摘要:本实验采用超高效液相色谱仪，建立并优化了检测蔬菜中喹啉铜残留量的方法。其方法是用1%草酸水溶液提取基质中的喹啉铜。其次通过氨基柱净化并过0.45 μm的微孔滤膜。最后使用配有紫外检测器的超高效液相色谱仪在254 nm条件下进行测定，其方法是在流动相为10%甲醇水—0.05%三氟乙酸=8+92的混合液等度洗脱。从液相色谱图中可辨别出是否有喹啉铜残留并进行定量比较不同提取方法对回收率的影响。实验进行了0.1mg/kg、0.2 mg/kg和0.4mg/kg三个添加水平测试。回收率在82.1%~92.7%。这个方法的精确性、准确性以及其灵敏度符合农药残留分析测定的要求。23917
毕业论文关键字　喹啉铜；检测技术；液相色谱
The Method of the Determination of Pesticide oxine-copper Residues in Vegetables
Abstract: The research established a method of the determination of oxine-copper residues in vegetables by an ultra Performance Liquid Chromatography (UPLC). The method is the extraction of oxine-copper in Vegetable with 1% Oxalic acid solution. followed by purification of the obtained vegetables on an amino column, and filtered with 0.45 μm filter membrane before use. And then detect the oxine-copper by the UPLC system which equipped with PDA detector at 254 nm. The UPLC method has been developed on reversed phase for separation of oxine-copper with isocratic elution with the mixture of 10%methanol and 0.05% CF3COOH (8:92, v:v). The oxine-copper residue could be identified by the chromatogram data.The precision and accuracy were determined by analyzing the recovery of standard oxine-copper in vegetables samples at three different concentration levels (0.01 mg/kg, 0.2 mg/kg, 0.4 mg/kg) and the results showed that the recoveries for oxine-copper were in a range of 82.1 %~92.7 % . This indicated that the proposed method could be used for the analysis of oxine-copper in vegetables with good accuracy and sensitivity.
Keywords：oxine-copper；determination of residue；UPLC
目  录
1 前言    1
1.1 农药的发展历程    1
1.2 喹啉铜的发展历程及前景    1
1.3 国内外研究进展    2
1.3.1 喹啉铜的理化性质    2
1.3.2 喹啉铜的剂型    2
1.3.3 喹啉铜的作用机理    3
1.3.4 应用状况    3
1.4 现代农药残留检测仪器分析方法    3
1.4.1 气相色谱法(GC)    3
1.4.2 高效液相色谱法(HPLC)    4
1.4.3 超临界流体色谱(SFC)技术    4
1.4.4 液相色谱-质谱联用技术(LC/MS)    4
1.5 超高效液相色谱的认识    5
1.5.1 高效液相色谱仪的原理    5
1.5.2 高效液相色谱仪的应用    5
1.5.3 超高效液相色谱仪的特点    5
1.6 研究目的和意义    6
2 实验部分    7
2.1 试剂与材料    7
2.2 仪器设备    7
2.3 分析步骤    8
2.3.1 提取    8
2.3.2 净化    8
2.3.3 测定    8
2.4 结果与分析    9
2.4.1 仪器条件的讨论    9
2.4.2 比较玻璃容器和塑料容器对喹啉铜的吸附    9
2.4.3 提取剂的比较    11
2.4.4 提取辅助方法及其时间的比较    12
2.4.5 提取量和单双次提取的比较    15
2.4.6 比较过膜和过柱对回收率的影响    15
2.4.7 比较过柱各阶段对回收率的影响    16
2.4.8 比较过柱洗脱液对回收率的影响    17 蔬菜中喹啉铜的检测技术研究:http://www.751com.cn/yixue/lunwen_17177.html