基于功能化纳米碳材料的痕量药物萃取分离方法研究

发布时间：2018-03-16 09:32

  本文选题：石墨烯　切入点：碳纳米管　出处：《河北大学》2017年硕士论文　论文类型：学位论文

【摘要】：随着人们对药物残留及超标问题的日益关注,复杂基质样品中痕量药物的萃取与分离不断面临着更大的挑战;新药研发过程需要对药物进行药代动力学等考察,而快速准确分离分析生物样品中痕量药物的需求在相关领域中显得尤为迫切。基于上述需求,样品前处理方法的选择和优化越来越成为分析的关键环节。固相萃取技术是近年来认可度较高的样品前处理技术之一,由其衍生的小型化固相萃取技术能够在保证萃取效率不降低的情况下,缩短样品处理时间、减少吸附剂和试剂用量,目前已成为样品前处理领域的开发热点。小型化固相萃取中吸附剂用量的减少对吸附剂性能提出了更高的要求,因此本文致力于开发新型吸附剂材料,制备了两种纳米碳材料,并用于管尖固相萃取过程,结合高效液相色谱,建立了生物样品中痕量药物的分离检测方法。第一章,简要说明了样品前处理在痕量药物分析中的重要性,详细介绍了纳米碳材料及离子液体的优点和不足,以及它们在分析领域的应用。第二章,通过向二维的石墨烯片层间引入一维的碳纳米管,制备了立体网状的石墨烯/碳纳米管复合纳米碳材料,并将其用于自组装的管尖固相萃取装置,结合高效液相色谱-荧光检测法,成功检测了牛奶样品中的痕量雌二醇。该方法在5 250 ng m L-1范围内线性良好,校准方程为Y=6.4×103 X+4.5×102,相关系数r=0.9998。LOD和LOQ分别为0.7 ng m L-1和2.3 ng m L-1。日内精密度RSD≤3.7%,日间精密度RSD≤5.8%。雌二醇的回收率范围在88.4 110.7%,RSDs≤7.4%。第三章,引入一种含末端氨基的离子液体对石墨烯/碳纳米管复合材料进行进一步修饰,得到了性能更优良、吸附机制更丰富的离子液体-石墨烯/碳纳米管复合材料,并将其作为管尖固相萃取的吸附剂,结合高效液相色谱-紫外检测法,用于检测尿样中的(顺)-3-(氯代亚甲基)-6-氟-硫色满-4-酮。该方法在0.03 5.0μg mL-1范围内具有良好的线性,相关方程为Y=7.7×104 X+2.8×102,r=0.9999。检测限为9×10-3μg mL-1;定量限为3.0×10-2μg m L-1。日内精密度和日间精密度RSD分别为4.8%和5.5%。CMFT的回收率范围在73.9-93.9%,RSDs≤7.8%。
[Abstract]:As people pay more and more attention to the problem of drug residue and over-standard, the extraction and separation of trace drugs in complex matrix samples are facing more and more challenges. The need for rapid and accurate separation and analysis of trace drugs in biological samples is particularly urgent in related fields. The selection and optimization of sample pretreatment methods are becoming more and more important in analysis. Solid phase extraction (SPE) is one of the most recognized sample pretreatment techniques in recent years. The miniaturized solid-phase extraction technique derived from it can shorten the sample treatment time and reduce the amount of adsorbent and reagent without reducing the extraction efficiency. The reduction of adsorbent amount in miniaturized solid phase extraction (SPE) has put forward higher requirements for the performance of adsorbents. Therefore, this paper is devoted to the development of new adsorbent materials and the preparation of two kinds of nanocrystalline carbon materials. A method for the separation and determination of trace drugs in biological samples was established by means of tube tip solid phase extraction (SPE) and high performance liquid chromatography (HPLC). In Chapter 1, the importance of sample pretreatment in the analysis of trace drugs was briefly explained. The advantages and disadvantages of nanocrystalline carbon materials and ionic liquids and their applications in the field of analysis are introduced in detail. A three-dimensional netted graphene / carbon nanotube composite carbon composite material was prepared and used in a self-assembled tubular tip solid-phase extraction device, which was combined with high performance liquid chromatography (HPLC) and fluorescence detection method. Trace estradiol in milk samples was successfully determined with a good linearity in the range of 5 ~ 250ng mL ~ (-1). The calibration equation is YTX 6.4 脳 103X 4.5 脳 102, and the correlation coefficients r 0.9998.LOD and LOQ are 0.7 ng mL ~ (-1) and 2.3 ng m ~ (-1), respectively. The intra-day precision RSD 鈮，

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