HPLC method development for fampridine using Analytical Quality by Design approach

Abstract

Offering a systematic and multivariate analysis of the analytical procedure, development and validation of HPLC methods using Quality by Design approach are in the limelight of current research trends. A new, experimental design-aided HPLC method for fampridine was developed and preliminarily validated according to current in-force international guidelines for linearity, accuracy, robustness and precision.The method offers a high throughput sample analysis, with an elution time of 2.9 minutes, and signal detection without excipient interference performed at 262 nm. The method proved to be linear between 1–15 µg mL−1 (R2= 0.9996). The mean recovery was found to be 98.7 ± 1.9 % in the tested range of 2.5–7.5 µg mL−1. Low RSD values (< 1 %) were obtained for both model, intra- and inter-day precision. The limit of detection and limit of quantification were 0.24 and 0.78 µg mL−1, resp. The method proved to be applicable for active substance assay in a pharmaceutical dosage form.

Enantioseparation of solriamfetol and its major impurity phenylalaninol by capillary electrophoresis using sulfated gamma cyclodextrin

“…In the latter case, low model validity was observed, which was due to the high reproducibility of replicate runs and thus, low pure error inside the models. Similar observations were described during several chromatographic method optimizations [26][27][28].…”

Development and validation of stability-indicating RP-HPLC method for estimation of dalfampridine in bulk drug and tablet dosage form

“…Few methods like UV [12][13][14] spectroscopy and RP-HPLC [15][16][17][18][19] were reported for the estimation of dalfampridine. In the present method, dalfampridine was eluted at 4.5 min with a run time of 10 min.…”

Quality-by-design in pharmaceutical development: From current perspectives to practical applications

“…Numerous reverse phase HPLC methods optimized using AQbD are published, but there are several using gradient HILIC (hydrophilic interaction chromato graphy) methods as well (53). Using isocratic HPLC methods, the most frequent CMPs are the aforementioned input variables (54,55).…”

“…Similarly, we previously developed an RP-HPLC method for the quantification of fampridine from the solid oral dosage form by applying a full factorial experimental design (55). A MODR was achieved in terms of flow rate, column temperature and buffer proportion in the mobile phase, for chromatographic system CQAs (retention time, theoretical plate number and tailing factor).…”