摘要：本论文从实验室中常见的分离填料：硅胶（200-300目）、D101型大孔吸附树脂、IR120钠型阳离子交换树脂和新型PET粉（聚对苯二甲酸乙二醇酯）出发，自制固相萃取（SPE）小柱，考察其分离富集性能和应用。将上述四种填料物质分别干法装入针筒式塑料SPE空柱并封顶，活化后将模拟样品溶液过柱，经淋洗后用适当的洗脱剂洗脱，通过高效液相色谱技术对样品溶液和流出液的分析，对自制SPE柱的富集和洗脱效果进行了评价。实验结果表明，在初步选择的SPE实验条件下，自制IR120阳离子交换SPE柱对于L-苯丙氨酸SPE萃取的粗算回收率在90%~106%，奎宁的回收率在36%~78%；D101型大孔吸附树脂SPE柱对于乙基苯的SPE萃取回收率为115%，对白酒中的己酸乙酯的回收率范围在69%~83%，对心得安（原料药）的SPE萃取回收率为27%~38%；自制硅胶SPE柱对于酮康唑的SPE的回收率为103%，奎宁的SPE回收率为15%。自制固相萃取SPE柱对部分模拟化合物有较好的分离富集能力，进一步的研究可用于实际样品的预处理。81836

毕业论文关键词：固相萃取；自制；硅胶；阳离子交换；大孔树脂；聚对苯二甲酸乙二醇酯

Preparation and application of solid phase extraction columns

Abstract: In this paper, 4 kinds of solid phase extraction (SPE) columns were made in laboratory using normal materials in laboratory of silica gel (200-300 mesh), D101-type macroporous adsorption resin, IR120 sodium cation exchange resin and a new type of PET powder(polyethylene terephthalate)。 The columns were investigated for their enrichment characteristics and application。 Each of the four kinds of matrix material was filled respectively into a plastic syringe SPE empty column and capped。After the SPE column was activating, the simulated sample solutions were loaded on the column, then elution with the appropriate solvent or solution。 The enrichment and elution of the SPE columns were evaluated by analysing the sample solution and effluent using high performance liquid chromatography with peak area to calculate crude recovery。As result, using the selected SPE conditions, the crude recoveries of the IR120 cation exchange SPE column for L-phenylalanine SPE were in 90% ~ 106%, and that for quinine were in 36%~78%。 The crude recovery of the D101 type macroporous adsorption resin SPE column for ethylbenzene was 115%, the recovery of ethyl caproate in liquor were in 69%~83% and the recovery of propranolol was 27%~38%。 The crude recovery of the lab-made silica gel SPE column for ketoconazole was 103%,and that for quinine was 15%。The SPE columns perform on certain compounds respectively, and further research can be used in real sample preparation。

Keywords: solid phase extraction; homemade; silica gel; cation exchange ;macroporous resin ; polyethylene terephthalate

目录

1 前言 1

1。1 本课题的研究目的与意义 1

1。2 固相萃取的概要 1

1。2。1 固相萃取的简介 1

1。2。2 固相萃取的原理与步骤 1

1。2。3 固相萃取柱的类型 2

1。2。4 影响固相萃取的因素 2

1。3 回收率的计算 3

1。4 几种不同类型的固相萃取柱在实际分析中的应用 3

1。4。1 C18型 3

1。4。2 弗罗里硅土（florisil）型 4

1。4。3 HLB型 5

1。4。4 氧化铝型