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机构地区:[1]山东大学药学院,山东济南250012 [2]山东大学第二医院,山东济南250033
出 处:《齐鲁药事》2007年第4期214-217,共4页qilu pharmaceutical affairs
摘 要:目的建立测定人血浆中氟罗沙星浓度的高效液相色谱方法,并用于其药代动力学研究。方法采用加替沙星为内标,血浆样品经甲醇沉淀蛋白后直接进样。色谱柱为Diamonsil C18柱,流动相为1%三乙胺-磷酸缓冲液(pH4.8)/乙腈(80/20,V/V),流速1.0mL·min^-1。采用荧光检测器,激发波长290nm,发射波长458nm。结果氟罗沙星血浆浓度0.025~8.00μg·L^-1范围内线性关系良好(W=1/x,r=0.9999),低、中、高浓度质控样品的日内、日间精密度不超过5.16%,方法精密度99.1%~100.9%,提取回收率86.7%~92.0%。氟罗沙星血浆样品实验条件下均稳定。结论该方法灵敏度高,定量准确,适用于氟罗沙星人体药代动力学研究。OBJECTIVE To develop a sensitive and accurate HPLC method for the determination of fleroxacin in human plasma,and study its pharmacokinetics in healthy subjects. METHODS Gatifloxacin was used as internal standard. The analytes were isolated from plasma by simple protein precipitation with methanol,separated on a Diamonsil C18 column by isocratic elution with the mobile phase composed of 1% triethylamine-phosphate buffer (adjusted to p H 4. 8) and acetonitrile (80/20, V/V) at a flow rate of 1.0mL · min^-1 ,and analyzed by fluorescence detection with an excitation and emission wavelength of 290 nm and 458 nm,respectively. RESULTS The weighted (1/x) calibration curve was linear over the plasma concentration range of 0. 025-8. 00 (g · mL^-1 ,with a correlation coefficient ( r ) of 0. 9999. The inter- and intra-day precisions ( RSD/%) of the method were no more than 5.16 %,and the method accuracies and extraction recoveries at three concentrations ranged form 99. 1 to 100.9% and 86.7 to 92. 0% ,respectively. Fleroxacin in plasma was stable Under all conditions tested. The devel- oped method was successfully applied to the pharmacokinetic study of fleroxacin in healthy subjects. CONCLUSION The method is sensitive and accurate,and proved to be suitable for human pharmacokinetic study of fleroxacin.
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