A validated stability-indicating LC method for acetazolamide in the presence of degradation products and its process-related impurities

Srinivasu, P.; SubbaRao, Devarakonda V.; Vegesna, Raju V. K.; Babu, K. Sudhakar

doi:10.1016/j.jpba.2009.12.011

Cited by 18 publications

(8 citation statements)

References 12 publications

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“…The specificity of the developed LC method for fluocinonide was determined in the presence of its impurities (namely imp-1, imp-2, imp-3, imp-4, imp-5, imp-6, imp-7 and imp-8) and degradation products. Forced degradation studies were also performed on fluocinonide to provide an indication of the stability-indicating property and specificity of the proposed method [7][8][9][10][11][12]. The stress conditions employed for the degradation study included light (carried out as per ICH Q1B), heat (60°C), acid hydrolysis (1M HCl), base hydrolysis (0.1M NaOH) and oxidation (5% H 2 O 2 ).…”

Section: Stress Studies/specificitymentioning

confidence: 99%

“…The developed LC method was validated with respect to specificity, LOD, LOQ, linearity, precision, accuracy and robustness. Forced degradation studies were performed on the drug substance and drug products to show the stability-indicating nature of the method [7][8][9][10][11][12][13]. These studies were performed in accordance with established ICH guidelines [14][15].…”

Section: Introductionmentioning

confidence: 99%

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A Validated Stability-Indicating LC Method for Fluocinonide in the Presence of Degradation Products, Its Process-Related Impurities and Identification of Degradation Products

Srinivasu¹,

SubbaRao²,

Vegesna³

et al. 2010

AJAC

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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 fluocinonide and its related substances. The determination was done for active pharmaceutical ingredient and its pharmaceutical dosage forms 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 per International Conference on Harmonization (ICH) prescribed stress conditions to show the stability-indicating power of the method. Significant degradation was observed during acid, base hydrolysis, and peroxide degradation. The major degradants were identified by LC-MS, FTIR and 1 H/ 13 C NMR spectral analysis. The chromatographic conditions were optimized using an impurity-spiked solution and the samples generated from forced degradation studies. In the developed HPLC method, the resolution between fluocinonide and its process-related impurities, (namely imp-1, imp-2, imp-3, imp-4, imp-5, imp-6, imp-7 and imp-8) and its degradation products was found to be greater than 2.0. 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 240 nm. The stress samples were assayed against a qualified reference standard and the mass balance was found to be close to 99.3%. The developed RP-LC method was validated with respect to linearity, accuracy, precision and robustness.

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Section: Stress Studies/specificitymentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

A Validated Stability-Indicating LC Method for Fluocinonide in the Presence of Degradation Products, Its Process-Related Impurities and Identification of Degradation Products

Srinivasu¹,

SubbaRao²,

Vegesna³

et al. 2010

AJAC

Self Cite

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“…Presently, only few analytical methods 9 , 10 , 11 , 12 , 13 , 14 , 15 , 16 , 17 , 18 for the detection of CAIs in biological samples have been published in the international literature and none of them simultaneously determined the three main CAIs (dorzolamide, brinzolamide, and acetazolamide) and/or their metabolites.…”

Section: Introductionmentioning

confidence: 99%

Development and validation of a fast ultra‐high‐performance liquid chromatography tandem mass spectrometry method for determining carbonic anhydrase inhibitors and their metabolites in urine and hair

Faro

Tini

Gottardi³

et al. 2021

Drug Testing and Analysis

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A new, rapid, sensitive, and comprehensive ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method for quantifying diuretics (acetazolamide, brinzolamide, dorzolamide, and their metabolites) in human urine and hair was developed and fully validated. Twenty-five milligrams of hair were incubated with 500-μl M3 ® buffer reagent at 100 C for 1 h for complete digestion. After cooling, 1-μl supernatant was injected onto chromatography system. Urine samples were simply diluted before injection. The chromatographic run time was short (8 min) through a column with a mobile phase gradient. The method was linear (determination coefficients always higher than 0.99) from limit of quantification (LOQ) to 500 ng/ml in urine and from LOQ to 10 ng/mg in hair. LOQs ranged from 0.07 to 1.16 ng/ml in urine and from 0.02 to 0.15 ng/mg in hair. No significant ion suppression due to matrix effect was observed, and process efficiency was always higher than 80%. Intra-and inter-assay precision was lower than 15%. The suitability of the methods was tested with six urine and hair specimens from patients treated with acetazolamide, dorzolamide, or brinzolamide for ocular diseases or systemic hypertension. Average urine concentrations were 266.32 ng/ml for dorzolamide and 47.61 ng/ml for N-deethyl-dorzolamide (n = 3), 109.27 ng/ml for brinzolamide and 1.02 ng/ml for O-desmethyl-brinzolamide (n = 2), and finally, 12.63 ng/ml for acetazolamide. Average hair concentrations were 5.94 ng/mg for dorzolamide and 0.048 ng/mg for N-deethyl-dorzolamide (n = 3), 3.26 ng/mg for brinzolamide (n = 2), and 2.3 ng/mg for acetazolamide (n = 1). The developed method was simple and fast both in the extraction procedures making it eligible in high-throughput analysis for clinical forensic and doping purposes.

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“…Acetazolamide a carbonic anhydrase inhibitor, which is used primarily to reduce intraocular pressure by decreasing aqueous humor formation, therapeutically for treatment of glaucoma, epilepsy and as a diuretic and has been used clinically since 1954 [1][2][3][4] . Acetazolamide in either medicinal forms or biological fluids were estimated in several techniques and methods have been declared in the literature, including HPLC for the quantification of acetazolamide in human and rat plasma [5][6][7] , LC/MS and GC/MS [8][9][10] , LC-UV [11][12][13] , and spectrophotometry for determination acetazolamide and other sulfonamide drugs [14][15][16][17][18][19] .…”

Section: Introductionmentioning

confidence: 99%

Novel approach and Cloud Point Extraction Method for Determination of Acetazolamide Drug

2020

IJFMT

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Acetazolamide was hydrolyzed to primary aromatic amine by using (0.4) M NaOH under reflux. The product was evaluated by two a ways. The first way, Diazotization coupling reaction (approach) as simple, sensitive, rapid and selective Spectrophotometric method, using 8-hydroxyquinoline as Chromogenic reagent to give Azo dye (red) in basic medium. The second way involves applying Cloud point extraction, using Triton-x 114 as surfactant. The Azo dye was diagnosed by FT-IR, 1 HNMR and UV-Visible technique. The analytical data for Approach and Cloud point extraction method, involve concentration rang (5-150), (0.5-6) µg.mL -1 , molar absorptivity (2.3×10 3 ), (1.3×10 4 ) L.mol -1. cm -1 , Sandall's sensitivity (0.096) µg.cm -2 (0.017) µg.cm -2 and detection limits (0.952) µg.mL -1 and (0.043) µg.mL -1 respectively. In addition the measurement enrichment factor (100) and preconcentration factor (6.30), The proposed methods don't affect by the existence of excipients so the methods were applied successfully in determining Acetazolamide in pharmaceutical preparations.

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A validated stability-indicating LC method for acetazolamide in the presence of degradation products and its process-related impurities

Cited by 18 publications

References 12 publications

A Validated Stability-Indicating LC Method for Fluocinonide in the Presence of Degradation Products, Its Process-Related Impurities and Identification of Degradation Products

A Validated Stability-Indicating LC Method for Fluocinonide in the Presence of Degradation Products, Its Process-Related Impurities and Identification of Degradation Products

Development and validation of a fast ultra‐high‐performance liquid chromatography tandem mass spectrometry method for determining carbonic anhydrase inhibitors and their metabolites in urine and hair

Novel approach and Cloud Point Extraction Method for Determination of Acetazolamide Drug

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