scholarly journals Determination of Amlodipine in Pharmaceutical Dosage Forms by Liquid Chromatography and Ultraviolet Spectrophotometry

2006 ◽  
Vol 89 (2) ◽  
pp. 359-364 ◽  
Author(s):  
Marcelo Donadel Malesuik ◽  
Simone Gonalves Cardoso ◽  
Lisiane Bajerski ◽  
Fibele Analine Lanzanova
Keyword(s):  
Liquid Chromatography ◽  
Pharmaceutical Preparations ◽  
Forced Degradation ◽  
Uv Spectrophotometry ◽  
Ultraviolet Spectrophotometry ◽  
Pharmaceutical Dosage Forms ◽  
Relative Standard ◽  
Significant Difference ◽  
Interday Precision

Abstract A liquid chromatography (LC) method and an ultraviolet (UV) spectrophotometricmethod were developed and validated for quantitative determination of amlodipine in tablets and compounded capsules. The isocratic LC analyses were performed on an RP18 column using a mobile phase composed of 0.1 (v/v) ortho-phosphoric acid (pH 3.0) acetonitrile (60 40, v/v) at a flow rate of 1.0 mL/min. The UV spectrophotometricmethodwas performed at 238 nm. The analytical methodswere validated according to International Conference on Harmonization Guidelines. The calibration graphswere linear correlation coefficient (r) > 0.999 in the studied concentration range of 1030 g/mL for LC and 1035 g/mL for UV spectrophotometry. The relative standard deviation values for intraday and interday precision studies were less than 2, and the accuracywas greater than 98 for bothmethods. The specificity of the LC method was proved using forced degradation. Statistical analyses showed no significant difference between the results obtained by the 2 methods. The proposed methods are precise and accurate and can be applied directly and easily to the oral pharmaceutical preparations of amlodipine.

scholarly journals Stability indicating HPLC-Fluorescence detection method for the simultaneous determination of linagliptin and empagliflozin in their combined pharmaceutical preparation

2021 ◽  
Vol 12 (2) ◽  
pp. 168-178
Author(s):  
Mohamed Rizk ◽  
Ali Kamal Attia ◽  
Heba Yosry Mohamed ◽  
Mona Elshahed
Keyword(s):  
Fluorescence Detection ◽  
Mobile Phase ◽  
Pharmaceutical Preparation ◽  
Pharmaceutical Preparations ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Significant Difference

A sensitive, accurate, and precise liquid chromatographic method has been developed and validated for the determination of Linagliptin (LNG) and Empagliflozin (EMP) in their combined tablets. Chromatographic separation was carried out on ODS-3 Inertsil® C18 column (150×4.6 mm, 5 µm). The mobile phase A (consisting of 0.30% Triethyl amine buffer (TEA) at pH = 4.5, adjusted using ortho-phosphoric acid); the mobile phase B (consisting of acetonitrile) was pumped through the column whose temperature was maintained at 40 °C, with a flow rate 1.7 mL/min, using gradient elution from 0-3 min A:B (75:25, v:v), then from 3-6 min the ratio changed to be A:B (60:40, v:v). Fluorescence detection (FLD) was performed at 410 nm after excitation at 239 nm. Acceptable linearity, accuracy and precision values of the proposed method were found over the concentration ranges of 0.5-15 µg/mL for LNG and 1.0-30 µg/mL for EMP with correlation coefficients of 0.9997 and 0.9998 in the case of LNG and EMP, respectively. The recoveries and relative standard deviations percentages were found in the following ranges: 98.56-101.85 and 0.53-1.52% for LNG and 98.00-101.95 and 0.31-1.05% for EMP. The detection and quantification limits were 0.15 and 0.45 µg/mL for LNG and 0.22 and 0.67 µg/mL for EMP. The optimized method was validated and proved to be specific, robust, accurate and reliable for the determination of the drugs in pure form or in their combined pharmaceutical preparations. No significant difference was found regarding accuracy and precision upon statistical comparison between the obtained results of the proposed method and those of the reported method. Furthermore, the proposed method is proved to be a stability-indicating assay after exposure of the studied drugs to variable forced degradation parameters, such as acidic, alkaline and oxidative conditions, according to the recommendations of the International Conference on Harmonization guidelines. The simplicity and selectivity of the proposed method allows its use in quality control laboratories.

scholarly journals Spectrophotometric determination of Phenylephrine hydrochloride and Salbutamol sulphate drugs in pharmaceutical preparations using diazotized Metoclopramide hydrochloride

2015 ◽  
Vol 12 (1) ◽  
pp. 167-177 ◽  
Author(s):  
Baghdad Science Journal
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Correlation Coefficients ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Salbutamol Sulphate ◽  
Phenylephrine Hydrochloride ◽  
Relative Standard ◽  
Metoclopramide Hydrochloride

A spectrophotometric method has been proposed for the determination of two drugs containing phenol group [phenylephrine hydrochloride (PHP) and salbutamol sulphate (SLB)] in pharmaceutical dosage forms. The method is based on the diazotization reaction of metoclopramide hydrochloride (MCP) and coupling of the diazotized reagent with drugs in alkaline medium to give intense orange colored product (?max at 470 nm for each of PHP and SLB). Variable parameters such as temperature, reaction time and concentration of the reactants have been analyzed and optimized. Under the proposed optimum condition, Beer’s law was obeyed in the concentration range of 1-32 and 1-14 ?g mL-1 for PHP and SLB, respectively. The limit of detection (LOD) and limit of quantification (LOQ) for each of PHP and SLB were 0.60, 0.52 ?g mL-1 and 2.02, 1.72 ?g mL-1, respectively. No interference was observed from common excipients present in pharmaceutical preparations. The good correlation coefficients and low relative standard deviation assert the applicability of this method. The suggested method was further applied for the determinations of drugs in commercial pharmaceutical preparations, which was compared statistically with reference methods by means of t- test and F- test and were found not to differ significantly at 95% confidence level. The procedure was characterized by its simplicity with accuracy and precision.

scholarly journals Simultaneous Determination of Sitagliptin and Metformin in Pharmaceutical Preparations by Capillary Zone Electrophoresis and its Application to Human Plasma Analysis

2012 ◽  
Vol 7 ◽  
pp. ACI.S9940 ◽  
Author(s):  
Mohamed Salim ◽  
Nahed El-Enany ◽  
Fathallah Belal ◽  
Mohamed Walash ◽  
Gabor Patonay
Keyword(s):  
Simultaneous Determination ◽  
Human Plasma ◽  
Capillary Zone Electrophoresis ◽  
Pharmaceutical Preparations ◽  
Effective Length ◽  
Relative Standard ◽  
Significant Difference ◽  
Zone Electrophoresis ◽  
Capillary Zone

A novel, quick, reliable and simple capillary zone electrophoresis CZE method was developed and validated for the simultaneous determination of sitagliptin (SG) and metformin (MF) in pharmaceutical preparations. Separation was carried out in fused silica capillary (50.0 cm total length and 43.0 cm effective length, 49 μm i.d.) by applying a potential of 15 KV (positive polarity) and a running buffer containing 60 mM phosphate buffer at pH 4.0 with UV detection at 203 nm. The samples were injected hydrodynamically for 3 s at 0.5 psi and the temperature of the capillary cartridge was kept at 25 °C. Phenformin was used as internal standard (IS). The method was suitably validated with respect to specificity, linearity, limit of detection and quantitation, accuracy, precision, and robustness. The method showed good linearity in the ranges of 10-100 μg/mL and 50-500 μg/mL with limits of detection of 0.49, 2.11 μm/mL and limits of quantification of 1.48, 6.39 μg/mL for SG and MF, respectively. The proposed method was successfully applied for the analysis of the studied drugs in their synthetic mixtures and co-formulated tablets without interfering peaks due to the excipients present in the pharmaceutical tablets. The method was further extended to the in-vitro determination of the two drugs in spiked human plasma. The estimated amounts of SG/MF were almost identical with the certified values, and their percentage relative standard deviation values (% R.S.D.) were found to be ≤1.50% (n = 3). The results were compared to a reference method reported in the literature and no significant difference was found statistically.

scholarly journals Development of an Ultraviolet Spectrophotometric Method for the Determination of Ceftiofur Sodium Powder

2009 ◽  
Vol 92 (6) ◽  
pp. 1673-1680 ◽  
Author(s):  
marinês J E Souza ◽  
Natália Canedo ◽  
Paulo S Souza Filho ◽  
Ana M Bergold
Keyword(s):  
Spectrophotometric Method ◽  
Spectrophotometric Analysis ◽  
Uv Spectrophotometry ◽  
Accuracy And Precision ◽  
Significant Difference ◽  
Student’S T ◽  
Ceftiofur Sodium ◽  
Interday Precision ◽  
Student’S T Test

Abstract A UV spectrophotometric method was developed for determination of ceftiofur sodium in the drug substance and sterile powder for injection. The method validation, which yielded good results, included evaluation of the range, linearity, intraand interday precision, accuracy, recovery, specificity, robustness, LOQ, and LOD. The UV spectrophotometric determinations were performed at 292 nm. Good linearity was obtained between 2.5 and 20.0 g/mL. A prospective validation showed that the method is linear (r = 0.9999) and precise, with RSD values of 0.3 for product A and 0.4 for product B. The intraand interday precision values were <2 for all samples analyzed. Comparison of UV spectrophotometry and LC by analysis of variance and Student's t-test showed no significant difference between methodologies. Moreover, the accuracy and precision obtained with the UV method correlated well with the values obtained with the LC method, and this correlation suggests that UV spectrophotometric analysis can be an inexpensive, reliable, and less time-consuming alternative to chromatographic analysis. The results demonstrated the validity of the proposed method as a simple and useful alternative for the determination of ceftiofur in routine QC analyses.

scholarly journals Validation and Uncertainty Estimation of an Ecofriendly and Stability-Indicating HPLC Method for Determination of Diltiazem in Pharmaceutical Preparations

2013 ◽  
Vol 2013 ◽  
pp. 1-10 ◽  
Author(s):  
Fahimeh Sadeghi ◽  
Latifeh Navidpour ◽  
Sima Bayat ◽  
Minoo Afshar
Keyword(s):  
Degradation Products ◽  
Pharmaceutical Preparations ◽  
Hplc Method ◽  
Forced Degradation ◽  
Solution Ph ◽  
Validation Data ◽  
Column Temperature ◽  
Stability Indicating ◽  
Relative Standard

A green, simple, and stability-indicating RP-HPLC method was developed for the determination of diltiazem in topical preparations. The separation was based on a C18analytical column using a mobile phase consisted of ethanol: phosphoric acid solution (pH = 2.5) (35 : 65, v/v). Column temperature was set at 50°C and quantitation was achieved with UV detection at 240 nm. In forced degradation studies, the drug was subjected to oxidation, hydrolysis, photolysis, and heat. The method was validated for specificity, selectivity, linearity, precision, accuracy, and robustness. The applied procedure was found to be linear in diltiazem concentration range of 0.5–50 μg/mL (r2=0.9996). Precision was evaluated by replicate analysis in which % relative standard deviation (RSD) values for areas were found below 2.0. The recoveries obtained (99.25%–101.66%) ensured the accuracy of the developed method. The degradation products as well as the pharmaceutical excipients were well resolved from the pure drug. The expanded uncertainty (5.63%) of the method was also estimated from method validation data. Accordingly, the proposed validated and sustainable procedure was proved to be suitable for routine analyzing and stability studies of diltiazem in pharmaceutical preparations.

scholarly journals Kinetic Spectrophotometric Determination of Gemifloxacin Mesylate and Moxifloxacin Hydrochloride in Pharmaceutical Preparations Using 4-Chloro-7-nitrobenzo-2-oxa-1,3-diazole

2014 ◽  
Vol 2014 ◽  
pp. 1-12 ◽  
Author(s):  
Mohammed G. Abdel Wahed ◽  
Ragaa El Sheikh ◽  
Ayman A. Gouda ◽  
Sayed Abou Taleb
Keyword(s):  
Limit Of Detection ◽  
Kinetic Method ◽  
Pharmaceutical Preparations ◽  
Fixed Time ◽  
Spectrophotometric Methods ◽  
Relative Standard ◽  
Significant Difference ◽  
Kinetic Spectrophotometric ◽  
Comparison Of The Results

Simple, sensitive, and accurate kinetic spectrophotometric method was proposed for the determination of gemifloxacin mesylate (GMF) and moxifloxacin hydrochloride (MOX) in pure forms and pharmaceutical preparations (tablets). The method is based on coupling the studied drugs with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) in the presence of alkaline borate buffer. Spectrophotometric measurement was achieved by recording the absorbance at 466 and 464 nm for GMF and MOX, respectively, after a fixed time of 20 and 15 min on a water bath adjusted at 70 ± 5°C for both drugs. The different experimental parameters affecting the development and stability of the color were carefully studied and optimized. The absorbance-concentration plots were linear over the ranges 0.5–8.0 and 2.0–12 μg mL−1for GMF and MOX, respectively. The limit of detection of the kinetic method was about 0.12 (2.47 × 10−7 M) and 0.36 (8.22 × 10−7 M) μg mL−1for GMF and MOX, respectively. The proposed methods have been applied and validated successfully with percentage relative standard deviation (RSD% ≤ 0.52) as precision and percentage relative error (RE% ≤ 1.33) as accuracy. The robustness of the proposed method was examined with recovery values that were 97.5–100.5 ± 1.3–1.9%. Statistical comparison of the results with the reference spectrophotometric methods shows excellent agreement and indicates no significant difference in accuracy or precision.

scholarly journals Determination of metoprolol in pure and pharmaceutical dosage forms by spectrofluorometry and high performance liquid chromatography

2011 ◽  
Vol 17 (1) ◽  
pp. 25-31 ◽  
Author(s):  
Bilal Yilmaz ◽  
Kadem Meral ◽  
Ali Asci ◽  
Yavuz Organer
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Solvent System ◽  
Dosage Forms ◽  
Content Uniformity ◽  
Pharmaceutical Dosage Forms ◽  
Relative Standard ◽  
Limit Of Quantitation

In this study, a new and rapid spectrofluorometry and high performance liquid chromatography (HPLC) methods were developed for determination of metoprolol in pure and pharmaceutical dosage forms. The solvent system, wavelength of detection and chromatographic conditions were optimized in order to maximize the sensitivity of both the proposed methods. The linearity was established over the concentration range of 50-4000 ng ml-1 for spectrofluorometry and 5.0-300 ng ml-1 for HPLC methods. The intra- and inter-day relative standard deviation (RSD) was less than 4.14 and 3.86% for spectrofluorometry and HPLC, respectively. Limit of quantitation was determined as 30 and 5.0 ng ml-1 for spectrofluorometry and HPLC, respectively. No interference was found from tablet excipients at the selected assay conditions. The methods were applied for the quality control of commercial metoprolol dosage forms to quantify the drug and to check the formulation content uniformity.

A Validated HPLC Method for Simultaneous Determination of Perindopril Arginine, Amlodipine, and Indapamide: Application in Bulk and in Different Pharmaceutical Dosage Forms

2017 ◽  
Vol 100 (4) ◽  
pp. 992-999 ◽  
Author(s):  
Ramzia I El-Bagary ◽  
Ehab F Elkady ◽  
Shereen Mowaka ◽  
Maria A Attallah
Keyword(s):  
Potassium Dihydrogen Phosphate ◽  
Pharmaceutical Preparations ◽  
Dosage Forms ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Pharmaceutical Dosage Forms ◽  
Potassium Dihydrogen ◽  
Accuracy And Precision ◽  
Significant Difference

Abstract A simple, accurate, and precise LC method with a reversed stationary phase was developed and validated for the determination of perindopril (PER) arginine, amlodipine (AML), and indapamide (IND) alone and in binary mixtures (PER arginine is found in two dosage forms, i.e., with either AML or IND). Chromatographic separation was carried out on a BDS Hypersil® C18 column (100 × 3 mm, 5 μm). The mobile phase, consisting of 0.05 M potassium dihydrogen phosphate buffer (pH 2.6)–methanol (50 + 50, v/v), was pumped through the column whose temperature was maintained at 50°C at a flow rate of 0.6 mL/min using isocratic elution, and UV detection at 215 nm was performed. Acceptable values of linearity, accuracy, and precision of the method were found over the concentration ranges of 5–80 μg/mL PER, 2.5–80 μg/mL AML, and 0.5–20 μg/mL IND. The proposed chromatographic method was statistically compared to that of reference methods using one-way analysis of variance. The results showed that there was no significant difference between the methods. The developed method proved reliable for use in accurate QC of the drugs in their pharmaceutical preparations.

scholarly journals NEW STABILITY-INDICATING ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY METHOD DEVELOPMENT AND VALIDATION OF LENVATINIB MESYLATE IN BULK DRUG AND PHARMACEUTICAL DOSAGE FORMS

2018 ◽  
Vol 11 (9) ◽  
pp. 140
Author(s):  
Jahnavi Bandla ◽  
S. Ganapaty
Keyword(s):  
Liquid Chromatography ◽  
Dosage Form ◽  
Ultra Performance Liquid Chromatography ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Relative Standard ◽  
Validation Parameters ◽  
Bulk Drug

Objective: The objective of the present study was to develop and validate a new stability-indicating method for the quantification of lenvatinib mesylate in bulk drug and pharmaceutical dosage form using ultra performance liquid chromatography (UPLC).Methods: The optimized chromatographic conditions for elution of drug included UPLC HSS C18 (100 mm × 2.1 mm, 1.8 m) column, mixture of 0.1% orthophosphoric acid and acetonitrile (50:50 v/v%) mobile phase run on an isocratic mode at a flow rate of 0.3 mL/min, 240 nm detection wavelength, and column oven temperature maintained at 30°C.Results: The retention time for lenvatinib was found to be 1.24 min. The developed method was validated for various validation parameters in accordance with the International Conference on Harmonization guidelines. The method obeyed Beer’s law in the concentration range of 2.5– 15 μg/mL with a correlation coefficient of 0.9996. The percentage relative standard deviation and percentage recovery were determined to be 0.4 and 99.66–100.30%, respectively. The developed method was found to be accurate, precise, specific, linear, rugged, and robust. Forced degradation studies were conducted by exposing the drug to diverse stress conditions such as acidic, basic, peroxide, neutral, photolytic, and thermal conditions. The net degradation was obtained within the limits.Conclusion: The developed method for the estimation of lenvatinib can be employed to routine analysis of pharmaceutical dosage form.

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