Versapharm Incorporated | Date: 2012-08-28
Srinivasu P.,Versapharm Incorporated |
Srinivasu P.,Sri Krishnadevaraya University |
SubbaRao D.V.,Versapharm Incorporated |
Vegesna R.V.K.,Versapharm Incorporated |
Sudhakar Babu K.,Sri Krishnadevaraya University
Journal of Pharmaceutical and Biomedical Analysis | Year: 2010
The objective of the current study was to develop a validated, specific and stability-indicating reverse phase liquid chromatographic method for the quantitative determination of acetazolamide and its related substances. The determination was done for an active pharmaceutical ingredient, its pharmaceutical dosage form in the presence of degradation products, and its process-related impurities. The drug was subjected to stress conditions of hydrolysis (acid and base), oxidation, photolysis and thermal degradation as per International Conference on Harmonization (ICH) prescribed stress conditions to show the stability-indicating power of the method. Significant degradation was observed during acid and base hydrolysis, and the major degradant was identified by LC-MS, FTIR and 1H/13C NMR spectral analysis. The chromatographic conditions were optimized using an impurity-spiked solution and the generated samples were used for forced degradation studies. In the developed HPLC method, the resolution between acetazolamide and, its process-related impurities (namely imp-1, imp-2, imp-3, imp-4 and its degradation products) was found to be greater than 2. The chromatographic separation was achieved on a C18, 250 mm × 4.6 mm, 5 μm column. The LC method employed a linear gradient elution, and the detection wavelength was set at 254 nm. The stress samples were assayed against a qualified reference standard and the mass balance was found to be close to 99.6%. The developed RP-LC method was validated with respect to linearity, accuracy, precision and robustness. © 2009 Elsevier B.V. All rights reserved.
Prabha S.,Versapharm Incorporated |
Prabha S.,Sri Krishnadevaraya University |
Vegesna R.V.K.,Versapharm Incorporated |
Sudhakarbabu K.,Sri Krishnadevaraya University
Current Pharmaceutical Analysis | Year: 2012
Chemical degradation of drugs often results in altered therapeutic efficacy and can lead to toxic side effects. A single, short and sensitive GC-ECD method for the quantification of degradation and process related impurities of lindane has been developed and validated in all of its pharmaceutical topical dosage forms (shampoo, cream and lotion). Three major degradants were observed during forced degradation (stress stability) studies of lindane dosage forms under various conditions recommended by International Conference on Harmonization (ICH). These were identified and confirmed by using both chemical ionization (CI) and electron ionization (EI) techniques of GC-MS analysis. One major degradation component was identified to be the same as the one that was enhanced during the accelerated and long term stability studies of the dosage forms. A dehydrohalogenation mechanism was proposed for this degradation process, which should considerably ease the pharmaceutical development of lindane dosage forms. The chromatographic conditions were optimized using an impurity-spiked solution and the samples that were generated from forced degradation studies. The best chromatographic separation was achieved on a USP-G27 column using electron capture detector (ECD). The newly developed GC-ECD method was validated with respect to linearity, accuracy, precision and robustness. The limit of detection for the lindane and its impurities were found to be 0.004,0.005,0.005 and 0.004μg/mL respectively. The accuracy (%recovery) was observed to be 100.0±3.0% for lindane and 100.0±5.0% for its impurities respectively in all-three dosage forms. The current method provides a significant improvement in monitoring stability, quality and therapeutic efficacy of lindane pharmaceutical dosage forms. © 2012 Bentham Science Publishers.
Versapharm Incorporated and Douglas Pharmaceuticals Ltd. | Date: 2000-08-29
PHARMACEUTICAL PREPARATIONS CONTAINING ISOTRETINOIN FOR THE TREATMENT OF ACNE AND OTHER SKIN CONDITIONS RESPONSIVE TO RETINOID THERAPY.
VersaPharm Incorporated | Date: 2002-07-02
Pharmaceutical preparations for the treatment of tuberculosis, hemophilia and other blood disorders; antibiotics; pharmaceutical preparations for the treatment of central nervous system disorders; nutritional supplements.