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Ampicillin and cloxacillin were degraded together under different stress test conditions prescribed by International Conference on Harmonization. The samples so generated were used to develop a stability-indicating high performance liquid chromatographic (HPLC) method for the two drugs. The drugs were well separated from degradation products using a reversed-phase (C-18) column and a mobile phase comprising of acetonitrile:phosphate buffer (pH 5.0), which was delivered initially in the ratio of 15:85 (v/v) for 1 min, then changed to 30:70 (v/v) for next 14 min, and finally equilibrated back to 15:85 (v/v) from 15 to 20 min. Other HPLC parameters were: flow rate, 1 ml/min; detection wavelength, 225 nm; and injection volume, 5 microl. The method was validated for linearity, precision, accuracy, specificity and selectivity. It was also compared with the assay procedures given in British Pharmacopoeia for individual drugs. Similar results were obtained, indicating that the proposed single method allowed selective analysis of both ampicillin and cloxacillin, in the presence of their degradation products formed under a variety of stress conditions. The developed procedure was also applicable to the determination of instability of the drugs in commercial products.

A method for the analysis of degraded products of amoxycillin, ampicillin and cloxacillin in drug formulations, obtained as a result of their base hydrolysis is described. Simultaneous spectrophotometric and volumetric determinations of the antibiotic is based on the neutralization of the degraded product by dilute hydrochloric acid to get a pH approximately 2 to be conducive for redox titration using potassium iodate as titrant. A red purple colour is developed in carbon tetrachloride at the end point. Spectrophotometry is done after separating the organic layer and measuring the absorbance of red-purple colour at lambda(max) 520 nm. The pathways of different degraded products and their oxidation mechanism is described on IR, TLC and UV spectroscopic studies.

A spectrophotometric method is described for the assay of ampicillin in the presence of cloxacillin in pharmaceutical preparations. It involves the reaction of hydrolysed ampicillin with formaldehyde in an acidic phosphate buffer (pH 2.5) and measurement of the absorbance of the product at 373 nm after dilution with 2 M sulphuric acid. The method is selective for ampicillin in the presence of cloxacillin. The absorbance had a linear relationship with concentration for the range studied (5-35 micrograms ml-1). By this method the ampicillin content of combined preparations of ampicillin and cloxacillin has been successfully determined in capsules, injections and a syrup.

A method of reducing disturbing peaks in LC-chromatograms is described. The technique, here called digital subtraction chromatography (DSCh), makes use of the new generation of integrating chromatographic data processors. These processors are able to store the LC-detector signal and then subtract one chromatogram from another with the resulting chromatogram reintegrated and reprinted. The possibility of getting a useful chromatogram by subtracting a zero sample chromatogram from a sample with disturbing peaks is demonstrated. The theoretical background of the method is given together with a discussion of the optimisation of the chromatographic conditions. A bioanalytical application is given.