A simple, fast, sensitive and accurate spectrophotometric method has been developed for the quantitative determination of cephalexin monohydrate in dosage form and in commercial formulations. The method involves the addition of Ce IV to cephalexin in acidic medium, followed by the determination of residual Ce IV by reacting with a fixed amount of methyl orange, and the absorbance was measured at 510 nm. Beer's law was obeyed in the concentration range of 0.6-20 µg mL -1 with correlation coefficient of 0.992. The molar absorptivity was calculated and was found to be 9.8 × 10 4 L mol -1 cm -1. Different variables affecting the reaction conditions such as concentration and volume of Ce IV , type and concentration of acids used, reaction time and temperature were carefully studied and optimized. The limit of detection (LOD) and limit of quantification (LOQ) were calculated and found to be 0.221 and 0.736 µg mL -1 , respectively. The proposed method was found to have good reproducibility with a relative standard deviation of 4.4% (n = 9). The interference effects of common excipients found in pharmaceutical preparations were studied. The developed method was validated statistically by performing recoveries studies and successfully applied for the determination of cephalexin in bulk powder and pharmaceutical preparations. Percent recoveries were calculated and found to range from 90.6 to 102.9% for bulk powder and from 98.7 to 104.8% for pharmaceutical preparations.
A responsive spectrofluorimetric method was developed for the determination of sitagliptin phosphate using L‐tyrosine as a fluorescence probe. The fluorescence intensity of L‐tyrosine was quenched with sitagliptin phosphate. The fluorescence intensity was recorded at 307 nm using a 272 nm excitation wavelength. The calibration plot between fluorescence intensity and the concentration of drug was liner in the range of 0.1 to 2.0 mM with a good correlation value of 0.997. The limit of detection and quantification were established to be 3.7 × 10‐4 and 1.23 × 10‐3 mM, respectively. Commonly used excipients did not interfere with sitagliptin phosphate measurement. The proposed method was used to measure the sitagliptin phosphate in its standard type, dosage form, and biological samples. The percent recovery were ranged from 97.41–103.36 %. The static quenching was shown to be responsible for quenching as indicated by the Stern–Volmer plot. The method was validated usin ICH guidelines and profitably applied for the content uniformity test, ensuing in a high percent recovery and small relative standard deviation. The proposed approach is effortless, susceptible, selective, economic, and provides a high precision and accuracy, and can be used to determine sitagliptin phosphate in pharmaceutical industry.
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