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摘要：本论文在探索751椒碱HPLC分离方法的基础上，用自制银离子液相色谱柱研究了含有不饱和键的751椒碱和食用油的高效液相色谱分离方法。研究了温度、进样量、流速等对分离效果的影响。以含有0.6%乙腈的正己烷为流动相，流速1.5ml/min，柱温5℃，检测波长206nm，样品（浓度约0.5%）进样量5ul，考察了食用油分离的重复性，并实际分离分析了几种食用油商品，显示了不同食用油成分的区别。通过实验验证了自制银离子柱的分离能力和寿命。为食用油的分析检测提供了参考方法。9858
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关键词: 银离子柱；高效液相色谱；食用油；751椒碱
Study on silver ion high performance liquid chromatography and its application for capsaicins and triacylglycerides separation
Abstract: The thesis studied silver ion high performance liquid chromatography method and its application for the separation of unsaturated bond-containing capsaicin and triacylglycerides. Based on home–made silver ion HPLC column, some experimental conditions were investigated including column temperature, injection volume, and flow rate. For triacylglycerides, the HPLC conditions were selected with mobile phase as 0.6% acetonitrile in n-hexane, flow rate as 1.5 ml/min, column temperature as 5 ºC, detector wavelength as 206 nm, injection volume as 5ul, sample concentration as 0.5%(v/v). The repeatability of the separation of triacylglycerides in edible oil was evaluated and presented suitable. Several edible oil products were separated by the method and showed some differences in chromatogram. The silver ion column life was experimentally estimated. This method is useful for edible oil analysis and identification.
Key words: Silver ion column; HPLC; edible oil; capsaicin
目 录
1前言 1
1.1 选题意义 1
1.2 文献综述 2
1.2.1 751椒性状描述 2
1.2.2 751椒样品提取 2
1.2.3 高效液相色谱法在测定751椒制品中751椒素应用 2
1.2.4 化学发光法在测定751椒素含量的应用 5
1.2.5 银离子色谱柱的应用和条件选择 5
1.2.6 HPLC分析食用油 6
2仪器与试剂 8
2.1 仪器 8
2.2.1 色谱仪 8
2.2.2 色谱柱 8
2.2.3 辅助仪器 8
2.2 试剂 8
2.3 样品 9
3实验内容 10
3.1 样品前处理 10
3．1.1 751椒碱标样配制 10
3.1.2 751椒样品配制 10
3.1.3三油酸甘油酯和食用油样品配制 10
3.3仪器操作流程 10
4结果与讨论 11
4.1 用HPLC，C18，手性柱分析751椒碱 11
4.1.1 用C18柱分析751椒碱 11
4.4.2751椒样品不同提取液的分析结果 11
4.4.3 用手性柱分析751椒碱 12
4.2 HPLC银离子柱的制备 12
4.3 HPLC银离子柱用于751椒碱分析 12
4.3.1 正己烷乙腈体系 12
4.3.2 正己烷乙醇体系 13
4.3.2 尝试在低温条件下检测751椒碱 15
4.3.3 HPLC银离子柱分析751椒碱 16
4 HPLC银离子柱分析三油酸甘油酯 16
4.4.1 初步试验 16
4.4.2 温度对三油酸甘油酯的影响 17
4.4.3 降低流动相中乙腈比例的影响 18
4.4.4 流速的影响 19
4.5 HPLC银离子柱低温分析食用油中甘油三酯 20