Department of Pharmacy, Urumqi General Hospital of PLA, Urumqi, Xinjiang 830000, China.
Anal Bioanal Chem. 2012 Jun;403(7):1951-60. doi: 10.1007/s00216-012-6013-8. Epub 2012 May 5.
In this work, a new sample-preparation method based on hollow-fiber liquid-phase microextraction (HF-LPME) was developed for analysis of magnoflorine in rat plasma. Analysis was accomplished by reversed-phase high-performance liquid chromatography (HPLC), with ultraviolet detection by use of a photodiode-array detector. An orthogonal array design (OAD) was found to be effective for optimization of major conditions which may affect the efficiency of HF-LPME. Under the optimized conditions (pH of donor and acceptor phases 12 and 2.0, respectively; extraction time 20 min; stirring speed 800 rpm; and addition of 10 % (w/v) salt), the preconcentration factor for magnoflorine was 355. Calibration curves with reasonable linearity (r(2)≥0.9994) were obtained in the range 10-1000 ng mL(-1). Intra-day and inter-day precision (RSD) were <5.5 % and the limit of detection (LOD) for the analyte was 3.0 ng mL(-1) (S/N=3). The validated method was successfully used for pharmacokinetic studies of magnoflorine in rat plasma after intravenous administration.
本工作建立了一种基于中空纤维液相微萃取（HF-LPME）的新型样品前处理方法，用于大鼠血浆中美防己碱的分析。采用反相高效液相色谱（HPLC）法，紫外检测，二极管阵列检测器检测。正交试验设计（OAD）被发现可有效优化可能影响 HF-LPME 效率的主要条件。在优化条件下（供体相和受体相的 pH 值分别为 12 和 2.0；萃取时间 20 min；搅拌速度 800 rpm；添加 10%（w/v）盐），美防己碱的预浓缩因子为 355。在 10-1000 ng mL(-1)范围内，获得了具有合理线性（r(2)≥0.9994）的校准曲线。日内和日间精密度（RSD）均<5.5%，分析物的检测限（LOD）为 3.0 ng mL(-1)（S/N=3）。该验证方法成功用于大鼠静脉注射美防己碱后的药代动力学研究。
