Spectroscopic Substantiation for the Identification of Degradants by Q-TOF Micromass (ESI-MS) in Bisoprolol Fumarate with an Inventive Validation Approach for Stability Indicating HPLC Method

A simple, accurate and precise stability-indicating RP-HPLC method was developed and subsequently validated for simultaneous determination of ilaprazole and domperidone in bulk and pharmaceutical dosage form. The proposed HPLC method utilizes C18 (250 mm × 4.6 mm × 5 µm) column with mobile phase comprising of 0.5 % glacial acetic acid in water pH 5.5 adjusted with ammonia solution: methanol in the ratio 45:55 v/v at a flow rate of 1.0 ml/min. Quantitation was achieved with UV detection at 286 nm based on peak area with linear calibration curves at concentration ranges 80-120µg/ml for ilaprazole and 240-360 µg/ml for domperidone with correlation coefficient of 0.999.The retention times of ilaprazole and domperidone were found to be 3.0 min, 5.4 min respectively. The mean recoveries obtained for ilaprazole and domperidone were found to be 99.76 ± 0.6463 % and 100.7 ± 0.2424 % respectively. Stress testing which covered acid, alkali hydrolysis, and peroxide, photolytic, thermal degradation was performed to prove the specificity of the proposed method and degradation was achieved. The proposed method was successfully applied for the stability indicating simultaneous estimation of ilaprazole and domperidone in routine quality control analysis in bulk and pharmaceutical formulation.

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Development and Validation of Stability Indicating HPLC Method for the Determination of Impurities in the Sterile Mixture of Cefoperazone and Sulbactam

Current Pharmaceutical Analysis ◽

10.2174/1573412914666180914163419 ◽

2019 ◽

Vol 15 (7) ◽

pp. 762-775

Author(s):

Ramu Ivaturi ◽

Thuttagunta Manikya Sastry ◽

Satyaveni Sunkara

Keyword(s):

Quantitative Estimation ◽

Ammonium Hydroxide ◽

Hplc Method ◽

Forced Degradation ◽

Buffer Solution ◽

Solution Ph ◽

Pharmaceutical Dosage Forms ◽

Stability Indicating ◽

Validation Parameters ◽

Abdominal Infections

Background: Cefoperazone Sulbactam injection is a cephalosporin antibiotic with a β- lactamase inhibitor used in the treatment for intra abdominal infections, Urinary track infections, surgical infections, etc. The combination is not official in any of the pharmacopeia for their content and impurities determination. Introduction: The present study involves the development of a simple, rapid, accurate, sensitive and stability indicating RP-HPLC method for the quantitative estimation of Cefoperazone Sulbactam mixture and its impurities in bulk and pharmaceutical dosage forms. Methods: 0.005 M Tetrabutyl ammonium hydroxide buffer solution pH adjusted to 6.80 and Acetonitrile combination has been used in a gradient programme with a flow rate of 1.0 ml/min. The retention time of Cefoperazone and Sulbactam were observed at around 8.5 and 19.5 minutes respectively. The UV detection was carried out at a wavelength of 230 nm. The chromatographic separation was achieved using Waters xbridge C18-150*4.6 mm, 3.5 µm HPLC column. The method has been validated according to the current International Council for Harmonization (ICH) guidelines for the method validation parameters such as Specificity, linearity, range, accuracy, precision, robustness and sensitivity. Results: The validation results indicate that the method is specific, as the known impurities and other impurities formed during the forced degradation studies were not co-eluting with the main components. Moreover, all these impurities were found to be spectrally pure, proving the stability indicating power of the method. The linearity and range of the method is in the range of 0.01-150%, highly accurate (100.2%), precise (<1%) and robust. Conclusion: The proposed method was accurate and specific for the quantitative analysis of Cefoperazone and Sulbactam and their related impurities in the sterile mixture. Hence the proposed method can be used for the quantification of impurities in routine as well as stability analysis in the development as well as quality control laboratories.

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