Determination of the active metabolite of prulifloxacin in human plasma by liquid chromatography-tandem mass spectrometry.
A liquid chromatographic-tandem mass spectrometric method (LC-MS/MS) for the determination of ulifloxacin, the active metabolite of prulifloxacin, in human plasma is described. After sample preparation by protein precipitation with methanol, ulifloxacin and ofloxacin (internal standard) were chromatographically separated on a C(18) column using a mobile phase consisting of methanol, water and formic acid (70:30:0.2, v/v/v) at a flow rate of 0.5 ml/min and then were detected using MS/MS by monitoring their precursor-to-product ion transitions, m/z 350-->m/z 248 for ulifloxacin and m/z 362-->m/z 261 for ofloxacin, in selected reaction monitoring (SRM) mode. Positive electrospray ionization was used for the ionization process. The linear range was 0.025-5.0 microg/ml for ulifloxacin with a lower limit of quantitation of 0.025 microg/ml. Within- and between-run precision was less than 6.6 and 7.8%, respectively, and accuracy was within 2.0%. The recovery ranged from 92.1 to 98.2% at the concentrations of 0.025, 0.50 and 5.0 microg/ml. Compared with the reported LC method, the present LC-MS/MS method can directly determine the ulifloxacin in human plasma without any need of derivatization. The present method has been successfully used for the pharmacokinetic studies of a prulifloxacin formulation product after oral administration to healthy volunteers.
Department of Analytical Chemistry, School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, China.
Lixia
L
Guo
Meiling
M
Qi
Xin
X
Jin
Peng
P
Wang
Huaiqing
H
Zhao
D000900:Anti-Bacterial Agents / Q000097:blood* / Q000493:pharmacokinetics; D002138:Calibration; D002853:Chromatography, Liquid / Q000379:methods*; D004148:Dioxolanes / Q000097:blood* / Q000493:pharmacokinetics; D024841:Fluoroquinolones / Q000097:blood* / Q000493:pharmacokinetics; D006801:Humans; D010879:Piperazines / Q000097:blood* / Q000493:pharmacokinetics; D015363:Quinolones / Q000097:blood* / Q000493:pharmacokinetics; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*
D000900:Anti-Bacterial Agents; D004148:Dioxolanes; D024841:Fluoroquinolones; D010879:Piperazines; D015363:Quinolones; C074191:prulifloxacin