Analytical Separation and Characterisation of Degradation Products and the Development and Validation of a Stability-Indicating Method for the Estimation of Impurities in Levosalbutamol Respules Formulation

Anas Rasheed, Dr. Osman Ahmed

Abstract


A short selective, precise, accurate and sensitive stability-indicating gradient LC-MS/MSn method was developed for the quantitative determination of process-related impurities and degradation products of Levosalbutamol in pharmaceutical respules formulations. During the stress study, the degradation products of Levosalbutamol were well-resolved from Levosalbutamol and its impurities and the mass balances were found to be satisfactory in all the stress conditions, thus proving the stability-indicating capability of the method. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection and quantification, accuracy, precision, ruggedness, and robustness. During the stability analysis of the drug product, one unknown impurity was detected by the above stability-indicating method. The flow rate was 0.8 ml/min and effluent was monitored at 242nm. Retention time was found to be 2.237±0.08 min. The LOD and LOQ values were found to be 0.20984 (μg/ml) and 0.6359 (μg/ml) respectively.

Keywords


Levosalbutamol; LC-MS/MSn ; Validation; respules; stability indicating method; degradation products;

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References


International Conference on Harmonization (2005). Guideline on Validation of Analytical Procedures Text and Methodology: Q2 (R1).

Jain DK, Patel PN, Kushwaha A, Raghuwanshi RS, Jain N. Simultaneous determination of salbutamol sulphate and doxophylline in tablets by reverse phase liquid chromatography; Der Pharmacia Lettre. 2011;3(4):56–62.

Martis EA, Gangrade DM (2011). Reverse phase isocratic HPLC method for simultaneous estimation of salbutamol sulphate and beclomethasone dipropionate in rotacaps formulation dosage forms. Int J Pharm Pharm Sci. 3:64–7.

Michael E Swartz (2005). Ultra performance liquid chromatography UPLC: an introduction. Separation science redefined. 1:8-14.

S. Singh, M. Bakshi (2000). Guidance on conduct of stress tests to determine Inherent Stability of Drugs. Pharmaceutical Technology On-line. April 1-14..

Wu J, Ding C, Ge Q, Li Z, et al (2011). Simultaneous determination of ipratropium and salbutamol in rat plasma by LC–MS/MS and its application to a pharmacokinetic study. J Chromatogr B Anal Technol Biomed Life Sci. 879:3475–83.




DOI: http://dx.doi.org/10.21477/ijapsr.v2i03.8254

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