title: A Validated TLC-Densitometric Method for the Determination of Mesterolone in Bulk Material and in Tablets.
abstract: Mesterolone is a synthetic androgenic steroid indicating a weak anabolic activity. A new, simple in use, and economical TLC-densitometric method in normal phase system (NP-TLC) has been developed and validated for the identification and quantitative determination of mesterolone in bulk drug and in tablet formulation. NP-TLC analysis was performed on aluminium plates precoated with silica gel 60F254 as the stationary phase using chloroform-acetone (40 : 10, v/v) as mobile phase. Densitometric analysis was carried out at λ = 745 nm after staining with phosphomolybdic acid. These conditions were found to give visible (dark blue) spot and sharp peak, respectively, for mesterolone at R F 0.75 ± 0.02 and enabled satisfactory separation of mesterolone from its related substance (potential impurity). The proposed NP-TLC-densitometric method was validated for specificity, linearity, precision, accuracy, robustness, and sensitivity according to ICH guideline and other validation requirements. The limit of detection (LOD) and limit of quantification (LOQ) were 61.0 ng · spot(-1) and 184.0 ng · spot(-1), respectively. The percent content of mesterolone in marketed tablet formulation was found to be 99.40% of label claim. The developed TLC-densitometric method can be successfully used in quality control of mesterolone in bulk material and also tablet formulation.
authors.affiliation: Department of Analytical Chemistry, School of Pharmacy and the Division of Laboratory Medicine, Medical University of Silesia in Katowice, 4 Jagiellońska, 41-200 Sosnowiec, Poland.
authors.forename: Małgorzata
authors.initials: M
authors.lastname: Dołowy
authors.affiliation: Department of Analytical Chemistry, School of Pharmacy and the Division of Laboratory Medicine, Medical University of Silesia in Katowice, 4 Jagiellońska, 41-200 Sosnowiec, Poland.
authors.forename: Alina
authors.initials: A
authors.lastname: Pyka-Pająk
authors.affiliation: R&D Analytical Chemistry Department, Pharmaceutical Research Institute, 8 Rydygiera, 01-793 Warsaw, Poland.
authors.forename: Katarzyna
authors.initials: K
authors.lastname: Filip
authors.affiliation: R&D Analytical Chemistry Department, Pharmaceutical Research Institute, 8 Rydygiera, 01-793 Warsaw, Poland.
authors.forename: Joanna
authors.initials: J
authors.lastname: Zagrodzka
mesh_terms: D003720:Densitometry / Q000379:methods*; D008655:Mesterolone / Q000032:analysis*; D013607:Tablets
chemical_list: D013607:Tablets; D008655:Mesterolone