调味品中合成辣椒碱的HPLC分析
关键词: 银离子柱；高效液相色谱；食用油；吹冰椒碱
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 吹冰椒性状描述 2
1.2.2 吹冰椒样品提取 2
1.2.3 高效液相色谱法在测定吹冰椒制品中吹冰椒素应用 2
1.2.4 化学发光法在测定吹冰椒素含量的应用 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 吹冰椒碱标样配制 10
3.1.2 吹冰椒样品配制 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，手性柱分析吹冰椒碱 11
4.1.1 用C18柱分析吹冰椒碱 11
4.4.2吹冰椒样品不同提取液的分析结果 11
4.4.3 用手性柱分析吹冰椒碱 12
4.2 HPLC银离子柱的制备 12
4.3 HPLC银离子柱用于吹冰椒碱分析 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吹冰椒碱 15
4.3.3 HPLC银离子柱分析吹冰椒碱 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
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