Authors :
Piyusha Nejdar; Sujeet Salunkhe; Sachin Pishawikar
Volume/Issue :
Volume 8 - 2023, Issue 6 - June
Google Scholar :
https://bit.ly/3TmGbDi
Scribd :
https://tinyurl.com/54baumjw
DOI :
https://doi.org/10.5281/zenodo.8133710
Abstract :
Sibutramine, {1-[1-(4-chlorophenyl)
cyclobutyl]-3-methylbutyl} dethylamine is potent
serotonin and norepinephrine inhibitor.
Pharmacologically it acts as antihypertensive and anti-
obesity agent via its secondary (M1) and primary (M2)
amine metabolites. In present work an attempt has been
done to develop a simple, rapid, precise and accurate
isocratic reversed-phase HPLC method for the
determination of sibutramine. As a novelty along with
validation of developed method as per ICH guidelines, a
QbD approach has been applied. As critical quality
attributes related to analytical method have been
identified and optimized more robustness and accurate
method HPLC method has been developed. Slection of
column, composition of mobile phase and flow rate were
identified as critical quality attributes where by selection
of KYA TECH HIQ Sil C18 (4.6 mm × 250 mm) 5μm
column, Acetonitrile: water in composition 80:20 v/v as
mobile phase with flow rate 1mL/min was done. The λmax
was detected as 239 nm. The linearity range of the
proposed method was found to be in the range of 10–50
μg/ml (r = 0.999). The limits of detection was 0.081 μg/ml
and the limits of quantitation were 0.172 μg/ml
respectively.
Keywords :
Sibutramine, Quality by Design (QbD), Analytical Method Development and Validation. RP-HPLC.
Sibutramine, {1-[1-(4-chlorophenyl)
cyclobutyl]-3-methylbutyl} dethylamine is potent
serotonin and norepinephrine inhibitor.
Pharmacologically it acts as antihypertensive and anti-
obesity agent via its secondary (M1) and primary (M2)
amine metabolites. In present work an attempt has been
done to develop a simple, rapid, precise and accurate
isocratic reversed-phase HPLC method for the
determination of sibutramine. As a novelty along with
validation of developed method as per ICH guidelines, a
QbD approach has been applied. As critical quality
attributes related to analytical method have been
identified and optimized more robustness and accurate
method HPLC method has been developed. Slection of
column, composition of mobile phase and flow rate were
identified as critical quality attributes where by selection
of KYA TECH HIQ Sil C18 (4.6 mm × 250 mm) 5μm
column, Acetonitrile: water in composition 80:20 v/v as
mobile phase with flow rate 1mL/min was done. The λmax
was detected as 239 nm. The linearity range of the
proposed method was found to be in the range of 10–50
μg/ml (r = 0.999). The limits of detection was 0.081 μg/ml
and the limits of quantitation were 0.172 μg/ml
respectively.
Keywords :
Sibutramine, Quality by Design (QbD), Analytical Method Development and Validation. RP-HPLC.
