【摘要】 以α-溴苯乙酮酯为衍生化试剂,合成了α-氟乙酸苯乙酮酯(APFA)化合物,并以其为标准,建立了柱前衍生-高效液相色谱法测定生物检材中氟乙酸钠的方法。样品中的氟乙酸钠经酸化,丙酮-水(体积比4∶1)萃取,与α-溴苯乙酮衍生化后进行HPLC分析。色谱条件为:Hypersil ODS柱,乙腈-水(体积比50∶50)为流动相,紫外检测波长为254 nm。α-氟乙酸苯乙酮酯在1×10-5~1×10-2mol/L的浓度范围内与峰面积呈良好的线性关系,线性相关系数为0.999 4,生物样品空白添加实验的回收率为86%~93%,检出限为6.0μmol/L(S/N=3),相对标准偏差(RSD)小于3%。该方法灵敏度高、重复性好,适用于生物检材中氟乙酸钠的测定。更多还原

【Abstract】 A new HPLC method for the determination of sodium monofluoroacetate in biological sample has been developed using pre-column derivatization.Sodium monofluoroacetate was extracted with acetone-water(4 ∶ 1,by volume),and followed by derivatization with α-bromoacetophenone in the presence of tetrabutylammonium bromide.The derivatives were separated by HPLC on Hypersil ODS column using 0.5 mL/min acetonitrile-water(50 ∶ 50,by volume) as mobile phase.The UV detection was performed at 254 nm.The calibration curve has a linear range of 1×10-5-1×10-2 mol/L with a correlation coefficient of 0.999 4 and a detection limit of 6.0 mol/L(S/N=3).The recovery range of sodium monofluoroacetate from biological samples was 86%-93% and the relative standard deviation was less than 3%.The method is reliable,simple and suitable for the determination of sodium monofluoroacetate in biological samples.更多还原