固相萃取离子色谱法测定生物样品中氟乙酸钠含量的研究-有机化学专业论文.docxVIP

根离r，用小体积的洗脱液沈脱而使样品富集，能够同时净化和富集氟乙酸钠。 根离r，用小体积的洗脱液沈脱而使样品富集，能够同时净化和富集氟乙酸钠。 通过对固相萃取条件的优化，取得良好的萃取效果，用1．5mL的O．5mol／L的盐 酸做洗脱液t fui收率为9i％以上，富集倍数可达25倍，最低能够检测0．001mg／L 的氟乙酸钠溶液，血样中最低能够检测到O．5mg／L，全程回收率在80％以上 本论文建立了用离子色谱测定生物样品中氟乙酸钠含量的方法。在O．2mL 血液样品中加入lmL纯水，然后用乙腈沉淀蛋白质，待蛋白质沉降后取上层清 液经O．45,um过滤头过滤，滤液注进离子色谱仪进行氟乙酸钠的定性和定量分析。 用Dionex600离子色谱仪，配合电导检测器，Dionex Ion Pac ASl 1明离子交换 色谱柱(结合相应的AGll保护柱)，以2．0mmol／L的Na／B407溶液为淋洗液， 25,uL定量进样环，测定生物样品中的氟乙酸钠，在0．10～10．OⅣg／mL浓度范围 内峰面积和质量浓度呈良好的线性范围(r2=0．9978)，方法的检测限为0．05ug／mL。 实际测定了血液样品的氟乙酸钠，平均全程回收率在85％以L。该法也可用于食 物和生物检材中氟乙酸钠的测定。 本研究还对毛细管电泳测定氟乙酸钠的方法进行了初步研究。 关键词： 氟乙酸钠； 固相萃取：离子色谱；毛细管电泳 Study Study on Determination of Sodium Fluoroacetate in Biological Sample by Solid Phase Extraction—Ion Chromatography Name：YangPing Supervisor：Professor Deng Qinying Major：Organic Chemistry Abstraet The poisoning of raticide has become a serious social and environmental issue these days．Fluoroacetamide is the main part of poisoning of mticide．Which is acute poisonous and easy to translate into sodium fluoroacetate and other matters when entering the organism．Because the content of fluoroacetamide in the toxic organism is very little and the composing of organism is complicated，the pretreatment is necessary for the effective extraction，separation and enrichment．Furthermore， fluoroacetamide is the compound of small molecules with strong polarity,poor volatilization and weak absorption of UV．So it cannot be directly detected using GC and HPLC，derivation is necessary．However,derivation is likely tO bringing new impurity that make the graph of chromatogram complicated and interference larged， Fluomacetate becomes one of the most dimcult poison to be detected．Therefore． developing a qualitative and quantitative analysis method that is simple，sensitive and quick is of important meaning for investigating and solving more and more progressive poisoning of fluoroacetamide，finding out the reason，looking for the resource of poison,beating crime efficiently and ensuring the lives and we