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摘要：本论文使用高温气相色谱-质谱（HT-GC/MS）联用技术研究了食用油中甘油三酯的分析方法，并通过EI质谱图确定食用油中甘油三酯组成。考察了实验条件对分离检测的影响，选择测定条件为：DB-5HT30m×0.25mm×0.25μm毛细管柱，进样量0.8 μL（正己烷为溶剂样品浓度为1.5%），分流比20：1；进样口温度350ºC，程序升温：柱温330 ºC，保持5min，以1ºC/min速率升至350ºC，保持5min，然后以1ºC/min速率升至360ºC，保持25min。质谱离子源温度200ºC，接口温度320ºC。用上述条件测定了不同厂家的玉米油、调和油、大豆油和动物油（包括自制的猪油、羊油），并且进行了重复性实验。结果显示，不同厂家玉米油的甘油三酯在组成上相似，在含量上差异不大。结合色谱图与质谱图，动物油中发现了与植物油不同的特征离子峰如m/z341、m/z771、m/z607。关键词： 高温气相色谱-质谱（HTGC-MS）；食用油；甘油三酯（TAGs）；分析7811
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The GC/MS Analysis Of Triglycerides in Edible Oil
Abstract：In the thesis, high temperature gas chromatography-mass spectrometry was studied to analyze and identify triglycerides in edible oil. After the experimental conditions were investigated on the impact of separation and detection, we selected measurement conditions as: DB-5HT30m×0.25mm×0.25μm capillary column, injection volume is 0.8μL(Use hexane as solvent, the concentration is 1.5%), split ratio is 20:1, injection temperature 350ºC, the GC column temperature was programmed from330ºC to 350ºC(hold 5min) at 1ºC/min, and then rose to 360ºC(hold 25min) at 1ºC/min. MS ion source temperature was 200ºC and interface temperature was 320ºC. Some edible oil made by different manufacturers, such as corn oil, cooking oil, soybean oil and animal oil (lard, suet) , was determined using the method and repeated result was obtained. By comparing different oils, we found the triglyceride composition in corn oils of different manufactures are similar while a slightly difference on the content. Combining chromatography and mass spectra, animal oils were compared with vegetable oils. They are different in some characteristic ions like m/z341, m/z771, m/z607.
Keywords：gas chromatography/mass spectrometry；edible oil；triglycerides；analysis
目录
1前言 1
1.1 选题意义 1
1.2 文献综述 1
1.2.1 高温气相色谱（>300ºC） 2
1.2.2 非高温气相色谱（<250ºC） 4
1.2.3 其他技术 5
1.2.4 总结 6
2仪器与试剂 7
2.1 仪器 7
2.2 试剂 7
2.3 样品来源与性状 7
3实验内容 8
3.1 标样的配制 8
3.2 样品的配制 8
3.3 仪器的操作流程 8
3.4 标样的测定 9
3.4.1 三丁酸甘油酯的测定条件 9
3.4.2 甘油三月桂酸酯的测定条件 9
3.4.3 三油酸甘油酯的测定条件 9
3.5 油样的测定 9
3.5.1 玉米油测定条件的选择 9
3.5.2 不同厂家玉米油的测定 11
3.5.3 不同食用油的测定 11
3.5.4 玉米油中掺入猪油的测定 11
4结果与讨论 12
4.1 标样的测定 12
4.1.1 三丁酸甘油酯 12
4.1.2 三月桂酸甘油酯 13
4.1.3 三油酸甘油酯 14
4.2 玉米油测定条件的影响 14