title: A validated spectrophotometric and liquid chromatography method for determination and purity evaluation of 4-methoxy-2-[2-hydroxy-3(4-phenyl-1-piperazinyl)]propyl-2,3-dihydro-6-methyl-1,3-dioxo-1H-pyrrolo[3,4-c]pyridine.
abstract: A spectrophotometric analysis of the UV-spectrum of 4-methoxy-2-[2-hydroxy-3(4-phenyl-1-piperazinyl)]propyl-2,3-dihydro-6-methyl-1,3-dioxo-1H-pyrrolo[3,4-c]pyridine (I) in 0.01 M HCl was performed by determining the values of specific absorption coefficients at the following analytical wavelengths: 224, 285 and 348 nm. The separation by means of TLC of compound I and of its five decomposition products was also studied. Silica gel coated plates (60 F(254)) were used and the mobile phase was consisted of butanol-acetic acid (1.05 kg/l)-water (80:12:30, v/v/v). The HPLC method (LiChrosorb(R) 100 RP-18 column 250 x 4.0 mm I.D., dp=5 microm; mobile phase: acetonitrile-0.01 M phosphate buffer (H(3)PO(4)+KH(2)PO(4); pH 3) (50:50, v/v-phase A) or (30:70, v/v-phase B) was validated by determination of the following parameters: selectivity, precision, linearity, stability of the analite and LOD as well as LOQ. Kinetic studies of the decomposition process of I in both acidic and alkaline environments indicate instability of the imide group.
authors.affiliation: Department of Pharmaceutical Chemistry, K Marcinkowski University of Medical Sciences, Grunwaldzka 6, 60-780 Poznań, Poland. imuszals@am.poznan.pl
authors.forename: Izabela
authors.initials: I
authors.lastname: Muszalska
authors.forename: Helena
authors.initials: H
authors.lastname: Sadowska
authors.forename: Dominika
authors.initials: D
authors.lastname: Szkatula
mesh_terms: D000700:Analgesics / Q000302:isolation & purification*; D019086:Bridged Bicyclo Compounds, Heterocyclic / Q000302:isolation & purification*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D002855:Chromatography, Thin Layer / Q000379:methods*; D004355:Drug Stability; D013058:Mass Spectrometry / Q000379:methods*; D011725:Pyridines / Q000302:isolation & purification*; D011809:Quinones / Q000302:isolation & purification*; D013053:Spectrophotometry / Q000379:methods*
chemical_list: C478822:4-methoxy-2-(2-hydroxy-3-(4-phenyl-1-piperazinyl))propyl-2,3-dihydro-6-methyl-1,3-dioxo-1H-pyrrolo(3,4-c)pyridine; D000700:Analgesics; D019086:Bridged Bicyclo Compounds, Heterocyclic; D011725:Pyridines; D011809:Quinones