论文总字数：19118字

摘 要

苍术具有抗菌消炎、抗溃疡、调节胃肠道蠕动等作用，不同产地苍术的挥发性成分具有明显的差异。脂肪酸类成分除了是人体能源之一，也具有众多的药理活性，特别是多不饱和脂肪酸。至今，对苍术中的脂肪酸类成分未有评价研究。本论文采用气相色谱-质谱联用（GC-MS）结合衍生化方法来测定苍术中脂肪酸的含量。经超声提取法提取苍术中的脂肪酸，采用BSTFA试剂对脂肪酸进行衍生化处理，对各衍生化涉及的条件进行优化，最终衍生化产物用GC-MS检测分析。实验结果表明超声提取法的最佳溶剂为石油醚，衍生化反应的最佳实验条件为：衍生温度80℃，衍生时间20min，衍生试剂量75µL。以此衍生化反应来比较不同产地苍术中脂肪酸的含量。结果表明苍术中主要含有棕榈酸、亚油酸以及油酸，且亚油酸含量最高。

关键词：苍术；脂肪酸；衍生化；气相色谱-质谱联用

Determination of fatty acids in Rhizome Atractylodis by GC-MS after derivatization

Abstract

Rhizome Atractylodis has the activities of anti-bacterial, anti-inflammatory, anti-ulcer and regulation of gastrointestinal motility effects. Previous study has demonstrated that volatile components in Rhizome Atractylodis from different origins have significant differences; however there has been no study about the fatty acids in Rhizome Atractylodis. Fatty acids are not only one of important source of energy, but also beneficial to the human health, especially the polyunsaturated fatty acid. In this study, gas chromatography - mass spectrometry (GC-MS) was applied to determine fatty acids in Rhizome Atractylodis after derivatization. The fatty acids were firstly extracted by ultrasonic extraction, then the extracts were derivated by BSTFA and finally analyzed by GC-MS. The extraction and derivatization parameters were optimized. The results showed that the optimum extraction solvent was petroleum. The optimum derivatization conditions were derivative temperature 80 ℃, derivative time 20min, and amount of reagent 75μL. The developed method was applied to determine the fatty acids in Rhizome Atractylodis from different origins, and palmitic acid, linoleic acid and stearic acid were the main fatty acids in Rhizome Atractylodis, which linoleic acid is the most abundant one.

Keywords：Rhizome Atractylodis；Fatty Acids；Derivatization；GC-MS

目录

1. 文献综述……………………………………………………………………1
   1. 苍术中的脂肪酸成分简介……………………………………………………...1

1.1.1苍术的简介及活性…………………………………………………………….1

1.1.2脂肪酸.................................................................................................................1

1.1.2.1脂肪酸的简介..................................................................................................1

1.1.2.2脂肪酸的活性………………………………………………………………..2

1.2研究脂肪酸成分的提取方法……………………………………………………2

1.2.1超声提取法…………………………………………………………………….2

1.2.2加压溶剂萃取法…………………………………………………………….…3

1.2.3索氏提取法…………………………………………………………………….3

1.2.4超临界CO2萃取法……………………………………………………………4

1.3研究脂肪酸类成分的衍生化方法………………………………………………5

1.3.1硅烷化反应………………………………………………………………….....5

1.3.2酰基作用…………………………………………………………………….....5

1.3.3酯化作用…………………………………………………………………….....5

1.3.4烷基化反应………………………………………………………………..…...6

1.4研究脂肪酸类成分的分析方法………………………………………………....6

1.4.1薄层色谱法（TLC）…………………………………………………………..6

1.4.2气相色谱法（GC）…………………………………………………………….6

1.4.3高效液相色谱法(HPLC)………………………………………………………7

1.5检测方法…………………………………………………………………………7

1.5.1质谱检测器（MS）…………………………………………………………….7

1.5.2蒸发光散射检测器（ELSD）…………………………………………………8

1.5.3示差检测器（RI）…………………………………………………………….8

1.6本课题的研究意义………………………………………………………………9

1. 实验材料与方法…………………………………………………………..10

2.1实验材料………………………………………………………………………..10

2.1.1实验仪器……………………………………………………………………...10

2.1.2实验试剂……………………………………………………………………...10

2.2实验方法………………………………………………………………………..11

2.2.1苍术的前处理………………………………………………………………...11

2.2.2提取方法…………………………………………………………………..….11

2.2.3氮吹浓缩样品………………………………………………………………...11

2.2.4衍生化反应过程……………………………………………………………...11

2.2.4.1衍生温度的选择…………………………………………………………....11

2.2.4.2衍生试剂加入量的选择……………………………….…………………...12

2.2.4.3衍生时间的选择…………………………………………………………....12

2.2.4.4样品再处理………………………………………………………………....12

2.2.5测定不同产地苍术中脂肪酸的含量………………………………………...12

2.3GC-MS测定条件……………………………………………………………….13

2.3.1色谱条件……………………………………………………………………...13

2.3.2质谱条件……………………………………………………………………...13

第三章 结果与讨论………………………………………………………………..14

3.1色谱条件的优化………………………………………………………………..14

3.2提取条件的优化………………………………………………………………..16

3.3衍生化条件的优化……………………………………………………………..17

3.3.1衍生温度的影响……………………………………………………………...17

3.3.2衍生试剂加入量的影响…………………………………………………...…17

3.3.3衍生时间的影响……………………………………………………………...18

3.4不同产地苍术中脂肪酸含量分析……………………………………………..18

第四章 结论与展望..................................................................................................20

4.1结论……………………………………………………………………….....….20

4.2展望…………………………………………………………………………......20

参考文献…………………………………………………………………………....21

致谢………………………………………………………………………………....25

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