Rapid determination of total benzalkonium chloride content in ophthalmic formulation

Labranche, Louis-Philippe; Dumont, Suzanne N.; Levesque, Suzanne; Carrier, Alain

doi:10.1016/j.jpba.2006.09.022

Cited by 34 publications

(14 citation statements)

References 7 publications

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“…The flow rate was 1.0 ml/minute at column oven temperature 50°C. The wavelength was 208 nm and injection volumn was 20 µL [23]. The main objective of this work was the determination of BKC in azelastine hydrochloride ophthalmic solution by reverse phase high-performance liquid chromatographic (HPLC) method development, validation, and robustness.…”

Section: Gupta and Chaturvedimentioning

confidence: 99%

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A Study on Forced Degradation and Validation of Stability Indicating Rp-HPLC Method for Determination of Benzalkonium Chloride in Azelastine Hydrochoride Pharmaceutical Ophthalmic Formulation

Gupta

Chaturvedi

2017

Asian J Pharm Clin Res

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Objective: This study was designed to conduct forced degradation and validation studies for determination the benzalkonium chloride (BKC) as major homologues form in azelastine hydrochloride pharmaceutical ophthalmic formulation by a novel stability indicating reverse phase high-performance liquid chromatographic method (RP-HPLC).Methods: Forced degradation study and validation were carried out with a analytical approach of reverse phase chromatographic analysis with C18, cosmosil (250mm x 4.6mm i.d. x 5µm) column using mobile phase consisting acetonitrile -buffer of pH 5.0 with 5N NaOH (45:55 %v/v) at a flow rate of 1.5 ml per minute. Column temperature was maintained at 25°C and detection wavelength was 210nm.By using these chromatographic conditions of method, two major homologues of benzalkonium chloride were separated without any interference of drug components and exciepients.Results: Forced degradation studies were carried out as per ICH guidelines and established a stability indicating property of a method .The method was found linear in concentration range 40µg/ml to 60µg/ml (50µg/ml±20%), correlation coefficient was found 0.999. The recovery was found to be 99.2%, 100.7% and 101.4% at ±30% of target concentration. The %RSD for method precision and intermediate precision were found 0.28% and 0.30 % respectively. The method was found specific, selective, precise, accurate, linear, robust and stability indicating for quantification benzalkonium chloride in azelastine pharmaceutical ophthalmic formulation. Conclusion:The method has been found successful for determination of BKC pharmaceutical formulation and validated for all the parameters of validation and found within the acceptance criteria as per ICH guideline Q2R1.

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Section: Gupta and Chaturvedimentioning

confidence: 99%

“…A number of analytical methods have been reported for the estimation of BKC in various products including ophthalmic preparations [7][8][9][10][11][12][13][14][15][16][17][18][19][20][21][22][23]. However, there was no method available for estimation of BKC in azelastine hydrochloride ophthalmic formulations.…”

Section: Introductionmentioning

confidence: 99%

A Study on Forced Degradation and Validation of Stability Indicating Rp-HPLC Method for Determination of Benzalkonium Chloride in Azelastine Hydrochoride Pharmaceutical Ophthalmic Formulation

Gupta

Chaturvedi

2017

Asian J Pharm Clin Res

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“…benzalkonium chloride [9], ipratropium bromide [10], paraquat and diquat [11] and atracurium [12,13]). The presence of the quaternary nitrogen atom and an additional strongly basic amidino moiety, as in M&B4180A and its related compounds, makes separation by reversed-phase liquid chromatography (RP-LC) challenging as it can result in pronounced peak tailing due to secondary interactions with residual silanol groups on silica-based chromatographic columns [5,14].…”

Section: Introductionmentioning

confidence: 99%

Chromatographic retention behaviour, modelling and separation optimisation of the quaternary ammonium salt isometamidium chloride and related compounds on a range of reversed-phase liquid chromatographic stationary phases

Schad

Euerby²,

Skellern

et al. 2012

Anal Bioanal Chem

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This paper describes the reversed-phase liquid chromatographic behaviour of the trypanocidal quaternary ammonium salt isometamidium chloride and its related compounds on a range of liquid chromatographic phases possessing alkyl and phenyl ligands on the same inert silica. In a parallel study with various extended polar selectivity phases which possessed different hydrophobic/silanophilic (hydrogen bonding) activity ratios, the chromatographic retention/selectivities of the quaternary ammonium salts was shown to be due to a co-operative mechanism between hydrophobic and silanophilic interactions. The highly aromatic and planar isometamidium compounds were found to be substantially retained on stationary phases containing aromatic functionality via strong π-π interactions. The chemometric approach of principal component analysis was used to characterise the chromatographic behaviour of the isometamidium compounds on the differing phases and to help identify the dominant retention mechanism(s). Two-dimensional (temperature/gradient) retention modelling was employed to develop and optimise a rapid liquid chromatography method for the separation of the six quaternary ammonium salts within 2.5 min which would be suitable for bioanalysis using liquid chromatography-mass spectrometry. This is the first reported systematic study of the relationship between stationary phase chemistries and retention/selectivity for a group of quaternary ammonium salts.

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“…Although several compounds can be used as ophthalmic preservatives, benzalkonium chloride (BKC), a quaternary ammonium compound, is commonly used (Labranche et al, 2007) because of its high potency. Azithromycin ophthalmic drops were developed to treat ocular bacterial infections.…”

Section: Introductionmentioning

confidence: 99%

“…This type of column packing can be problematic with certain types of ophthalmic formulations. For example, formulations with sulfamide and sulfamide/morpholine as active ingredient and multiple excipients, when injected at high concentration, were not suitable for use with the CN stationary phase (Labranche et al, 2007).…”

Section: Introductionmentioning

confidence: 99%

Determination of benzalkonium chloride in viscous ophthalmic drops of azithromycin by high-performance liquid chromatography

Shen

Wang

et al. 2009

J. Zhejiang Univ. Sci. B

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Abstract:A high-performance liquid chromatography (HPLC) system was used in the reversed phase mode for the determination of benzalkonium chloride (BKC) in azithromycin viscous ophthalmic drops. A Venusil-XBP(L)-C 18 (150 mm×4.6 mm, 5 μm) column was used at 50 °C. The mobile phase consisted of a mixture of methanol-potassium phosphate (16:5, v/v). Two sample preparation methods were compared. The results suggested that, compared with an extraction procedure, a deproteinization procedure was much quicker and more convenient. Using the deproteinization procedure for sample preparation, calibration curves were linear in the range 5.0~50 μg/ml. The within-day and inter-day coefficients of variation were less than 10%. The average recoveries were determined as 96.70%, 98.52%, and 97.96% at concentrations of 10.0, 30.0, and 50.0 μg/ml, respectively. Variability in precision did not exceed 5%. In conclusion, this HPLC method using a simple sample treatment procedure appears suitable for monitoring BKC content in azithromycin viscous ophthalmic drops.

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Rapid determination of total benzalkonium chloride content in ophthalmic formulation

Cited by 34 publications

References 7 publications

A Study on Forced Degradation and Validation of Stability Indicating Rp-HPLC Method for Determination of Benzalkonium Chloride in Azelastine Hydrochoride Pharmaceutical Ophthalmic Formulation

A Study on Forced Degradation and Validation of Stability Indicating Rp-HPLC Method for Determination of Benzalkonium Chloride in Azelastine Hydrochoride Pharmaceutical Ophthalmic Formulation

Chromatographic retention behaviour, modelling and separation optimisation of the quaternary ammonium salt isometamidium chloride and related compounds on a range of reversed-phase liquid chromatographic stationary phases

Determination of benzalkonium chloride in viscous ophthalmic drops of azithromycin by high-performance liquid chromatography

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