【摘要】 采用荧光包合色谱法测定痕量的氧氟哌酸(ofloxacin,OFLX)、甲氟哌酸(pefloxacin,PFLX)和司帕氟哌酸(sparfloxacin,SPLX)。实验采用聚酰胺膜为固定相,β环糊精(βcyclodextrin,βCD)水溶液为流动相,并在流动相中直接加入EDTA消除金属离子的干扰,使混合物得到较好的分离。实验表明,氟哌酸化合物在βCD和EDTA的浓度比为0.005∶0.1(mol/L)时最为适宜。在此条件下,OFLX、PFLX、和SPLX的Rf值分别为0.74、0.60和0.25。试样斑点用薄层荧光色谱法扫描测定,激发波长为280nm(OFLX)、278nm(PFLX)和282(SPLX)。各化合物的线性范围分别0～110ng/斑点(OFLX)、0～90ng/斑点(PFLX)和0～93ng/斑点(SPLX);相对标准偏差为2.7%～6.9%;在血样和尿样中的回收率为98.2%～104.6%。更多还原

【Abstract】 Simultaneous determination of ofloxacin (OFLX), peflxacin (PFLX) and sparfloxacin (SPLX) was realized by inclusion thin layer chromatography-fluorescence detection using β-cyclodextrin (β-CD) solutions as mobile phases, EDTA was used here for the mask of some transition metal ions to avoid the formation of norfloxacian-metal complexes. The experimental results show that the optimal molar ratio of β-CD solutions to EDTA is 0.005∶[KG-3/5]0.1. On the polyamide thin layer sheet, OFLX, PFLX and SPLX were separated from each other, and the corresponding R_f values were 0.74, 0.61 and 0.25, respectively. Fluorescence measurement was done using 278 nm(PFLX), 280 nm(OFLX) and 282 nm (SPLX) as the excitation wavelength and the cut-off filter was set at 400 nm. The respective linear ranges correspondingly fell in the concentration of 0~110 ng/spot for OFLX, 0~90 ng/spot for PFLX, and 0~93 ng/spot for SPLX. For all the three components, the relative standard deviations were in the range of 2.7%~6.9% and the recoveries were found to be 98.2%~104.6% in urine and serum samples.更多还原