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Application of a validated stability-indicating densitometric thin-layer chromatographic method to stress degradation studies on moxifloxacin.
Anal Chim Acta 2007; 582(1):75-82AC

Abstract

A simple, sensitive, selective, precise and stability-indicating high-performance thin-layer chromatographic (HPTLC) method for densitometric determination of moxifloxacin both as a bulk drug and from pharmaceutical formulation was developed and validated as per the International Conference on Harmonization (ICH) guidelines. The method employed TLC aluminium plates pre-coated with silica gel 60F-254 as the stationary phase and the mobile phase consisted of n-propanol-ethanol-6M ammonia solution (4:1:2, v/v/v). Densitometric analysis of moxifloxacin was carried out in the absorbance mode at 298 nm. Compact spots for moxifloxacin were found at R(f) value of 0.58+/-0.02. The linear regression analysis data for the calibration plots showed good linear relationship with r=0.9925 in the working concentration range of 100-800 ng spot(-1). The method was validated for precision, accuracy, ruggedness, robustness, specificity, recovery, limit of detection (LOD) and limit of quantitation (LOQ). The LOD and LOQ were 3.90 and 11.83 ng spot(-1), respectively. Drug was subjected to acid and alkali hydrolysis, oxidation, dry heat, wet heat treatment and photodegradation. All the peaks of degradation products were well resolved from the standard drug with significantly different R(f) values. Statistical analysis proves that the developed HPTLC method is reproducible and selective. As the method could effectively separate the drug from its degradation products, it can be employed as stability-indicating one. Moreover, the proposed HPTLC method was utilized to investigate the kinetics of the acidic and alkaline degradation processes at different temperatures. Arrhenius plot was constructed and apparent pseudo-first-order rate constant, half-life and activation energy were calculated. In addition the pH-rate profile for degradation of moxifloxacin in constant ionic strength buffer solutions within the pH range 1.2-10.8 was studied.

Authors+Show Affiliations

Department of Pharmaceutics, Faculty of Pharmacy, Jamia Hamdard, Hamdard Nagar, New Delhi 110062, India. sanjay_bcp@rediffmail.com <sanjay_bcp@rediffmail.com>No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Validation Studies

Language

eng

PubMed ID

17386477

Citation

Motwani, Sanjay K., et al. "Application of a Validated Stability-indicating Densitometric Thin-layer Chromatographic Method to Stress Degradation Studies On Moxifloxacin." Analytica Chimica Acta, vol. 582, no. 1, 2007, pp. 75-82.
Motwani SK, Khar RK, Ahmad FJ, et al. Application of a validated stability-indicating densitometric thin-layer chromatographic method to stress degradation studies on moxifloxacin. Anal Chim Acta. 2007;582(1):75-82.
Motwani, S. K., Khar, R. K., Ahmad, F. J., Chopra, S., Kohli, K., & Talegaonkar, S. (2007). Application of a validated stability-indicating densitometric thin-layer chromatographic method to stress degradation studies on moxifloxacin. Analytica Chimica Acta, 582(1), pp. 75-82.
Motwani SK, et al. Application of a Validated Stability-indicating Densitometric Thin-layer Chromatographic Method to Stress Degradation Studies On Moxifloxacin. Anal Chim Acta. 2007 Jan 16;582(1):75-82. PubMed PMID: 17386477.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Application of a validated stability-indicating densitometric thin-layer chromatographic method to stress degradation studies on moxifloxacin. AU - Motwani,Sanjay K, AU - Khar,Roop K, AU - Ahmad,Farhan J, AU - Chopra,Shruti, AU - Kohli,K, AU - Talegaonkar,S, Y1 - 2006/09/01/ PY - 2006/06/09/received PY - 2006/08/25/revised PY - 2006/08/25/accepted PY - 2007/3/28/pubmed PY - 2007/6/1/medline PY - 2007/3/28/entrez SP - 75 EP - 82 JF - Analytica chimica acta JO - Anal. Chim. Acta VL - 582 IS - 1 N2 - A simple, sensitive, selective, precise and stability-indicating high-performance thin-layer chromatographic (HPTLC) method for densitometric determination of moxifloxacin both as a bulk drug and from pharmaceutical formulation was developed and validated as per the International Conference on Harmonization (ICH) guidelines. The method employed TLC aluminium plates pre-coated with silica gel 60F-254 as the stationary phase and the mobile phase consisted of n-propanol-ethanol-6M ammonia solution (4:1:2, v/v/v). Densitometric analysis of moxifloxacin was carried out in the absorbance mode at 298 nm. Compact spots for moxifloxacin were found at R(f) value of 0.58+/-0.02. The linear regression analysis data for the calibration plots showed good linear relationship with r=0.9925 in the working concentration range of 100-800 ng spot(-1). The method was validated for precision, accuracy, ruggedness, robustness, specificity, recovery, limit of detection (LOD) and limit of quantitation (LOQ). The LOD and LOQ were 3.90 and 11.83 ng spot(-1), respectively. Drug was subjected to acid and alkali hydrolysis, oxidation, dry heat, wet heat treatment and photodegradation. All the peaks of degradation products were well resolved from the standard drug with significantly different R(f) values. Statistical analysis proves that the developed HPTLC method is reproducible and selective. As the method could effectively separate the drug from its degradation products, it can be employed as stability-indicating one. Moreover, the proposed HPTLC method was utilized to investigate the kinetics of the acidic and alkaline degradation processes at different temperatures. Arrhenius plot was constructed and apparent pseudo-first-order rate constant, half-life and activation energy were calculated. In addition the pH-rate profile for degradation of moxifloxacin in constant ionic strength buffer solutions within the pH range 1.2-10.8 was studied. SN - 1873-4324 UR - https://www.unboundmedicine.com/medline/citation/17386477/Application_of_a_validated_stability_indicating_densitometric_thin_layer_chromatographic_method_to_stress_degradation_studies_on_moxifloxacin_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0003-2670(06)01829-0 DB - PRIME DP - Unbound Medicine ER -