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论文编号:SP100 论文字数:10759,页数:18
摘要:本文评述了高效液相色谱(HPLC)对食品中苏丹红检测的研究进展,内容着重包括样品的制备、样品预处理、净化、萃取剂的选择、检测波长的选择、色谱检测器的选择等。实验部分,采用高效液相色谱法测定鸡蛋黄中的苏丹红Ⅰ、苏丹红Ⅱ、苏丹红Ⅲ、苏丹红Ⅳ。以乙腈提取鸡蛋黄中的苏丹红,以甲酸、乙腈、丙酮和水按一定变化的比率混合作为流动相,经Zorbox-C18色谱柱(4.6mm×150mm)分离,采用478nm,520nm二段变波长检测,获得了较好的分离效果和较低的检测限。该法用于鸡蛋中苏丹红的测定,苏丹红Ⅰ、苏丹红Ⅱ、苏丹红Ⅲ、苏丹红Ⅳ的回收率分别为85%、90%、92%、95%,相对标准偏差分别为2.7%、4.3%、5.3%、3.5%。该法简便、快速、准确,能够满足实际的检测需要。
关键词:食品;检测;苏丹红; 萃取; 高效液相色谱分析
Abstract: In this paper,the progress on determination of Sudan dyes by HPLC were reviewed. The contents include the pretreatment and purification of sample,the selection of extraction agent of Sudan dyes,wavelength,mobile phase,chromatographic detector,and so on. In the part of experiment, the content of SudanⅠ、SudanⅡ、SudanⅢ、SudanⅣ in chick egg yolk has been determined with a high performance liquid chromatographic method. These Sudan dyes were extracted with acetonitrile. The Sudan dyes were separated on a ZorboxSB-C18 column(4.6mm×150mm) with a mixture of acetonitrile、acetone、formic acid and water in certain varied ratio as mobile phase. They were then detected at two shifted wavelength 478nm-520nm,with it the experiment gains good effect for separation and low detecting limit. The recoveries of SudanⅠ、SudanⅡ、SudanⅢ、SudanⅣ were 85%、90%、92%、95% respectively. The relative standard deviations were 2.7%、4.3%、5.3%、3.5% respectively. The method is simple, rapid and accurate,and can meet the needs of practical determination entirely.
Key words: Foodstuff; Determination; Sudan Dyes; Extraction; High Performance Liquid
Chromatographic
目 录
中文摘要 I
英文摘要 II
目录 III
1. 绪论 1
1.1 样品的制备 1
1.2 样品的前处理 2
1.3 样品的净化 3
1.3.1 氧化铝固相萃取净化 3
1.3.2 凝胶渗透过滤净化 4
1.4 高效液相色谱法 4
1.4.1 高效液相色谱分析原理 4
1.4.2 高效液相色谱的类型 5
1.5 色谱分析条件的优化 6
1.5.1 波长的选择 6
1.5.2 流动相的选择 7
1.5.3 检测器的选择 7
1.5.4 色谱柱、柱温、流动相流速和进样量的选择 8
2 实验部分 9
2.1 实验设备 9
2.2 实验试剂与标准品 9
2.3 色谱条件 9
2.4 实验操作 10
2.4.1 溶剂配制 10
2.4.2 样品预处理 10
2.4.3 分离原理 10
3 实验结果与讨论 11
3.1 检测波长的选择 11
3.2 萃取剂的选择 11
3.3 消除色谱干扰的方法 12
3.4 校正曲线和最低检出限 14
3.5 加标回收率实验 14
4 总结与展望 15
致谢 16
参考文献 17