Determination Of Amlodipine Besylate Research Articles

Use of sodium tetraphenylborate reagent for conductometric titration of Amlodipine Besylate in pure and pharmaceutical forms

Simple, accurate and reliable conductometric method for the quantitative determination of Amlodipine Besylate (AML) in pure form and pharmaceutical formulations using sodium tetraphenylborate (TPB) in aqueous solution at 20°C has been described. The method is based on the formation of ion association complex of cation coming from the cited drug with tetraphenylborate anion and the conductance of the solution is measured as a function of the volume of titrant. Many experimental conditions were evaluated. The described procedure allowed the determination of AML in double distilled water in the range of 0.200-1.000mM. The accuracy of the method is indicated by the excellent recovery 98.60-101.40%, and the precision is supported by the low relative standard deviation < 4.74 %. The method was further applied successively to pharmaceutical formulations with no interference from the excipients, the results obtained were compared statistically with those obtained by the official method and showed no significant differences regarding accuracy and precision.

Use of sodium tetraphenylborate reagent for conductometric titration of Amlodipine Besylate in pure and pharmaceutical forms

Simple, accurate and reliable conductometric method for the quantitative determination of Amlodipine Besylate (AML) in pure form and pharmaceutical formulations using sodium tetraphenylborate (TPB) in aqueous solution at 20°C has been described. The method is based on the formation of ion association complex of cation coming from the cited drug with tetraphenylborate anion and the conductance of the solution is measured as a function of the volume of titrant. Many experimental conditions were evaluated. The described procedure allowed the determination of AML in double distilled water in the range of 0.200-1.000mM. The accuracy of the method is indicated by the excellent recovery 98.60-101.40%, and the precision is supported by the low relative standard deviation < 4.74 %. The method was further applied successively to pharmaceutical formulations with no interference from the excipients, the results obtained were compared statistically with those obtained by the official method and showed no significant differences regarding accuracy and precision.

UV Spectrophotometric Method Development and Validation for Amlodipine Besylate in Bulk and Tablet Dosage Form

Analytical method development and validation is important in development of pharmaceutical preparations. In present study a spectroscopic method for determination of Amlodipine besylate in pharmaceutical dosage form has been developed and validated. The wavelength maxima of Amlodipine besylate was found to be 360nm. Ethanol was used as a solvent. Amlodipine besylate obeys beers law in the concentration range of 5-40μg/ml. The line equation obtained is y = 0.0136x + 0.001 with correlation coefficient (r2) of 0.998. Interday, intraday variations were studied to determine the precision of the proposed method and was found to be with good precision as the %RSD was less than 2%. The assay of 2 different marketed formulation (A and B) has been performed and the % assay of A and B was found to be 98.3% and 99.2% respectively. The sensitivity of the method was determined by LOD and LOQ was found to be 0.08123µg/ml and 0.2461µg/ml respectively. The method employed the parameters like linearity, accuracy, precision, sensitivity, robustness, ruggedness and all the procedures were as per ICH guidelines.

Validated green chromatographic methods for determination of amlodipine and celecoxib in presence of methylacetophenone.

Aim: Green, accurate and rapid methods, namely LC-MS/MSand thin layer chromatography-densitometric methods, were developed for determination of amlodipine besylate and celecoxibin presence of its process-related impurities, 4-methylacetophenonein pure and formulated tablets. Results: LC-MS/MS was achieved on ZORBAX Eclipse Plus C18 column using methanol:aqueous solution of 5mM formic acid (95:5v/v). High sensitivity with low limit of detectionvalues 0.00028, 0.00027 and 0.0003 for amlodipine, celecoxib and 4-methylacetophenone, respectively were obtained. While, thin layer chromatography-densitometric was established using methanol:water:ammonia (70:25:1.5, by volume). Good linearity was obtained in the range of 0.1-10μg/band, 1-150μg/band and 0.01-2μg/band for amlodipine, celecoxib and 4-methylacetophenone, respectively. Conclusion: The proposed method validation was achieved according to ICH guidelines. Those methods possess advantages of being ecofriendly methods which permit their application in quality control laboratories.

Development and Validation of RP-HPLC Method for Determination of Amlodipine Besylate, Telmisartan and Rosuvastatin Calcium from Synthetic Mixture

Development and Validation of RP-HPLC Method for Determination of Amlodipine Besylate, Telmisartan and Rosuvastatin Calcium from Synthetic Mixture

Development of Colorimetric Method for the Quantitative Analysis of Amlodipine Besylate in Dosage form Using 4- Dimethyleaminobenzaldehyde as Derivatizing Reagent

The study is based on the determination of amlodipine besylate (AB) after derivatization with 4-dimethylaminobenzaldehyde (DMAB) using UV/Visible spectrophotometer at pH 5 to yield derivative that is measured at λ max 399 nm. The calibration graph obtained was liner and fulfilled Beer Lambert’s law in the concentration range 05-25 μg/mL of (AB) and DMAB having coefficient of determination R² 0.9988 with RSD 0.93% and molar absorptivity 4.04x103 mole-1 cm-1. Quantitative / analytical parameters such as pH, heating time, temperature were optimized. Reagent concentration /volume, interday and intraday studies were also carried out. There was no effect of various solvents and additives observed on the determination of AB in commercially available drugs. The method is stable, accurate, rapid and simple for the study of imine derivative of AB.

Количественное определение амлодипина бесилат в таблетках комбинированных антигипертензивных препаратов методом УФ-спектрофотометрии

Количественное определение амлодипина бесилат в таблетках комбинированных антигипертензивных препаратов методом УФ-спектрофотометрии

Spectrophotometric and High Performance Liquid Chromatographic Determination of Amlodipine Besylate and Nebivolol Hydrochloride in Tablets Dosage Form

Introduction: Absorbance ratio spectrophotometric method and high performance liquid chromatographic method were developed for the determination of the Amlodipine Besylate and Nebivolol Hydrochloride in tablet dosage form. Methods: Absorbance ratio spectrophotometric method and high performance liquid chromatographic method were developed for the determination of the Amlodipine Besylate and Nebivolol Hydrochloride in tablet dosage form. A simple liquid chromatographic assay has been developed for the determination of Amlodipine Besylate and Nebivolol Hydrochloride. A C 18 (250×4.6 mm, 5 μ) column was used with a mobile phase consisting of Water: Acetonitrile ( pH adjusted to 3.5 with ortho phosphoric acid) at a flow rate of 1.0 ml min -1 . Quantitation was achieved with UV detection at 268 nm based on the peak height ratios. Results: Calibration curves were linear in the range of 10–30 μg/ml for Amlodipine Besylate and 10-30 μg/ml for Nebivolol Hydrochloride in absorbance ratio method. Correlation coefficient found to be close to 0.9995 for both the drugs. Accuracy for both the drugs was in the range of 99-101%. Beer’s law was obeyed in a concentration range of 10-30 mg ml -1 for Amlodipine Besylate and 10-30 mg ml -1 for Nebivolol Hydrochloride and the regression line equation was derived with a correlation coefficient of 0.9999 and 0.9998 for Amlodipine Besylate and Nebivolol Hydrochloride respectively. Discussion: The proposed procedures were successfully applied to the determination of Amlodipine Besylate and Nebivolol Hydrochloride in bulk and tablet form, with high percentage of recovery, good accuracy and precision. Key words: Amlodipine Besylate, Nebivolol Hydrochloride, Absorbance ratio method, HPLC, Tablets.

Design of Experiments in Optimization and Validation of a Hydrophilic Interaction Liquid Chromatography Method for Determination of Amlodipine Besylate and Bisoprolol Fumarate

In this paper chemometrically-assisted optimization and validation of hydrophilic interaction liquid chromatographic (HILIC) method for the quantitative analysis of amlodipine besylate (AB) and bisoprolol fumarate (BF) in pharmaceuticals are presented. In this study, the development of HILIC method for AB and BF separation was performed by a systematic approach which included Design of Experiments (DoE) methodology. First, in method optimization, a central composite design was applied. Influence of the acetonitrile content in the mobile phase, pH of the aqueous phase, and concentration of ammonium acetate on selected chromatographic responses was investigated. Optimal chromatographic conditions in terms of adequate separation and minimal analysis duration were set by graphical optimization overlapping the contour plots as: acetonitrile–water phase (10 mM ammonium acetate, pH 4.0 adjusted with glacial acetic acid) (92:8, v/v), column Luna HILIC 200 A, 150 mm × 4.6 mm, 5 µm particle size, column temperature 30°C, flow rate 1 mL min−1, and UV detection at 230 nm. After this step, method robustness was tested using a 25-1 fractional factorial design. Statistical and graphical evaluation of results confirmed robustness of the method and then the method was fully validated. Finally, the proposed method was successfully applied for AB and BF determination in pharmaceuticals.

Quantitative Determination of Amlodipine Besylate, Losartan Potassium, Valsartan and Atorvastatin Calcium by HPLC in their Pharmaceutical Formulations

Amlodipine besylate is a calcium channel blocker which is used in treatment of hypertension alone or in combination with other antihypertensive drugs like angiotensin-II-receptor antagonists (ARA II) group (Losartan potassium and Valsartan) or in combination with anti hyperlipidemic agent like Atorvastatin calcium. RP- HPLC method was developed for the assay of these drugs. The method was performed by reversed phase high performance liquid chromatography using a mobile phase 0.01 M ammonium acetate buffer (pH 5.5): acetonitrile with detection at 240 nm on a spherical monomeric C18 column (250 mm × 4.6 mm, 5 μm) at flow rate of 1.5 ml/min. The proposed method was validated in terms of linearity ranged between [(2-12, 10-60, 16-96, 4-24 μg/ml) corresponding levels of 20-120% w/w of the nominal analytical concentration] with linear regression equations were [{y=64.627x – 3.6383 (r= 0.9998), y=75.385x – 8.3856 (r= 0.9997), y=64.492x – 25.981 (r= 0.9998), y=70.964x – 28.505 (r= 0.9998}], accuracy [100.18 ± 1.38, 100.79 ± 0.59, 100.45 ± 0.58 and 100.8 ± 1.69%], precision [99.29, 99.33, 99.30 and 99.30%], limits of detection [0.03, 0.18, 0.15, 0.007 μg/ml] and limits of quantitation [0.1, 0.54, 0.45, 0.024 μg/ml] for Amlodipine besylate, Losartan potassium, Valsartan and Atorvastatin calcium respectively. Method validation was developed following the recommendations for analytical method validation of International Conference on Harmonization (ICH) and Food and Drug Administration (FDA) organizations.

DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE SIMULTANEOUS ESTIMATION OF AMLODIPINE AND HYDROCHLOROTHIAZIDE IN TABLETS: APPLICATION TO DISSOLUTION STUDY

A sim ple, specific , accurate , rapid , inexpensive isocratic Reversed Phase - High Performance Liquid Chromatography (RP - HPLC) method was developed and validated f or the quantitative determin ation of Amlodipine besylate and Hydrochlorothiazide in pharmaceutical tablet dosage forms and HPLC method was used for an in vitro dissolution study of tablets containing the above drugs. RP - HPLC method was developed by using W elchrom C 18 Column (4.6 X 250 mm, 5 µm), Shimadzu LC - 20AT Prominence Liquid C hromatograph. The mobile phase composed of 10 mM P hosphate buffer (pH - 3.0, adjusted with triethylamine) : acetonitrile ( 50 : 50 v/v ) . The flow rate was set to 1.0 mL . min - 1 with the responses measured at 2 30 nm using Shimadzu SPD 20A Prominence UV - V is detector. The dissolution test was performed using 900 mL of distilled water as the dissolution media at 50 rpm using an USP Apparatus II at 37°C. The retention time s of Hydrochlorothiaz ide and Amlodipine besylate were found to be 3.373 min utes and 3.753 min utes respectively . Linearity was established for Amlodipine besylate in the range of 1 - 5 µg / mL with correlation coefficient 0.999 5 and Hydrochlorothiazide in the range of 3 - 15 µg / m l with correlation coefficient 0.9996 . The validation of the developed method was carried out for specificity, linearity, precision, accuracy, robustness, limit of detection, limit of quanti t ation. The developed method can be used for routine quality contr ol analysis of Amlodipine besylate and Hydrochlorothiazide in pharmaceutical tablet dosage form.

Simultaneous Determination of Amlodipine and Aliskren in Tablets by High-Performance Liquid Chromatography

A new, simple, rapid and specific reversed-phase high-performance liquid chromatography (HPLC) method was developed and validated for the simultaneous determination of amlodipine besylate and aliskiren hemifumarate. The HPLC separation was achieved on an RP-18 column (250 × 4.6 mm) using a mobile phase of triethylamine-orthophosphoric acid buffer (50 mM, pH 3.0), acetonitrile and methanol (50:40:10, v/v/v) at a flow rate of 1 mL/min. The method was validated for specificity, linearity, precision, accuracy and robustness. The degree of linearity of the calibration curves, the percent recovery values of amlodipine and aliskiren and the limits of detection (LOD) and quantification (LOQ) for the HPLC method were determined. The linearity of the method was found to be in the concentration range of 5.0-50.0 µg/mL for aliskiren hemifumarate and 2.65-26.50 µg/mL for amlodipine besylate, LOD and LOQ values were 0.51, 0.95, 1.70 and 3.18 µg/mL for amlodipine besylate and aliskiren hemifumarate. The proposed method was successfully applied to amlodipine besylate and aliskiren hemifumarate in pharmaceutical dosage mixtures without any interference from the excipients. The method was found to be precise, accurate, reproducible and robust. The results agreed with those obtained using the developed reference method.

HIGH PERFORMANCE LIQUID CHROMATOGRAPHY, TLC-DENSITOMETRY, AND FIRST-DERIVATIVE SPECTROPHOTOMETRY FOR SIMULTANEOUS DETERMINATION OF AMLODIPINE AND PERINDOPRIL IN BULK POWDER AND ITS TABLETS

Three simple, sensitive, and specific methods were developed for simultaneous determination of amlodipine besylate (AML) and Perindopril Erbumine (PER) without previous separation. The first method was dependent on the first derivative of the ratio spectra by measuring the amplitudes at 348 nm for amlodipine using 50 µg mL−1 of perindopril as a divisor and at 227 nm for perindopril using 30 µg mL−1 of amlodipine as a divisor. The second method was based on ion-pair RP-HPLC. Satisfactory resolution was achieved using RP-C18 chromatographic column Zorbax Extend column and a mobile phase consists of potassium dihydrogen phosphate buffer (0.05 M, pH 3.0 ± 0.02 adjusted by orthophosphoric acid): acetonitrile 30:70 v/v at a flow rate 1 mL/min using 0.002 M sodium heptanesulfonate in the aqueous phase. UV detection was performed at 215 nm. The third method was based on TLC; the separation was carried out on Fluka TLC aluminum sheets silica gel 60 F254, using n-butanol:water:glacial acetic acid (4:5:1, v/v/v) as the mobile phase. The validation of the proposed methods was applied according to ICH guidelines and LOD and LOQ were calculated. The suggested methods were successfully applied for the determination of the cited drugs in bulk powder and commercial tablets.

HPLC DETERMINATION OF AMLODIPINE IN BIOLOGICAL FLIUIDS USING HOLLOW FIBER BASED LIQUID-LIQUID-LIQUID MICROEXTRACTION

A sensitive and precise method is described for determination of amlodipine besylate (AMB) in biological samples using hollow fiber based liquid-liquid-liquid microextraction (HF-LLLME) followed by high performance liquid chromatography. Different effective parameters on extraction efficiency were studied and optimized. The analyte was extracted from 11.0 mL diluted urine and plasma samples containing 0.1 mol L−1 NaOH (donor phase) into dibenzyl ether membrane phase impregnated in the pores of the hollow fiber wall and back extracted into the 25 µL acceptor phase (0.01 mol L−1 HCl) located inside the lumen of the hollow fiber. The analyte enriched acceptor phase was finally withdrawn into the microsyringe and directly injected into HPLC for the separation and quantification of the target analyte. The performance of the proposed method was studied in terms of dynamic linear ranges, coefficients of determination, precision, and limits of detection and quantification. The relative recoveries of AMB in plasma and urine samples were 96.4% and 97.2% with RSDs of 6.3% and 4.8%, respectively.

Validated Chromatographic Methods for Simultaneous Determination of Amlodipine Besylate and Perindopril Arginine in Binary Mixtures and in Pharmaceutical Dosage Form

Two accurate, selective and precise chromatographic methods, namely TLC-densitometric method & RP-HPLC method & were developed and validated for the simultaneous determination of Amlodipine besylate and Perindopril Arginine in their binary mixtures. The developed TLC-densitometric method depends on separation and quantitation of the studied drugs on silica gel 60F254 TLC plates. Chloroform:methanol:deionized water:glacial acetic acid:triethylamine (10:7:5:0.3:0.2, by volume) was used as developing system and the separated bands were scanned at 208 nm. Linear relationship was obtained in the range 1-10 μg for both drugs. The developed RP-HPLC depends on quantitative chromatographic separation of the studied drugs on a C18 column using phosphate Buffer:acetonitrile (60:40, v/v), pH=4.6 as a mobile phase delivered at constant flow rate of 1 mL.min-1 with UV detection at 210 nm. Calibration curves for Amlodipine besylate and Perindopril Arginine were constructed over the concentration range of 1-50 μg.mL-1 for both drugs. The proposed methods were successfully applied for determination of the studied drugs in their bulk powder and in pharmaceutical formulations. The proposed methods were statistically compared to each other using student’s t test and F-test and no significant difference was found between them.

Development of HPTLC Method for Determination of Amlodipine Besylate and Olmesaratan Medoxomil Using Human Plasma by Liquid Liquid Extraction

A simple, sensitive, rapid and economic high performance thin layer chromatographic method has been developed for determination of amlodipine besylate and olmesaratan medoxomil in human plasma by liquid liquid extraction using paracetamol as an internal standard. The plasma sample was extracted using mixture of methanol: acetonitrile (3.0: 0.1). A concentration range from 500-3000 ng/spot of amlodipine besylate and olmesaratan medoxomil was used for calibration curve respectively. The percent recovery of amlodipine besylate and olmesaratan medoxomil was found to be 90.41 and 90.64 % respectively. The mobile phase consists of chloroform: methanol (9:1, v/v). Densitometric analysis was carried out at wavelength 254 nm. The Rf values for amlodipine besylate, olmesaratan medoxomil and paracetamol was 0.50 ± 0.05, 0.26 ± 0.05 and 0.66 ± 0.05 respectively. The stability of amlodipine besylate and olmesaratan medoxomil in plasma was confirmed during three freeze-thaw cycles at ‘-20°C’, on bench during 24 h and post preparative during 48 h. The proposed method was validated statistically and by performing recovery study for determination of amlodipine besylate and olmesaratan medoxomil in human plasma by liquid liquid extraction.

Validated HPLC and HPTLC Method for Simultaneous Quantitation of Amlodipine Besylate and Olmesartan Medoxomil in Bulk Drug and Formulation

Two methods are described for simultaneous determination of amlodipine besylate and olmesartan medoxomil in formulation. The first method was based on the HPTLC separation of two drugs on Merck HPTLC aluminium sheets of silica gel 60 F254 using n-butanol: acetic acid: water (5:1:0.1, v/v/v) as the mobile phase. The second method was based on the HPLC separation of the two drugs on the RP-PerfectSil-100 ODS-3–C18 column from MZ-Analysetechnik GmbH, Germany and acetonitrile/0.03 M ammonium acetate buffer (pH = 3) in a ratio of 55:45 as the mobile phase. Both methods have been applied to formulation without interference of excipients of formulation.

Determination of amlodipine besylate by adsorptive square-wave anodic stripping voltammetry on glassy carbon electrode in tablets and biological fluids

The adsorptive and electrochemical behavior of amlodipine besylate on a glassy carbon electrode were explored in Britton–Robinson buffer solution by using cyclic and square-wave voltammetry. Cyclic voltammetric studies indicated the oxidation of amlodipine besylate at the electrode surface through a single two-electron irreversible step and fundamentally controlled by adsorption. The solution conditions and instrumental parameters were optimized for the determination of the authentic drug by adsorptive square-wave stripping voltammetry. Amlodipine besylate gave a sensitive adsorptive oxidation peak at 0.510 V (versus Ag/AgCl). The oxidation peak was used to determine amlodipine besylate in range 4.0×10 −8 to 2.0×10 −6 with a detection limit of 1.4×10 −8 M. The procedure was successfully applied for the assay of amlodipine besylate in tablets (Norvasc) ®. The percentage recoveries were in agreement with those obtained by the reference method. Applicability to assay the drug in urine and serum samples was illustrated. The mean percentage recoveries were 96.31±1.18 and 96.98±1.17, respectively. The proposd method used for monotoring clinically relevant concntrations of drug in human urine and serum.

The Use of Charge-Transfer Complexation in The Spectrophotometric Determination of Amlodipine Besylate

A simple and sensitive analytical method has been developed for the spectrophotometric assay of amlodipine besylate (ADB) in pure forms and tablets have been described. The method is based on the formation of a charge-transfer complex between the drug and tetrachloquinone (TCQ). This complex exhibit intense absorption bands in the electronic spectrum. The molecular ratio of the reactant in the complex was established and the experimental conditions leading to maximum charge-transfer band was also studied. The reaction proceeds quantitatively at pH 9 and 55°C for 10 min, the absorbance was measured at 346 nm. The method was applied to commercially available tablets and the results were statistically compared wrth those obtained by UV spectrophotometric method, using Newman-Keuls tests. In our method, Beer's Law limits to 5-25 µg/ml. The optimum experimental parameters for colour production with reagent were studied and incorporated into procedure.

Spectrophotometric Determination of Amlodipine Besylate in Pure Forms and Tablets

ABSTRACT Two simple and sensitive spectrophotometric methods for the determination of amlodipine besylate (ADB) in pure forms and tablets are described. These methods are based on the formation of an ion association complex between the drug and an acidic dye, Bromothymol blue, which is extractable into chloroform and has an absorption maximum at 405nm (Method-A), or by the formation of an oxidative coupling product with 3-methyl-2-benzothiazolinone hydrazone hydrochloride (MBTH) in the presence of ceric ammonium sulphate (absorption maximum at 630nm (Method-B)). Beer's Law limits for Methods A and B are 5 to 40 μg/ml. All variables in these methods are optimised and the reaction mechanisms are presented. No interferences were observed from tablet additives and the applicability of the methods was examined by analysing tablets containing ADB. The quantities determined were 99.5–100.2% of the expected value.