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Development of characterization methods for entacapone in a pharmaceutical bulk
Nadejda Soukhova1, Zarema Kassymbek, Sanford Bradby
1Analytical Research and Development Laboratory, US Pharmacopeia, 12601 Twinbrook Parkway, Rockville, MD 20852, USA. ns@usp.org
Journal of Pharmaceutical and Biomedical Analysis
|November 30, 2010
Summary
A new high-performance liquid chromatography (HPLC) method accurately quantifies entacapone and its impurities in pharmaceutical bulk. This validated method ensures drug quality and stability through sensitive detection and reliable analysis.
Area of Science:
- Analytical Chemistry
- Pharmaceutical Analysis
- Chromatography
Background:
- Entacapone is a crucial pharmaceutical agent requiring robust analytical characterization.
- Ensuring the purity and accurate quantification of entacapone in bulk form is vital for drug safety and efficacy.
Purpose of the Study:
- To develop and validate a novel analytical method for entacapone characterization in pharmaceutical bulk.
- To establish procedures for the accurate assay and impurity determination of entacapone.
- To assess entacapone's stability and suitability for identification tests.
Main Methods:
- Development and validation of a reversed-phase HPLC method using a C18 column.
- Mobile phase: potassium phosphate buffer (pH 2.75, 30 mM)-methanol (50:50, v/v) at 1.0 mL/min.
- UV detection at 310 nm; supplemented with UV and FTIR spectroscopy for identification; water sorption analysis.
Main Results:
- The HPLC method demonstrated linearity from 50% to 150% of the assay concentration (0.2 mg/mL).
- Quantitation limit: 0.13 μg/mL; detection limit: 0.05 μg/mL; average recovery: 100.10% (RSD: 0.45%).
- Entacapone was well-resolved from degradation products; UV/FTIR spectra confirmed identity; no moisture effect observed.
Conclusions:
- The developed HPLC method is specific, sensitive, precise, linear, and accurate for entacapone analysis.
- UV and FTIR spectroscopy are suitable for entacapone identification.
- The validated methods provide reliable qualitative and quantitative analysis of entacapone in pharmaceutical bulk.
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