Development and Validation of a New LC Method for Analysis of Brimonidine Tartrate and Related Compounds

Madhavi, Alavala Siva; Naidu, A.; Rao, D. V. Subba; Srinivasu, P.

doi:10.1365/s10337-009-1083-2

Cited by 11 publications

(7 citation statements)

References 5 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%

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%

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 literature survey reveals several analytical methods for quantitative estimation of BRD in body fluids and in pharmaceutical formulations by spectrophotometry [4][5][6][7][8][9][10], liquid chromatography [11][12][13][14][15][16][17][18][19][20][21] and electrochemical methods [22][23][24].…”

Section: …………………………………………………………………………………………………… Introductionmentioning

confidence: 99%

Ion-Selective Membrane Sensors for Determination of Brimonidine Tartrate in Bulk Powder, Pharmaceutical Eyedrops and Biological Fluids.

Daabees¹,

Talaat²,

Shal³

et al. 2018

IJAR

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“…A literature survey revealed some analytical methods for the determination of BT, including electrochemical (3), spectrophotometric (4,5), HPTLC (6), high-performance liquid chromatography HPLC (7)(8)(9)(10)(11)(12)(13), ultra-performance LC-mass spectrometry (MS) (14) and LC-MS (15) methods. The chromatographic methods always require expensive solvents in addition to elaborate treatment; meanwhile the LC-MS instrument is not available in many laboratories.…”

Section: Introductionmentioning

confidence: 99%

Validated spectrofluorimetric and spectrophotometric methods for the determination of brimonidine tartrate in ophthalmic solutions via derivatization with NBD‐Cl. Application to stability study

et al. 2014

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Two simple, selective and accurate methods were developed and validated for the determination of brimonidine tartrate (BT) in pure state and pharmaceutical formulations. Both methods are based on the coupling of the drug with 4-chloro-7-nitro-2,1,3-benzoxadiazole in borate buffer (pH 8.5) at 70 °C and measurement of the reaction product spectrophotometrically at 407 nm (method I) or spectrofluorimetrically at 528 nm upon excitation at 460 nm (method II). The calibration graphs were rectilinear over the concentration ranges of 1.0-16.0 and 0.1-4.0 µg/mL with lower detection limits of 0.21 and 0.03, and lower quantification limits of 0.65 and 0.09 µg/mL for methods I and II, respectively. Both methods were successfully applied to the analysis of commercial ophthalmic solution with mean recovery of 99.50 ± 1.00 and 100.13 ± 0.71%, respectively. Statistical analysis of the results obtained by the proposed methods revealed good agreement with those obtained using a comparison method. The proposed spectrofluorimetric method was extended to a stability study of BT under different ICH-outlined conditions such as alkaline, acidic, oxidative and photolytic degradation. Furthermore, the kinetics of oxidative degradation of the drug was investigated and the apparent first-order reaction rate constants, half-life times and Arrhenius equation were estimated. The proposed methods are practical and valuable for routine applications in quality control laboratories for the analysis of BT.

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Development and Validation of a New LC Method for Analysis of Brimonidine Tartrate and Related Compounds

Cited by 11 publications

References 5 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

Ion-Selective Membrane Sensors for Determination of Brimonidine Tartrate in Bulk Powder, Pharmaceutical Eyedrops and Biological Fluids.

Validated spectrofluorimetric and spectrophotometric methods for the determination of brimonidine tartrate in ophthalmic solutions via derivatization with NBD‐Cl. Application to stability study

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