title: Optimization of on-line solid phase extraction and HPLC conditions using response surface methodology for determination of WM-5 in mouse plasma and its application to pharmacokinetic study.
abstract: Response surface methodology (RSM) was utilized for rapid and systematic optimization of on-line solid-phase extraction (SPE) parameters to maximize the response and separation of WM-5. The optimization was performed with Box-Behnken designs. Four major parameters were investigated for their contributions to the response and separation of WM-5, with a total of 29 experiments being performed for each instrument, respectively. Quantitative determination of WM-5 in mouse plasma was performed to evaluate the statistical significance of the parameters on chromatographic response. A fully automated on-line SPE and high-performance liquid chromatography (HPLC) with diode array detection (DAD) method was developed for the determination of WM-5 in mouse plasma. Calibration curve with good linearity (r=0.9989) was obtained in the range of 20-4000 ng/mL in mouse plasma. The limit of detection (LOD) and lower limit of quantification (LLOQ) of the assay were 6 ng/mL and 20 ng/mL, respectively. The overall intra-day and the inter-day variations were less than 1.90%. The recovery of the method was in the range of 93.74-96.33% with RSD less than 3.06%. The optimized method demonstrated good performance in terms of specificity, LLOQ, linearity, recovery, precision and accuracy, and was successfully applied to quantify WM-5 in mouse plasma to support the pharmacokinetic study.
authors: College of Pharmacy and State Key Laboratory of Elemento-Organic Chemistry, Nankai University, Tianjin 300071, PR China.
authors: Lei
authors: L
authors: Liu
authors: Ya-Bin
authors: YB
authors: Wen
authors: Kang-Ning
authors: KN
authors: Liu
authors: Liang
authors: L
authors: Sun
authors: Meng
authors: M
authors: Wu
authors: Gui-Fang
authors: GF
authors: Han
authors: Ya-Xin
authors: YX
authors: Lu
authors: Qing-Ming
authors: QM
authors: Wang
authors: Zheng
authors: Z
authors: Yin
mesh_terms: D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D002939:Ciprofloxacin / Q000031:analogs & derivatives* / Q000097:blood / Q000737:chemistry / Q000302:isolation & purification / Q000493:pharmacokinetics; D004355:Drug Stability; D007546:Isoquinolines / Q000097:blood* / Q000737:chemistry / Q000302:isolation & purification / Q000493:pharmacokinetics; D057230:Limit of Detection; D016014:Linear Models; D008297:Male; D051379:Mice; D015233:Models, Statistical; D011758:Pyrroles; D015203:Reproducibility of Results; D052616:Solid Phase Extraction / Q000379:methods*
chemical_list: D007546:Isoquinolines; D011758:Pyrroles; C486449:WM5 compound; D002939:Ciprofloxacin