荧光试剂柱前衍生高效液相色谱-荧光检测生物检材中的氟乙酸钠  

Determination of Sodium Monofluoroacetate(1080) in Biological Samples with Fluorescent Precolumn Derivatization by HPLC

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,广州510275 [2]广东省公安厅,广州510050

出　　处：《分析科学学报》2007年第6期685-688,共4页Journal of Analytical Science

基　　金：广东省科技计划资助项目(No.2001C32202);广东省公安厅科研基金资助项目(2001)

摘　　要：建立了以4-溴甲基7-甲氧基香豆素（BrMMC）为柱前荧光衍生试剂，反相高效液相色谱荧光检测（HPLC-FLD）生物检材中氟乙酸钠的分析方法。采用Hewlett Packard RP-18色谱柱，以甲醇-水（60／40，V／V）为流动相，流速1．0mL／min，柱温26℃，荧光检测：λex=319nm，λem=390nm，进样量2μL。结果表明：该法在氟乙酸钠含量为0．1～20μg／mL范围内与其峰面积呈良好的线性关系，线性相关系数为0．9996，检出限（S／N=3）为5×10^-10mol／mL，相对标准偏差（RSD）小于4％。本法用于中毒死亡者的血液样品及其它检材的测定，效果良好。A method was developed for the determination of trace amounts sodium monofluoroacetate （MFA-Na, 1080） in biological samples by high-performance liquid chromatography （HPLC） with fluorescence detector （FLD）. The use of 4-bromomethyl-7-methoxycoumarin （BrMMC） as a fluorescencelabeling reagent has been investigated. The HPLC with a Hewlett Packard RP-18 column and the fluorescence detector at λex 319nm/λem 390nm was employed using 1 mL/min methanol-water （60/40, V/V） as mobile phase. The calibration curve of MFA-Na had a linear range of 0. 1-20μg/mL with r=0. 999 6 and a detection limit of 5×10^-10 mol/mL （S/ N=3）. The relative standard deviation （RSD） was less than 4%. The practical applicability of the method to biological samples was demonstrated by samples of water and serum that were spiked with MFA-Na and by a sample of an individual with MFA-Na consumption.

关 键 词：氟乙酸钠 4-溴甲基-7-甲氧基香豆素(BrMMC) 4-氟乙酸-7-甲氧基香豆素甲酯(MMC-MFA) 高效液相色谱荧光检测 

分 类 号：O657.72[理学—分析化学]