固相萃取—反相HPLC荧光法快速测定血浆中氟罗沙星.pdfVIP

固相萃取—反相HPLC荧光法快速测定血浆中氟罗沙星 王乃毅1,* 白小红2 ( 1 山西职工医学院分析化学教研室，太原030012 2 山西医科大学药学院，太原030001) 摘要 目的: 建立固相萃取—反相HPLC荧光法快速测定人血浆中氟罗沙星的方法。 方法：采用C 固相 18 萃取小柱萃取血浆中的氟罗沙星。色谱柱为ODS—BP柱 （5μm，250mm×4.6mm），流动相为含1.31g/L L－ 异亮氨酸和0.80g/L CuSO 的水溶液－甲醇 （80:20 ,V:V）,激发波长为280nm,发射波长为504nm，流速为 4 0.8ml/min。结果：该方法在 0.4～20μg/ml浓度范围内线性关系良好（r 0.9993），最小检测限50ng/ml， 萃取回收率和方法回收率分别为89.52%和100.45%，高、中、低3个浓度的日内RSD为3.2%，日间RSD 为 1.5%。结论：该法血样处理简单，干扰小，灵敏度高，精密度好，可用于该药物体内监测的快速测定。 关键词：氟罗沙星；固相萃取；HPLC 荧光法；药物滥用 Quick Determination of Fleroxacin in Human Plasma by Solid Phase Extraction and RP--HPLC withFluorometry 1,* 2 Wangnaiyi , Baixiaohong ( 1Department ofAnalyticalChemistry,ShanxiMedical College for Continuing Education,Taiyuan 030012,China 2 PharmaceuticalCollege, ShanxiMedicalUniversity,Taiyuan 030001,China) Abstract Objective:To set up a new method to quickly determine Fleroxacin in human plasma by SPE and RP-HPLC with fluorescence detection. Method:The Fleroxacin in human plasma was extracted by SPE with C18 SPE column ， and then the quantities of the Fleroxacin were determined by RP-HPLC. The chromatography column usedwas a ODS BPcolumn (5 m 250mm 4.6mm).Andthemobilephasewasmadeup ofthewater — μ ， × solution (includingL–isoleucine(1.31g/L) and CuSO (0.80g/L) ) andmethanol 80:20 ,V:V .Theexcitation and 4 （ ） emission wavelengths were 280nm and 504nm. The flow rate was 0.8ml/min.Results: The linear range of the method was 0.4 ~20 g/ml and r value was 0.9993; the detection limits was 50ng/ml (S:N 3:1)