荧光试剂衍生化液相色谱分析生物检材中的氟乙酸钠

发布时间：2018-09-01 20:01

【摘要】：建立了使用新的荧光衍生试剂9-氯甲基蒽(CA)衍生化生物检材中的氟乙酸钠,并通过薄层色谱和荧光检测的高效液相色谱(HPLC)分析的方法。合成得到氟乙酸钠的荧光衍生物——氟乙酸-9-亚甲基蒽酯(MA-MFA),纯度达到98%以上,通过红外光谱、核磁共振、元素分析和质谱对其进行结构表征。薄层色谱中展开剂为石油醚/乙酸乙酯(体积比为95∶5),检测限为5×10-8g(TLC)。高效液相色谱用AgilentHypersilODS反相色谱柱,以乙腈/水(体积比为85∶15)为流动相,荧光检测波长λex为256 nm,λem为412 nm。方法在2.5×10-9~125×10-9mol/mL浓度范围内呈良好的线性关系,线性相关系数为0.9988,生物样品空白添加实验的回收率为83%~90%,最低检测限为2×10-10g(S/N=3),日内、日间RSD均小于4%。该方法用于中毒死亡者的血液样品及其他检材的测定,效果良好。
[Abstract]:A new fluorescent derivative, 9-chloromethyl anthracene (CA), was developed for the determination of sodium fluoroacetate in biological samples by TLC and HPLC with high performance liquid chromatography (HPLC). Fluoroacetic acid-methylene anthracene ester (MA-MFA), a fluorescent derivative of sodium fluoroacetate, was synthesized and its purity was over 98%. Its structure was characterized by IR, NMR, elemental analysis and mass spectrometry. In TLC, the developer was petroleum ether / ethyl acetate (95:5 by volume), and the detection limit was 5 脳 10 ~ (-8) g (TLC). AgilentHypersilODS reversed phase column for HPLC with acetonitrile / water (85:15 by volume) as mobile phase, detection wavelength 位 ex 256 nm, 位 em 412 nm. The linear correlation coefficient was 0.9988. The recovery rate of blank addition experiment for biological samples was 8390g. The lowest detection limit was 2 脳 10-10g (S/N=3). The intraday RSD was less than 4g. The method has been applied to the determination of blood samples and other samples of poisoning dead persons with good results.
【作者单位】：中山大学化学与化学工程学院广东省公安厅中山大学化学与化学工程学院中山大学化学与化学工程学院
【基金】：广东省科技计划资助项目(2001C32202) 广东省公安厅科研基金资助项目(2001)
【分类号】：D919

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