固相萃取-高效液相色谱法测定兔血清中环丙沙星的浓度

Determination of Ciprofloxacin Concentration in Rabbit Serum by SPE-HPLC

目的:建立以固相萃取-高效液相色谱法测定兔血清中环丙沙星浓度的方法。方法:取加有10μl内标(含盐酸洛美沙星0.403 mg·ml^(-1))的兔血清样品以OASIS HLB小柱提取其中的环丙沙星,色谱柱为Luna C_(18)柱(250 mm×4.6 mm,5μm),流动相:0.05 mol·L^(-1)枸橼酸-乙腈(82:18),检测波长277 nm。结果:环丙沙星线性范围为25.3～4 048 ng·ml^(-1)(r= 0.999 7),最低检测限为25.3 ng·ml^(-1);方法回收率为96.52%～101.25%;低、中、高3种浓度的日内RSD分别为1.10%,2.05%,1.59%,日间RSD分别为4.20%,4.06%,3.66%。结论:本方法灵敏度高,操作简便,结果准确,可用于兔血清中环丙沙星浓度的测定及其药动学研究。

Objective： To establish a method to determine the Ciprofloxacin in rabbit serum by Solid Phase extraction. Method： The serum sample with the internal standard lomefloxacin（0. 403 mg · ml^-1） was extracted with Waters OASIS solid-phase extractor, The Luna C18 column（250 mm ×4.6 mm, 5 μm） was used. The mobile phase consisted of 0.05 mol·L^-1 ammonium acetate and ace- tonitrile（82： 18） ,the deterction wavelength was 277 nm. Result： A linearity was obtained in the range of 25.3 -4048 ng·ml^-1 ,r = 0. 999 7. The limit of detection was 25.3 ng·ml^-1. The method recovery, was 96.52% - 101.25% ; Within-day precision（RSD） in low, medium, high concentrations were 1.10%, 2.05% and 1.59%, respectively, between-day precision （RSD） were 4.20%, 4.06% and 3.66% ,respectively. Conclusion： The method is sensitive, accurate and simple for the determination of ciprofloxacin in rabbit serum and it was suitable for the pharmacokinetic study.