کد مقاله | کد نشریه | سال انتشار | مقاله انگلیسی | نسخه تمام متن |
---|---|---|---|---|
1201169 | 1493513 | 2015 | 11 صفحه PDF | دانلود رایگان |
• UHPLC method for the assay for benzalkonium chloride in preserved drug formulations.
• A Quality-by-Design (QbD) approach used for the method development.
• QbD approach assured minimal risk of method failure during validation and routine use.
• Method is >10 times faster and >80 times more sensitive than US pharmacopeia method.
• Validation confirmed method is precise, accurate and linear for preserved drug formulations.
A rapid robust reversed-phase UHPLC method has been developed for the analysis of total benzalkonium chloride in preserved drug formulation. A systematic Quality-by-Design (QbD) method development approach using commercial, off the shelf software (Fusion AE®) has been used to optimize the column, mobile phases, gradient time, and other HPLC conditions. Total benzalkonium chloride analysis involves simple sample preparation. The method uses gradient elution from an ACE Excel 2 C18-AR column (50 mm × 2.1 mm, 2.0 μm particle size), ammonium phosphate buffer (pH 3.3; 10 mM) as aqueous mobile phase and methanol/acetonitrile (85/15, v/v) as the organic mobile phase with UV detection at 214 nm. Using these conditions, major homologs of the benzalkonium chloride (C12 and C14) have been separated in less than 2.0 min. The validation results confirmed that the method is precise, accurate and linear at concentrations ranging from 0.025 mg/mL to 0.075 mg/mL for total benzalkonium chloride. The recoveries ranged from 99% to 103% at concentrations from 0.025 mg/mL to 0.075 mg/mL for total benzalkonium chloride. The validation results also confirmed the robustness of the method as predicted by Fusion AE®.
Journal: Journal of Chromatography A - Volume 1413, 25 September 2015, Pages 22–32