Sensitive spectrophotometric methods for the determination of amoxycillin, ciprofloxacin and piroxicam in pure and pharmaceutical formulations

https://doi.org/10.1016/S0731-7085(02)00210-8Get rights and content

Abstract

Two simple, sensitive and accurate spectrophotometric methods have been proposed for the determination of amoxycillin (AMX), ciprofloxacin (CPF) and piroxicam (PIR) in pure and pharmaceutical preparations. The methods are based on the measurement of absorbances of tris(o-phenanthroline) iron(II) [method A] and tris (bipyridyl) iron(II) [method B] complexes at 510 and at 522 nm, respectively. Reaction conditions have been optimized to obtain coloured complexes of higher sensitivity and longer stability. The absorbances were found to increase linearly with increase in concentrations of AMX, CPF and PIR which were corroborated by correlation coefficient values. The complexes obeyed Beer's law over the concentration range of 0.06–5.2, 0.04–7.2 and 0.2–6.5 μg ml−1 for AMX, CPF and PIR, respectively, in method A, and of 0.05–8.5, 0.05–9.0 and 0.05–6.5 μg ml−1 for AMX, CPF and PIR, respectively, in method B. The developed methods have been successfully applied for the determination of AMX, CPF and PIR in bulk drugs and pharmaceutical formulations. The common excipients and additives did not interfere in their determinations. The results obtained by the proposed methods have been statistically compared by means of Student t-test and by the variance ratio F-test.

Introduction

Amoxycillin (AMX), chemically known as [6R-6-(α-p-hydroxyphenyl-d-glycylamino) penicillanic acid] trihydrate, is the only phenolic penicillin used as an antibacterial drug. Ciprofloxacin (CPF), 1-cyclopropyl-6-fluoro-4-dihydro-1,4-oxo-7-piperazine-1-ylquinoline-3-carboxylic acid, is an antibacterial agent with a broad spectrum of activity against a variety of gram positive and gram negative bacteria. Piroxicam (PIR), 4-hydroxy-2-methyl-N-2-pyridinyl-2H-1,2-benzothiazine-3-carboxamide 1,1-dioxide, is a non-steroidal anti-inflammatory agent used for the treatment of rheumatic diseases. AMX [1], [2], [3] and CPF [4] are official in BP and USP while PIR is official in USP [5]. The official methods involve potentiometric titration [1] using mercuric nitrate as titrant in acetate buffer and HPLC methods [2], [3] for the assay of AMX while those for CPF and PIR involve HPLC methods using phosphoric acid and acetonitrile (87:13), and phosphate buffer and methanol (55:45) as mobile phases, respectively.

Many spectrophotometric methods [6], [7], [8], [9], [10], [11], [12], [13], [14], [15], [16], [17], [18], [19], [20], [21], [22], [23], [24], [25], [26], [27], [28], [29], [30], [31], [32], [33], [34] have been reported for the determination of AMX [6], [7], [8], [9], [10], [11], [12], [13], [14], [15], [16], [17], CPF [18], [19], [20], [21], [22], [23], [24], [25], [26], [27] and PIR [28], [29], [30], [31], [32], [33], [34]. But none of these methods are satisfactory for routine quality assurance for one or the other reason. Some of these methods have low sensitivity [6], [8], [9], [10], [11], [13], [16], [17], [20], [21], [22], [23], [24], [26], [27], [29], [30], [31], [32], [33], [34] or work out only at higher concentrations of the drugs [6], [10], [11], [12], [18], [19], [26], [27], [29], [31], [32] or have less stability [13], [14], [17], [21], [22], [26], [32], [34] or involve extraction [9], [15], [24], [25], [28], [29]. Hence it was felt necessary to develop simple and sensitive spectrophotometric methods which do not suffer from the above limitations for the determination of AMX, CPF and PIR in bulk samples and pharmaceutical preparations using reagents such as Fe(III)-1,10-phenanthroline (FPL) and Fe(III)-2,2′-bipyridyl (FBL). The proposed methods are more advantageous compared to official methods, which are laborious.

Section snippets

Reagents

All chemicals used were of either analytical or pharmaceutical grade and quartz processed high-purity water was used throughout. Pure AMX was obtained from Cadila Healthcare Ltd., India and CPF and PIR were obtained from Cipla Ltd., India.

Various pharmaceutical formulations of AMX, CPF and PIR were obtained commercially. These formulations contain only one drug and do not exist in combination with other drugs.

Solutions

Aqueous solutions of standard AMX, CPF and PIR (1000 μg ml−1) were prepared and stored

Results and discussion

Ferric salts play a prominent role in the spectrophotometric determination of many pharmaceutical drugs. Acting as an oxidant, a ferric salt gets reduced to ferrous salt and this amount corresponds to drug concentration. The amount of Fe(II) can be determined using reagents such as 1,10-phenanthroline (PNL) and 2,2′-bipyridyl (BPL). These properties have been utilised to develop spectrophotometric methods for the determination of AMX, CPF and PIR.

Conclusion

The reagents provide fairly high sensitivity compared with most of the reagents reported earlier for the assay of AMX, CPF and PIR. The proposed methods are simple, accurate and economical with reasonable precision and accuracy. The FPL method was found to be more sensitive compared to FBL method for the assay of AMX, CPF and PIR. The coloured complexes are stable for more than 24 h, which makes the methods more practicable. The validity of the proposed methods is well demonstrated by analysing

Acknowledgements

The authors express their sincere thanks to Cadila Healthcare Ltd., India and Cipla Ltd., India for supplying gift samples of amoxycillin, ciprofloxacin and piroxicam. Thanks are also due to the Chairman, Department of Chemistry, Karnatak University, Dharwad for providing necessary facilities.

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