title: Optimization and validation of a high performance liquid chromatography method for rapid determination of sinafloxacin, a novel fluoroquinolone in rat plasma using a fused-core C(18)-silica column.
abstract: A novel, simple and rapid high performance liquid chromatographic method has been developed and validated for the determination of sinafloxacin, a new fluoroquinolone, in rat plasma using 96-well protein precipitation, fused-core C(18)-silica column (4.6mmx50mm, 2.7microm) packed with a new solid support, which is made of 2.7microm particles that consist of a 1.7microm solid core covered with a 0.5microm thick shell of porous silica.The chromatographic separation was achieved with a mobile phase of 20:80 (v/v) of acetonitrile and phosphate buffer (pH=3.0) at a flow rate of 1mlmin(-1). Fluorescence detection was employed with lambda(ex) 295nm and lambda(em) 505nm. Lomefloxacin was used as internal standard (IS). The total analysis time was as short as 3min. The method was sensitive with a limit of detection (LOD) of 2ngml(-1), with good linearity (R(2)=0.9996) over the linear range of 5-500ngml(-1). The intra-day and inter-day precision was less than 5.8% and accuracy ranged from 100.3% to 103.5% for quality control (QC) samples at three concentrations of 10, 50 and 400ngml(-1).The fused-core C(18)-silica column method offered high sample throughput, low injection volume and low consumption of organic solvents. The method was successfully employed in the pharmacokinetic study of sinafloxacin formulation product after tail vein injection to healthy rats.
authors.affiliation: Department of Pharmaceutical Analysis, School of Pharmacy, Second Military Medical University, No.325 Guohe Road, Shanghai 200433, PR China.
authors.forename: Shuowen
authors.initials: S
authors.lastname: Wang
authors.forename: Jun
authors.initials: J
authors.lastname: Wen
authors.forename: Lijun
authors.initials: L
authors.lastname: Cui
authors.forename: Xiurong
authors.initials: X
authors.lastname: Zhang
authors.forename: Hua
authors.initials: H
authors.lastname: Wei
authors.forename: Rui
authors.initials: R
authors.lastname: Xie
authors.forename: Bo
authors.initials: B
authors.lastname: Feng
authors.forename: Yutian
authors.initials: Y
authors.lastname: Wu
authors.forename: Guorong
authors.initials: G
authors.lastname: Fan
mesh_terms: D000818:Animals; D000900:Anti-Bacterial Agents / Q000008:administration & dosage / Q000097:blood* / Q000493:pharmacokinetics; D002021:Buffers; D011232:Chemical Precipitation; D002851:Chromatography, High Pressure Liquid / Q000592:standards; D004355:Drug Stability; D005260:Female; D024841:Fluoroquinolones / Q000008:administration & dosage / Q000097:blood* / Q000493:pharmacokinetics; D006863:Hydrogen-Ion Concentration; D007275:Injections, Intravenous; D008297:Male; D051381:Rats; D017207:Rats, Sprague-Dawley; D012015:Reference Standards; D015203:Reproducibility of Results; D012822:Silicon Dioxide / Q000737:chemistry*
chemical_list: D000900:Anti-Bacterial Agents; D002021:Buffers; D024841:Fluoroquinolones; C547576:sinafloxacin; D012822:Silicon Dioxide