title: Solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry for determination of trace rosiglitazone in urine.
abstract: This project evaluated solid-phase extraction (SPE) combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS) to determine the trace amount of rosiglitazone in human urine. The analytical performance of four modes of LC-MS and tandem MS operation (atmospheric pressure chemical ionization (APCI), electrospray ionization (ESI), positive and negative ionization) was compared for two mass spectrometers, a triple-quadrupole and a quadrupole ion trap instrument. Rosiglitazone was extracted from urine using a SPE cartridge of 50mg C8 sorbent and acetonitrile used as the eluting solvent. Samples were then separated on a RP18 column interfaced with a tandem mass spectrometer. The recovery of rosiglitazone was greater than 91.2%. The urine assay combining SPE and LC-APCI-MS/MS of triple-quadrupole was proved a very selective and sensitive method for determination of trace rosiglitazone. The assay was linear over a wide range, with a lower limit of quantification of 0.1 ng/mL using 1 mL of urine. The intra- and inter-day precisions were <9.8% and <7.9%, respectively, and the accuracies were in the range 91.0-103.6%. The rosiglitazone concentration profile in human urine was also determined. The results of this study reveal the adequacy of SPE-LC-APCI-MS/MS method for analyzing rosiglitazone from diabetic patients' urines. The concentrations of rosiglitazone were detected to range from 760 to 164 pg/mL.
authors.affiliation: Department of Chemistry, National Chung-Hsing University, 250 Kuo-Kuang Road, Taichung 40227, Taiwan.
authors.forename: Chi-Chi
authors.initials: CC
authors.lastname: Chou
authors.forename: Maw-Rong
authors.initials: MR
authors.lastname: Lee
authors.forename: Fu-Chou
authors.initials: FC
authors.lastname: Cheng
authors.forename: Dar-Yu
authors.initials: DY
authors.lastname: Yang
mesh_terms: D000284:Administration, Oral; D002623:Chemistry Techniques, Analytical / Q000295:instrumentation / Q000379:methods; D002853:Chromatography, Liquid / Q000379:methods*; D005260:Female; D006801:Humans; D007004:Hypoglycemic Agents / Q000008:administration & dosage / Q000652:urine; D015203:Reproducibility of Results; D000077154:Rosiglitazone; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D045162:Thiazolidinediones / Q000008:administration & dosage / Q000652:urine*; D013997:Time Factors
chemical_list: D007004:Hypoglycemic Agents; D045162:Thiazolidinediones; D000077154:Rosiglitazone