【作者】 肖晓杏；

【导师】 申书昌；

【作者基本信息】 齐齐哈尔大学 ， 分析化学， 2014， 硕士

【摘要】 固相萃取（Solid Phase Extraction，简称SPE）是由柱液相色谱和液固萃取相结合发展而来的。固相萃取过程是固相萃取填料选择性吸附和解吸附目标化合物的过程，在这一过程中实现了对目标化合物的纯化、分离和富集。由于固相萃取技术具有溶剂用量小、操作时间短、干扰少等特点，因此可用于多组分样品中微量或痕量目标物的预处理，并具有良好的重现性。由于液相色谱（LC）、气相色谱（GC）、电感耦合等离子体发射光谱（ICP-AES）、红外光谱（IR）等方法的样品前处理都可以使用固相萃取，因此，固相萃取有着广泛的应用。本文以氧氯化锆和氨水为原料，采用聚合诱导胶体凝聚法制备分布均匀的二氧化锆微球。用钛酸偶联剂对二氧化锆进行表面改性，使其表面具有碳碳双键基团。通过自由基聚合反应，使甲基丙烯酸、苯乙烯、二乙烯苯与改性氧化锆表面双键进行交联聚合，聚乙烯醇作为分散剂，BPO作为引发剂，得到聚苯乙烯-甲基丙烯酸/氧化锆固相萃取填料。借助FT-IR、XPS、SEM等手段对其元素组成及微观形貌进行分析与表征。用制得的填料制成固相萃取小柱，并与高效液相色谱联用测试水中的西玛津、特丁津和氰草津，在1.0μg/mL~5.0μg/mL范围内，色谱峰面积与西玛津、特丁津和氰草津浓度线性关系良好。相关系数（R2）分别为0.9991、0.9986和0.9961。测定结果的相对标准偏差分别为1.19%~3.33%、1.42%~4.99%、2.05%~5.14%。最低检出限分别为0.7329μg/L、0.9181μg/L、0.6443μg/L。考察洗脱液和过柱流速对回收率的影响，当过柱流速为2mL/min、洗脱液为2mL乙腈+3mL氨化甲醇时，自制小柱对水中的西玛津、特丁津和氰草津具有良好的回收效果，回收率分别为77.23%、71.56%和75.04%。更多还原

【Abstract】 Solid phase extraction(SPE) was developed from liquid-solid extraction and column liquidchromatography technology.The process of solid phase extraction is that target compoundsare selective adsorbed by solid phase extraction packing and desorbed by eluant.In the process,target compounds are purified, separated and concentrated. SPE has many features such assolvent dosage small, short operation time, less interference substances, etc. Therefore, it canbe used to preproccess trace target compounds in complex samples. And it has goodreproducibility. SPE can be used in many analytical methods such as liquid chromatography(LC), gas chromatography (GC), inductively coupled plasma emission spectrometer(ICP-AES), infrared spectra (IR). Therefore, SPE has been widely used.In this paper, distributed evenly zirconia microspheres were prepared with zirconiumoxychloride and ammonia by polymerization induced colloid aggregation method. Thesurface of zirconia microspheres were modified by titanate coupling agent, then its surfacehas the carbon-carbon double bond groups. Through radical polymerization, styrene,divinylbenzene, methacrylic acid and modified zirconia surface’s double bond werepolymerized, polystyrene-methacrylic acid/zirconia solid phase extraction packing wasobtained (Initiator is BPO, dispersant is PVA). The elementary composition and microcosmicmorphology of the material were analyzed and characterized by means of FT-IR, XPS, SEMand other means. Simazine, terbuthylazine and cyanazine in the water were tested by SPEcolumn prepared with high performance liquid chromatography (HPLC). Within the range of1.0μg/mL-5.0μg/mL, between of chromatographic peak areas and simazine, terbuthylazineand cyanazine’s concentration were linear. The correlation coefficients (R2) were0.9991,0.9986and0.9961respectively. The relative standard deviation of analysis results were1.19%-3.33%,1.42%-4.99%,4.99%-5.14%respectively. The minimum detection limit were0.7329μg/L,0.9181μg/L,0.6443μg/L respectively. The paper also discussed certain factorswhich influence the extracting efficiency. When flow rate was2mL/min and eluent was2mLacetonitrile and3mL ammoniated methanol, the SPE column had good recovery effect onsimazine, terbuthylazine and cyanazine in the water. The recoveries were77.23%,71.56%and75.04%respectively.更多还原