title: Validation of a stability-indicating RP-LC method for the determination of tigecycline in lyophilized powder.
abstract: A reversed-phase liquid chromatography (RP-LC) method was validated for the determination of tigecycline in lyophilized powder. The LC method was conducted on a Luna C18 column (250 × 4.6 mm i.d.), maintained at room temperature. The mobile phase consisted of buffer containing sodium phosphate monobasic (0.015M) and oxalic acid (0.015M) (pH 7.0)-acetonitrile (75:25, v/v), run at a flow rate of 1.0 mL/min and using ultraviolet detection at 280 nm. The chromatographic separation was obtained with a retention time of 8.6 min, and was linear in the range of 40-100 µg/mL (r(2) = 0.9997). The specificity and stability-indicating capability of the method was proven through forced degradation studies, which also showed no interference of the excipients. The accuracy was 99.01% with a bias lower than 1.81%. The limits of detection and quantitation were 1.67 and 5.05 µg/mL, respectively. Moreover, method validation demonstrated satisfactory results for precision and robustness. The proposed method was applied for the analysis of the lyophilized powder formulation, contributing to improve the quality control and to assure the therapeutic efficacy.
authors: Postgraduate Program in Pharmaceutical Sciences, Faculty of Pharmaceutical Sciences of Araraquara-UNESP, Araraquara-SP, Brazil. lucmsil@yahoo.com.br
authors: Lucélia Magalhães
authors: LM
authors: da Silva
authors: Hérida Regina Nunes
authors: HR
authors: Salgado
mesh_terms: D056148:Chromatography, Reverse-Phase / Q000379:methods*; D004355:Drug Stability; D057230:Limit of Detection; D016014:Linear Models; D008911:Minocycline / Q000031:analogs & derivatives* / Q000032:analysis / Q000737:chemistry / Q000592:standards; D011208:Powders / Q000737:chemistry / Q000592:standards; D015203:Reproducibility of Results; D000078304:Tigecycline
chemical_list: D011208:Powders; D000078304:Tigecycline; D008911:Minocycline