柱前衍生-高效液相色谱法测定生物检材中的氟乙酸钠  

Determination of Sodium Monofluoroacetate in Biological Sample by HPLC Using Pre-column Derivatization

作　　者：谢珍茗[1] 施文兵[2] 刘岚[1] 邓芹英[1] 

机构地区：[1]中山大学化学与化学工程学院,广东广州510275 [2]广东省公安厅,广东广州510050

出　　处：《分析测试学报》2007年第2期228-231,共4页Journal of Instrumental Analysis

基　　金：广东省科技计划资助项目(2001C32202)

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^-2 mol/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6.0 μmol/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.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.

关 键 词：氟乙酸钠 α-溴苯乙酮 α-氟乙酸苯乙酮酯 柱前衍生化 高效液相色谱 

分 类 号：O657.72[理学—分析化学] R979.8[理学—化学]