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Fractional factorial and central composite design for implementation of risk and DoE-based enhanced AQbD approach to eco-friendly HPTLC method for estimation of dalfampridine in pharmaceutical dosage forms and human plasma

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Abstract

Dalfampridine is a potassium channel blocker used for the improvement of motor function in patients with multiple sclerosis. Numerous analytical techniques have been published in the literature for estimation of dalfampridine but no report has been found in the literature for estimation of dalfampridine in pharmaceutical dosage forms and human plasma by the HPTLC method. Hence, an eco-friendly HPTLC method has been developed for the estimation of dalfampridine using risk and the DoE-based enhanced AQbD approach. The risk-based AQbD approach was applied by identification of method risk parameters followed by their risk assessment in method development by DoE-based FFD. The DoE-based AQbD approach was implemented for optimisation of high-risk method parameters by response surface methodology using CCD. The MODR and control strategy was framed for mitigation of risk of high-risk method parameters and low-risk life cycle management of developed method. The chromatogram was developed using silica gel G F254 as stationary phase and methanol–water-diethylamine (9.5:0.5:0.2, V/V) as mobile phase keeping saturation time of 10 min. The developed method was validated as per ICH Q2 (R1) guideline. The linearity range of the dalfampridine was found to be 200–1000 ng/band with a correlation coefficient of 0.995 both in bulk drug and human plasma. The % recovery of spiked standard from the pre-analysed sample was found to be in the range of 98–102%. The % recovery was found to be more than 80% from human plasma. The %RSD for all precision studies was found to be less than 2.0. The developed method was applied for the assay of pharmaceutical dosage forms, and results were found in compliance with the labelled claim. The developed method can be used as an eco-friendly alternative for routine bio-analysis and quality control of pharmaceutical dosage forms of dalfampridine in the pharmaceutical industry.

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Abbreviations

AQbD:

Analytical quality by design

FFD:

Fractional factorial design

CCD:

Central composite design

DFP:

Dalfampridine

MODR:

Method operable design ranges

IUPAC:

International Union for Pure and Applied Chemistry

ICH:

International Council for harmonization

DoE:

Design of experiments

RP-HPLC:

Reverse phase high-pressure liquid chromatography

HPTLC:

High-performance thin-layer chromatography

USFDA:

United state food and drug administration

UV:

Ultraviolet

API:

Active pharmaceutical ingredient

AR:

Analytical reagent

ANOVA:

Analysis of variance

BBD:

Box-Behnken design

TLC:

Thin-layer chromatography

LOD:

Limit of detection

LOQ:

Limit of quantitation

ATP:

Analytical target profile

CPAs:

Critical method performance attributes

%RSD:

% Relative standard deviation

Rf:

Retardation factor

TF:

Tailing factor

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Acknowledgements

The authors of the manuscript are thankful to the principal, Maliba Pharmacy College and the provost, Uka Tarsadia University for providing the necessary infrastructure and facilities to complete the research work.

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Authors and Affiliations

  1. Department of Quality Assurance, Maliba Pharmacy College, Uka Tarsadia University, Maliba Campus, Bardoli-Mahuva Road, Tarsadi, Mahuva, Surat, Gujarat, 394 350, India

    Pintu B. Prajapati, Urmi R. Patel & Shailesh A. Shah

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  1. Pintu B. Prajapati
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Correspondence to Pintu B. Prajapati.

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Prajapati, P.B., Patel, U.R. & Shah, S.A. Fractional factorial and central composite design for implementation of risk and DoE-based enhanced AQbD approach to eco-friendly HPTLC method for estimation of dalfampridine in pharmaceutical dosage forms and human plasma. J IRAN CHEM SOC 19, 2263–2277 (2022). https://doi.org/10.1007/s13738-021-02445-z

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