Stability-Indicating HPLC Method for Posaconazole Bulk Assay

Abstract

A stability-indicating liquid chromatographic (LC) method was developed for the determination of posaconazole in bulk. Chromatographic separation was achieved using an isocratic elution in a reversed-phase system, with a mobile phase composed of methanol-water (75:25, v/v), at 1.0 mL min−1 flow. Samples were exposed to degradation under thermal, oxidative and acid/basic conditions, and no interference in the analysis was observed. System suitability was evaluated and results were satisfactory (N = 4,900.00 tailing factor 1.04; RSD between injections = 0.65). The retention time of posaconazole was about 8.5 min and the method was validated within the concentration range 5–60 μg mL−1 (r = 0.9996). Adequate results were obtained for repeatability (RSD % = 0.86–1.22), inter-day precision (RSD % = 1.21) and accuracy (98.13% mean recovery). Robustness was also determined to be satisfactory after evaluation. The proposed method was successfully applied to posaconazole bulk quantification, showing the method is useful for determination of the drug in routine analysis.

A Comparative Study of Newly Developed HPLC-DAD and UHPLC-UV Assays for the Determination of Posaconazole in Bulk Powder and Suspension Dosage Form

“…The only HPLC-DAD method for the determination of PSZ in bulk powder reported elution time of 8.36 minutes [15]. As such our two methods show comparable retention/run times that fall on the lower range border.…”

“…Previous UHPLC methods for determination of PSZ in biological samples showed elution times ranging from 1.09 to 4.04 minutes [ 13 , 14 ], whereas previous HPLC methods reported elution times ranging from 9 to 19 minutes [ 19 , 21 – 24 ]. The only HPLC-DAD method for the determination of PSZ in bulk powder reported elution time of 8.36 minutes [ 15 ]. As such our two methods show comparable retention/run times that fall on the lower range border.…”

“…The only reported method for the determination of PSZ in bulk powder was an HPLC-DAD method using a C8 column and isocratically pumped mobile phase made of methanol : water (75 : 25), used only external standard quantitation method, had longer PSZ elution time and showed equivalent accuracy and precision [ 15 ].…”

“…Most of these methods are based on liquid chromatography using different types and detection modes such as HPLC with UV detection [ 4 – 6 ], HPLC with fluorescence detection [ 7 , 8 ], HPLC-tandem mass spectrometry (LC-MS/MS) [ 9 – 12 ], UPLC-UV detection [ 13 ], and UPLC-MS/MS [ 14 ]. Recently, HPLC with DAD detection was applied for the stability indicating determination of PSZ in bulk form [ 15 ]. Moreover, other separation techniques such as capillary electrophoresis [ 16 ] and micellar electrokinetic chromatography (MEKC) [ 17 ] were utilized for the quantification of PSZ in human plasma samples.…”

Hot Melt Extruded Amorphous Solid Dispersion of Posaconazole with Improved Bioavailability: Investigating Drug-Polymer Miscibility with Advanced Characterisation

“…Dissolution studies were performed as per USFDA reported method, in the 900 mL with 0.3% SLS medium (sodium lauryl sulphate) at 37 ± 0.2°C using a paddle USP type II apparatus (Electrolab DBK, Mumbai, India) at speed of 25 rpm. PCZ released from the SD and Noxafil was characterised by UV absorbance measurement at a wavelength of 262 nm [ 25 ].…”