本文選題：石墨烯　切入點：碳納米管　出處：《河北大學》2017年碩士論文　論文類型：學位論文

【摘要】：隨著人們對藥物殘留及超標問題的日益關注,復雜基質(zhì)樣品中痕量藥物的萃取與分離不斷面臨著更大的挑戰(zhàn);新藥研發(fā)過程需要對藥物進行藥代動力學等考察,而快速準確分離分析生物樣品中痕量藥物的需求在相關領域中顯得尤為迫切�；谏鲜鲂枨�,樣品前處理方法的選擇和優(yōu)化越來越成為分析的關鍵環(huán)節(jié)。固相萃取技術是近年來認可度較高的樣品前處理技術之一,由其衍生的小型化固相萃取技術能夠在保證萃取效率不降低的情況下,縮短樣品處理時間、減少吸附劑和試劑用量,目前已成為樣品前處理領域的開發(fā)熱點。小型化固相萃取中吸附劑用量的減少對吸附劑性能提出了更高的要求,因此本文致力于開發(fā)新型吸附劑材料,制備了兩種納米碳材料,并用于管尖固相萃取過程,結合高效液相色譜,建立了生物樣品中痕量藥物的分離檢測方法。第一章,簡要說明了樣品前處理在痕量藥物分析中的重要性,詳細介紹了納米碳材料及離子液體的優(yōu)點和不足,以及它們在分析領域的應用。第二章,通過向二維的石墨烯片層間引入一維的碳納米管,制備了立體網(wǎng)狀的石墨烯/碳納米管復合納米碳材料,并將其用于自組裝的管尖固相萃取裝置,結合高效液相色譜-熒光檢測法,成功檢測了牛奶樣品中的痕量雌二醇。該方法在5 250 ng m L-1范圍內(nèi)線性良好,校準方程為Y=6.4×103 X+4.5×102,相關系數(shù)r=0.9998。LOD和LOQ分別為0.7 ng m L-1和2.3 ng m L-1。日內(nèi)精密度RSD≤3.7%,日間精密度RSD≤5.8%。雌二醇的回收率范圍在88.4 110.7%,RSDs≤7.4%。第三章,引入一種含末端氨基的離子液體對石墨烯/碳納米管復合材料進行進一步修飾,得到了性能更優(yōu)良、吸附機制更豐富的離子液體-石墨烯/碳納米管復合材料,并將其作為管尖固相萃取的吸附劑,結合高效液相色譜-紫外檢測法,用于檢測尿樣中的(順)-3-(氯代亞甲基)-6-氟-硫色滿-4-酮。該方法在0.03 5.0μg mL-1范圍內(nèi)具有良好的線性,相關方程為Y=7.7×104 X+2.8×102,r=0.9999。檢測限為9×10-3μg mL-1;定量限為3.0×10-2μg m L-1。日內(nèi)精密度和日間精密度RSD分別為4.8%和5.5%。CMFT的回收率范圍在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，

本文編號：1619330