高效液相色谱-荧光检测法测定人血浆中福多司坦含量

目的建立快速测定人血浆中福多司坦药物浓度洗脱的高效液相色谱-荧光检测法。方法采用高效液相色谱反相柱,流动相：20 mmol/L醋酸钠溶液（含0.6%四氢呋喃,pH7.2）-乙腈（81.5∶18.5）,荧光检测,激发波长：338 nm;发射波长：450 nm。样品与邻苯二甲醛经2-巯基乙醇衍生反应,三氯乙酸沉淀蛋白,离心,上清液进样测定。结果福多司坦血浆浓度定量限和检测限分别为0.20、0.05μg/ml,在0.25~80μg/ml范围内,峰面积与浓度呈良好的线性关系（r=0.9995）,RSD为3.5%,平均回收率为96.2%（n=5）。样品贮存稳定性研究表明,冻融（-18℃）下贮存稳定性较室温稳定性高。结论本方法简便、准确,精密度良好,可用于临床福多司坦血浆样品含量的测定。

Determination of the Concentration of Fudosteine Plasma Sample by high performance liquid chromatography with Fluorescence

Objective To develop a determination method of fudosteine in plasma by high performance liquid chromatography with fluorescence.Methods The sample was separated on a ODS column.The mobile phase consisted of 20 mmol/L sodium acetate anhydrous solution（included 0.6% Tetrahydrofuran,pH 7.2）-acetonitrile（81.5∶18.5）.The wavelength for EX.was 338 nm and EM.was 450 nm.The fudosteine was derived by o-phthalaldehyde with 2-mercaptoethanol.Trichloracetic acid was used to deproteinize.The storage stability of fudosteine plasma was investigated by choosing different storage conditions（room temperature,freeze-thaw and long-term）.The supernatant was detected by the high performance liquid chromatography-Fluoresconce after centrifugation.Results The limit of quantization was 0.20 μg/ml.The limit of detection was 0.05 μg/ml.The calibration curve was linear within a range of 0.25~80 μg/ml for fudosteine plasma（r=0.9995）.The average recovery was 96.2%（n=5） and RSD was 3.5%.The relative standard deviation of the storage stability of fudosteine plasma was 2.7%,1.2% and 1.1% respectively at room temperature,freeze-thaw and long-term.Conclusion This method is accurate,simple and sensitive.It can be used for the determination of fudosteine plasma samples in drug clinical experiments.