scholarly journals Simultaneous Liquid Chromatographic Determination of Ezetimibe and Simvastatin in Pharmaceutical Products

2007 ◽  
Vol 90 (6) ◽  
pp. 1566-1572 ◽  
Author(s):  
Paulo Renato Oliveira ◽  
Thiago Barth ◽  
Vitor Todeschini ◽  
Sérgio luiz Dalmora

Abstract A reversed-phase liquid chromatographic (LC) method was developed and validated for the simultaneous determination of ezetimibe and simvastatin in pharmaceutical dosage forms. The LC method was carried out on a Synergi fusion C18 column (150 mm 4.6 mm id) maintained at 45C. The mobile phase consisted of phosphate buffer 0.03 M, pH 4.5acetonitrile (35 + 65, v/v) run at a flow rate of 0.6 mL/min, and detection was made using a photodiode array detector at 234 nm. The chromatographic separation was obtained within 15.0 min, and calibration graphs were linear in the concentration range of 0.5200 g/mL. Validation parameters such as specificity, linearity, precision, accuracy, and robustness were evaluated, giving results within the acceptable range for both compounds. Moreover, the proposed method was successfully applied for the routine quality control analysis of pharmaceutical products.

2006 ◽  
Vol 89 (4) ◽  
pp. 937-941 ◽  
Author(s):  
Alpana Srivastava ◽  
Richa Pandey ◽  
Ram K Verma ◽  
Madan M Gupta

Abstract A simple liquid chromatographic method was developed for the determination of sennosides B and A in leaves of Cassia angustifolia. These compounds were extracted from leaves with a mixture of methanolwater (70 + 30, v/v) after defatting with hexane. Analyte separation and quantitation were achieved by gradient reversed-phase liquid chromatography and UV absorbance at 270 nm using a photodiode array detector. The method involves the use of an RP-18 Lichrocart reversed-phase column (5 μm, 125 × 4.0 mm id) and a binary gradient mobile-phase profile. The various other aspects of analysis, namely, peak purity, similarity, recovery, repeatability, and robustness, were validated. Average recoveries of 98.5 and 98.6%, with a coefficient of variation of 0.8 and 0.3%, were obtained by spiking sample solution with 3 different concentration solutions of standards (60, 100, and 200 μg/mL). Detection limits were 10 μg/mL for sennoside B and 35 μg/ML for sennoside A, present in the sample solution. The quantitation limits were 28 and 100 μg/mL. The analytical method was applied to a large number of senna leaf samples. The new method provides a reliable tool for rapid screening of C. angustifolia samples in large numbers, which is needed in breeding/genetic engineering and genetic mapping experiments.


2000 ◽  
Vol 83 (1) ◽  
pp. 237-240 ◽  
Author(s):  
Eshwar Jagerdeo ◽  
Erin Passetti ◽  
Sumer M Dugar

Abstract This paper describes a reversed-phase liquid chromatographic method for the determination of vanillin, associated natural aromatic compounds and/or synthetic precursors, ethyl vanillin, and coumarin, a commonly encountered adulterant in nonbeverage and beverage alcohol products using a ternary gradient mobile phase. The compounds were separated on a Nova-Pak C18 column by using water, methanol, and tetrahydrofuran as the mobile phase. Measurements were made by using a photodiode array detector at 275 nm. The choice of the mobile phase and the column provides baseline resolution of vanillin and the associated aromatic compounds commonly found in vanilla-flavoring material. Because this method provides low-level detection/quantitation, it is suitable for the characterization of vanilla flavoring materials that are currently added to vanilla flavored beverage alcohol products.


1994 ◽  
Vol 77 (6) ◽  
pp. 1689-1694 ◽  
Author(s):  
Linda L Ng

Abstract This study, presented as a technical communication, describes a reversed-phase liquid chromatographic method for select commercial formulations, namely, inhalation solution, nasal solution, capsule and inhalation aerosol. Miscellaneous validation parameters are also discussed.


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.


2017 ◽  
Vol 1 (1) ◽  
pp. 38-43
Author(s):  
Maximiliano Da Silva Sangoi ◽  
Anna Karolina Mouzer da Silva Machado ◽  
Lorena Coimbra Florindo ◽  
Brenda Rocha Gonçalves ◽  
Vítor Todeschini

A reversed-phase liquid chromatography (LC) method is validated for the determination of pinaverium bromide (PB) in pharmaceutical dosage forms. The LC method is carried out on a reversed-phase monolithic C18 column (100 x 4.6 mm i.d.), maintained at 45 ºC. The mobile phase consisted of acetonitrile and a solution of triethylamine 0.3% pH 5.0 (50:50; v/v), run at a flow rate of 2.0 mL/min, with photodiode array detector set at 213 nm. The chromatographic separation is obtained with PB retention time of 3.4 min, and it is linear in the range of 5-100 μg/mL (r2 = 0.9991). The limits of detection and quantitation are 1.41 and 4.70 μg/mL, respectively. The specificity and stability-indicating capability of the method are proven through degradation studies, which also showed that there is no interference of the formulation excipients, showing that peak is free from any coeluting peak. The method showed adequate precision, with a relative standard deviation values lower than 1.38%. Excellent values of accuracy were also obtained, with a mean value of 100.68%. Experimental design is used during validation to calculate and prove method robustness. The proposed LC method is applied for the analysis of the PB pharmaceutical dosage forms, contributing to improve the quality control and to assure the therapeutic efficacy.


1997 ◽  
Vol 80 (3) ◽  
pp. 481-485 ◽  
Author(s):  
Nora M Angelini ◽  
Oscar D Rampin ◽  
Héctor Mugica

Abstract A liquid chromatographic (LC) method was developed and statistically validated for simultaneous determination of nitrofurazone, nitrofurantoin, furazolidone, and furaltadone residues in bovine muscle tissues. These antimicrobial residues in samples stabilized at pH 6.0 were extracted with acetonitrile and purified by liquid-liquid partition between dichloromethane-ethyl acetate and hexane saturated with acetonitrile. The acetonitrileethyl acetate extract was concentrated, and drug residues were dissolved in LC mobile phase, filtered, and determined by LC. A Cis reversed-phase (ODS Hypersil) column at 35°C, a mobile phase of 0.01 M sodium acetate buffer (pH 4.5)-acetonitrile (70 + 30), and a UV/visible diode array detector at 365 nm were used. The retention times and UV spectra of peaks in spiked samples were compared with those of known nitrofurans. Limits of detection (LD) and quantitation (LQ) were 1 and 2 μg/kg, respectively. Average recoveries were 76% (range, 60-110%). Relative standard deviations ranged from 6 to 18% at 5 fortification levels from 1.5 to 20 μg/kg. (Fortification levels for furaltadone were 3 to 40 μg/kg). The method was used to analyze 350 samples per year from 1993 to 1995.


1996 ◽  
Vol 79 (4) ◽  
pp. 829-832
Author(s):  
Euphemia Papadopoulou-Mourkidou ◽  
John Patsias ◽  
George Papadopoulos ◽  
Costas Galanis

Abstract A normal-phase liquid chromatographic (LC) system is presented for determination of fentin acetate in fentin and fentin-maneb wettable powder formulations. Fentin acetate is extracted from both formulations with glacial acetic acid-hexane (20 + 80), and the extract is analyzed after appropriate dilution. An isocratic LC system equipped with a photodiode array detector and a silica gel column, which is eluted with glacial acetic acid-hexane (5 + 95), are used. Quantitation at 258.5 nm is based on an external standard calibration curve. Relative standard deviations were 0.2 and 2.3% for the mean levels (w/w) of fentin acetate determined in fentin and fentin-maneb formulations, respectively.


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