title: Simultaneous determination of rosiglitazone and its metabolites in rat liver microsomal fraction using hollow-fiber liquid-phase microextraction for sample preparation.
abstract: A three-phase hollow-fiber liquid-phase microextraction method for the analysis of rosiglitazone and its metabolites N-desmethyl rosiglitazone and ρ-hydroxy rosiglitazone in microsomal preparations is described for the first time. The drug and metabolites HPLC determination was carried out using an X-Terra RP-18 column, at 22°C. The mobile phase was composed of water, acetonitrile and acetic acid (85:15:0.5, v/v/v) and the detection was performed at 245 nm. The hollow-fiber liquid-phase microextraction procedure was optimized using multifactorial experiments and the following optimal condition was established: sample agitation at 1750 rpm, extraction for 30 min, hydrochloric acid 0.01 mol/L as acceptor phase, 1-octanol as organic phase, and donor phase pH adjustment to 8.0. The recovery rates, obtained by using 1 mL of microsomal preparation, were 47-70%. The method presented LOQs of 50 ng/mL and it was linear over the concentration range of 50-6000 ng/mL, with correlation coefficients (r) higher than 0.9960, for all analytes. The validated method was employed to study the in vitro biotransformation of rosiglitazone using rat liver microsomal fraction.
authors: Department of Physics and Chemistry, Faculty of Pharmaceutical Sciences of Ribeirão Preto, University of São Paulo, Ribeirão Preto, São Paulo, Brazil.
authors: Leandro Augusto
authors: LA
authors: Calixto
authors: Pierina Sueli
authors: PS
authors: Bonato
mesh_terms: D000818:Animals; D001711:Biotransformation; D005591:Chemical Fractionation / Q000295:instrumentation / Q000379:methods*; D002853:Chromatography, Liquid / Q000295:instrumentation / Q000379:methods*; D007004:Hypoglycemic Agents / Q000737:chemistry / Q000378:metabolism; D008110:Liver Extracts / Q000032:analysis*; D008297:Male; D008862:Microsomes, Liver / Q000737:chemistry*; D051381:Rats; D017208:Rats, Wistar; D015203:Reproducibility of Results; D000077154:Rosiglitazone; D012680:Sensitivity and Specificity; D012997:Solvents / Q000737:chemistry; D045162:Thiazolidinediones / Q000737:chemistry / Q000378:metabolism
chemical_list: D007004:Hypoglycemic Agents; D008110:Liver Extracts; D012997:Solvents; D045162:Thiazolidinediones; D000077154:Rosiglitazone