values between 95.0-105.0%, precision with relative standard deviations of the calculated concentrations less than 5.0% and specificity in the presence of degradation products and excipients.Conclusion: The results presented in this paper showed that the developed method was fast and applicable, for the separation and determination of amlodipine/benazepril combination in capsules.

Author(s):  
Hanan Shasho ◽  
Amir Alhaj Sakur ◽  
Saleh Trefi

Objective: The objective of this study was to develop and validate a single HPLC method, in order to separate and assay four antihistamine drugs diphenhydramine, chlorpheniramine, cyproheptadine and fexofenadine in pharmaceutical forms. This method was a practical additional choice in quality control laboratories.Methods: The chromatographic conditions comprised of a classical C18-type stationary phase (150 × 4.6 mm, 5μ), with a mobile phase consisting of, 2.5g of sodium octane sulfonic acid in a mixture of 500 ml of deionized water and 500 ml of acetonitrile, and apparent pH of 2.0 was adjusted with phosphoric acid. The flow rate was 1 ml/min; the detection wavelengths were at 220 nm, 230 nm, 265 nm and 254 nm for diphenhydramine, chlorpheniramine, cyproheptadine and fexofenadine respectively. The temperature was ambient temperature.Results: The method was validated for linearity with correlation coefficients very close to one, the accuracy with mean recovery values between 95.0-105.0%, precision with relative standard deviations of the calculated concentrations less than 5.0% and specificity in the presence of degradation products. Then it was used successfully to separate a mixture of them and to assay these drugs in pharmaceutical forms purchased from Syria.Conclusion: The results presented in this paper showed that the developed method was simple and applicable, for the separation and determination of the four drugs in their pharmaceutical forms.


2006 ◽  
Vol 89 (6) ◽  
pp. 1552-1556
Author(s):  
ArmaĞan Önal ◽  
Olcay SaĞiri ◽  
S Müge Çetin ◽  
Sidika Toker

Abstract Reboxetine is used as a selective noradrenaline reuptake inhibitor for the treatment of major depressive disorders. It is effective in the treatment of severe depression and safer to use than traditional tricyclic antidepressants. In this study, a novel, simple, and rapid stability-indicating high-performance liquid chromatography (HPLC) method for reboxetine methansulfonate was successfully developed and validated for the assay of tablets. The method was used to quantify reboxetine in tablets; it employed a C18 column (150 4.6 mm id) with an isocratic mobile phase consisting of methanolphosphate buffer (pH 7, 0.02 M; 55 + 45, v/v) at a flow rate of 1.0 μmL/min. Reboxetine was detected by an ultraviolet detector at 277 nm. The retention time of reboxetine was about 4.5 min. The developed HPLC method was validated with respect to linearity, precision, sensitivity, accuracy, and selectivity. The method was linear over the concentration range 150 g/mL (r 0.9999). The limits of detection and the quantitation of reboxetine were 0.1 and 0.3 μg/mL, respectively. The relative standard deviation values for intraday and interday precision were 0.781.01 and 1.081.37%, respectively. Selectivity was validated by subjecting a stock solution of reboxetine to neutral, acid, and alkali hydrolysis, as well as oxidation, dry heat treatment, and photodegradation. The peaks of the degradation products did not interfere with the peak of reboxetine. The results indicated that the proposed method could be used in a stability assay. The proposed method was successfully applied to the determination of reboxetine in tablets. Excipients present in the tablets did not interfere with the analysis.


Author(s):  
Murlidhar V Zope ◽  
Rahul M Patel ◽  
Ashwinikumari Patel ◽  
Samir G Patel

Objective: The objective was to develop and validate the stability indicating reverse-phase high-performance liquid chromatography method for the quantification of potential degradation products of regadenoson (REGA) from its injectable dosage form.Methods: YMC-PAK ODS AQ, 150 mm × 4.6 mm, 3 μm composed with hydrophobic high carbon loading and a relatively hydrophilic surface chemically bonded to porous silica particles column was used with the temperature maintained at 40°C. Mobile phase A composed of 0.1% triethylamine buffer having pH 4.5 while mobile phase B is 100 % acetonitrile was used for gradient elution with 1.5 ml/min as a flow rate. The wavelength used for quantification was 245 nm and 20 μl as an injection volume. The suitability of the method has been checked and validated according to the International Council for Harmonization (ICH) guidelines for different parameters, namely, specificity, linearity, accuracy, precision, limit of quantification (LOQ), Limit of detection (LOQ), and robustness studies.Results: The resolution between REGA and its two-degradation product is >8.0 for all pairs of components. The high correlation coefficient (r2>0.990) values are for drug and all potential degradation products from LOQ to 150% of specification limits for impurities calculated based on the maximum daily dose of REGA. LOQ for the drug as well as each degradation product is <0.02% w/w. The % relative standard deviation (RSD) for precision and intermediate precision is in the range of 0.17–0.89, and % RSD for precision at LOQ is 0.86–2.35. The % RSD for robustness study is maximum 2.59.Conclusion: The developed method can quantify the specified and unknown degradation products from 0.1% in the injectable dosage form which indicates that method is sensitive. Method fulfills the ICH criteria for its different validation parameters and demonstrates that the developed analytical method is highly specific, precise, and robust and would have a great value when applied in quality control and stability studies for REGA injection.


Chemija ◽  
2018 ◽  
Vol 29 (2) ◽  
Author(s):  
Audrius Markevičius ◽  
Audrius Zolumskis ◽  
Audrius Sadaunykas ◽  
Birutė Knašienė ◽  
Adrian Vicent Claramunt ◽  
...  

A fast, precise and accurate high performance liquid chromatography method has been developed for the determination of dyes (Solvent Red 19 and Solvent Blue 35) and a marker (Solvent Yellow 124) in diesel. Separation was carried out on a 250 × 4.60 mm Agilent Zorbax Rx-SIL column (5 µm particle size). Detection was done in a visible wavelength range. The best performance of fuel dye separation and the shortest retention times were achieved when using hexane, toluene and ethyl acetate as a mobile phase. During this research the eluent composition and the elution gradient were optimized consequently that helped to perform the analysis within 15 min. The developed method was applied for the analysis of real samples of dyed diesel fuel. Preparation of the samples for the analysis simply consisted of filtering through a 0.45 µm filter previous to direct injection of the sample into the HPLC system for analysis.


2015 ◽  
Vol 30 (1) ◽  
pp. 35-41 ◽  
Author(s):  
Babak Basiri ◽  
James Michael Sutton ◽  
Bradley S. Hanberry ◽  
Jason A. Zastre ◽  
Michael G. Bartlett

2013 ◽  
Vol 781-784 ◽  
pp. 1708-1711 ◽  
Author(s):  
Yi Qing Yang ◽  
Qian Wang ◽  
Qiao Wang ◽  
Shi Jie Yan

HPLC (High Performance Liquid Chromatography) method for chloramphenicol residues in freshwater fish was developed. The samples were extracted with ethyl acetate. The LC was performed on a C18 column, mobile phase consisted of methanol-water (45:55 v/v) and eluted at 0.2mL/min at 20°C, inject volume was 20μl. The linear rang for chloramphenicol residual is within 0.5-20μg/mL, the limit of detection is 0.01ng/g. The average recovery is 80.06%-92.71%, and the RSD is 1.46%-5.61%. This method is employed to analyze freshwater fishes, such as catfish, chub and carp.


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