title: Liquid chromatography with electrospray ionization mass spectrometry method for the assay of glucosamine sulfate in human plasma: validation and application to a pharmacokinetic study.
abstract: A liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS) method was developed and validated for the assay of glucosamine sulfate in human plasma. Plasma proteins were precipitated by acetonitrile, followed by vortex mixing and centrifugation. The supernatant was transferred and derivatized with phenyl iso-thiocyanate in acetonitrile at 60 degrees C for 40 min. Chromatographic separation was performed on a C(18) column (Inertsil ODS-3 150 x 2.1 mm i.d., 5 microm, JP) with a mobile phase gradient consisting of 0.2% acetic acid (aqueous) and methanol at a flow-rate of 0.3 mL/min. MS detection using electrospray ionization (ESI) as an interface was used in single ion monitoring mode to determine positive ions at m/z 297. This method was shown to be selective and sensitive for glucosamine sulfate. The limit of detection was 35 ng/mL for glucosamine sulfate in plasma and the linear range was 0.1-20 microg/mL in plasma with a correlation coefficient (r) of 0.9991. The relative standard deviations (RSDs) of intra-day and inter-day assays were 8.7-11.4 and 9.8-12.6%, respectively. Extraction recoveries of glucosamine sulfate in plasma were greater than 73%. This method proved to be simple, reproducible and feasible for pharmacokinetic studies of glucosamine sulfate in healthy volunteers after a single oral administration (1500 mg). The pharmacokinetic parameters and relative bioavailabilities were investigated for both domestic glucosamine sulfate tablet and capsule preparations compared with an imported capsule product.
authors.affiliation: Department of Pharmaceutical Analysis, School of Pharmacy, Medical Center of Fudan University, Shanghai, People's Republic of China.
authors.forename: Tao-Min
authors.initials: TM
authors.lastname: Huang
authors.forename: Lei
authors.initials: L
authors.lastname: Cai
authors.forename: Bei
authors.initials: B
authors.lastname: Yang
authors.forename: Man-Xiang
authors.initials: MX
authors.lastname: Zhou
authors.forename: Yun-Fei
authors.initials: YF
authors.lastname: Shen
authors.forename: Geng-Li
authors.initials: GL
authors.lastname: Duan
mesh_terms: D019540:Area Under Curve; D002853:Chromatography, Liquid / Q000379:methods*; D005944:Glucosamine / Q000097:blood* / Q000493:pharmacokinetics; D006801:Humans; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*
chemical_list: D005944:Glucosamine