Determination of Amlodipine Besilate and Azilsartan Medoxomil by UHPLC, HPTLC and Spectrophotometric Techniques

Abstract

Aims: To develop methods with complete validation according to ICH guidelines and to be applied for the determination of both drugs in laboratory prepared mixtures and in synthetic tablets.
 Study Design: Ultra high performance liquid chromatography (UHPLC), High performance thin layer chromatography (HPTLC) and visible spectrophotometric methods are developed for determination of amlodipine besilate and azilsartan medoxomil in laboratory-prepared mixtures and in synthetic tablets.
 Methodology: Two techniques have been developed for the simultaneous determination of amlodipine besilate and azilsartan medoxomil in pure form and synthetic tablets. The first was UHPLC in which separation was achieved on a C18 column using 0.1% o-phosphoric acid - acetonitrile - methanol (60:10:30, by volume) as mobile phase with detection at 243nm. The second was HPTLC where separation was performed on silica gel 60 F254 plates using chloroform- tolune-methanol-glacial acetic acid (7: 1.5: 1.5: 0.5 by volume) as a developing system and UV detection at 243nm. In addition, visible- spectrophotometric method was developed for determination of amlodipine besilate in presence of azilsartan medoxomil through formation of yellowish orange colored product after reaction of amlodipine besilate with anisaldehde in acid medium with λmax at 443 nm.
 Results: UHPLC method was linear over the concentration ranges of 2-20 μg/ mL and 4-40 μg/ mL while HPTLC method was linear over the concentration ranges of 0.2 -4.0 μg/ spot and 0.5-8.0 μg/ spot for amlodipine besilate and azilsartan medoxomil, respectively. The visible spectrophotometric method was found to be valid over the concentration range of 10–80 μg/mL for amlodipine besilate.
 Conclusion: The proposed three techniques are rapid, accurate and precise, thus can be effectively applied for the routine estimation of both drugs in bulk and in their combined formulations.

The Development and Validation of Fast and Robust Stability Indicating RP-HPLC Method for Simultaneous Estimation of Azilsartan Medoxomil and Cilnidipine in Pharmaceutical Dosage Form

“…3 It is reported officially in Indian Pharmacopoeia (IP)-2018. 4 Literature study revealed that the analytical techniques like HPTLC, [5][6] HPLC, [7][8] UVspectrophotometry, 9,10 LC/MS-MS [11][12] methods have been presented for determination of Azilsartan medoxomil and Cilnidipine as a single, while for the combination of Azilsartan medoxomil and Cilnidipine method is available on UV-spectroscopy 13 and HPLC, 14 there is no article related to Stability Indicating HPLC Assay method to quantify Azilsartan medoxomil and Cilnidipine in bulk has ever been mentioned within literature referred. The primary goal of this project was to produce a specific, accurate, and reproducible stability indicating HPLC methods for determination of Azilsartan medoxomil and Cilnidipine as stated in the ICH guidelines.…”

Sensitive and validated TLC densitometry method coupled with fluorescence detection for quantitative determination of the newly co-formulated drugs, celecoxib and amlodipine besylate in tablet dosage form

“…Numerous analytical techniques have been established for the determination of CEL and AMLO alone or combined with other drugs as spectrophotometric [8][9][10][11], spectrofluorometric [12][13][14][15], high-performance thin-layer chromatography (HPTLC) [16][17][18][19][20][21][22][23][24][25][26][27][28][29][30], HPLC [31][32][33], and electrochemical methods [34,35]. A few recently analytical techniques have been established for the simultaneous estimation of CEL and AMLO such as spectrophotometric [36], spectrofluorimetric [37], and HPLC [38,39].…”

Application of Design of Experiment Based Innovative Approach in Method Development and Validation of RP-HPLC for Estimation of Azilsartan in Bulk and Pharmaceutical Tablet Dosage Form

“…The literature review on the availability of analytical methods for Azilsartan revealed a UV spectroscopic method, 7 few ultra-performance liquid chromatographic method and LC-MS methods for the quantification of Azilsartan in bulk drug, plasma 8,9 and combination with other drugs 10,11 and stability-indicating high-performance thin layer chromatographic (HPTLC) method. 12 In the literature survey, many chromatographic analytical methods were developed having several drawbacks include high buffer concentration leads to column damage, time-consuming and tedious. It needs to develop a method that resolves the problems of the previous methods.…”