论文总字数：19491字

摘 要

研究了从山茶油中提取角鲨烯的分离纯化方法，同时建立了角鲨烯的气相色谱检测法。预处理实验表明，山茶油中角鲨烯的含量可达17.66ug/ml,其中在反应温度为30℃，时间为2h时测得含量最高。气相色谱法对角鲨烯的分析结果为：角鲨烯进样量在1.0μL范围内，峰面积与进样量呈良好的线性关系，角鲨烯的回归方程为y=13.2161555x-11.971825，相关系数R²为0.9994，方法精密度为1.06%，回收率为98.5%~102.2%。

结论：本实验检测了山茶油中角鲨烯的含量是17.66ug/ml，为检测山茶油中角鲨烯含量提供了检测方法。本文建立了山茶油中角鲨烯含量的GC分析方法。山茶油中的脂肪酸甲酯化，角鲨烯同步萃取于石油醚-苯（1 1）溶剂中，经强极性毛细管柱HP- 5分离，质谱选择离子监测对角鲨烯进行定量测定。该方法在0.01～0.50mg/mL范围内线性关系良好，角鲨烯的回归方程为y=13.2161555x-11.971825，相关系数R²为0.9999，最小检测限为1.80ng/mL，方法回收率在99.5%～110.0%之间，相对标准偏差为4%。该方法前处理简单、便捷，定量准确，灵敏度高，可用于实验室检测山茶油中角鲨烯的含量。

关键词：山茶油 角鲨烯 GC分析 回收率

ABSTRACT

Study on the separation and purification method of extracting Squalene from camellia oil, also established the squalene gas chromatography. The experiment showed that pretreatment, camellia oil squalene content up to 17.66ug/ml, the reaction temperature 30 ℃, time 2H measured the highest content. Analysis results of gas chromatography of squalene: squalene in range of 1.0μL, there was a good linear relationship between peak area and the amount of sample, the regression equation of squalene is y=13.2161555x-11.971825, correlation coefficient R² is 0.9994, the precision is 1.06%, the recovery rate was 98.5%~ 102.2%.

Conclusion: this experiment was used to measure the content of Camellia Oil squalene is 17.66ug/ml, provides a detection method for detecting the content of squalene in Camellia oil. In this paper, the content of squalene camellia oil in the GC analysis method was established. Camellia oil is the fatty acid methyl ester, squalane synchronous extraction in petroleum ether and benzene (1 1) in the solvent, the strong polar capillary column HP- 5 separation, mass spectrometry with selected ion monitoring of squalene was quantitatively determined. The method is in the range of 0.01 ~ 0.50mg/mL good linear relationship, regression equation of squalene is y=13.2161555x-11.971825, correlation coefficient R² is 0.9999, the minimum detection limit is 1.80ng/mL, the recovery was 99.5% ~ 110%, the relative standard deviation is 4%. This method is simple, convenient, accurate, high sensitivity, and can be used for content of Camellia Oil squalene in testing laboratory.

KEYWORDS:Camellia oil; Squalene; GC analysis;Recovery

目录

摘要………………………………………………………………………………………………I

Abstract ………………………………………………………………………………………II

1. 文献综述 ……………………………………………………………………………1

1.1角鲨烯的理化性质………………………………………………………………………1

1.2角鲨烯的来源于分布……………………………………………………………………1

1.3角鲨烯的应用领域………………………………………………………………………1

1.4角鲨烯的分离与纯化……………………………………………………………………2

1. 实验材料及方法……………………………………………………………………8

2.1实验材料…………………………………………………………………………………8

2.1.1 主要实验试剂 ……………………………………………………………………8

2.1.2 主要实验仪器 ……………………………………………………………………8

2.2 实验方法 ………………………………………………………………………………9

2.2.1 GC分析条件的确定 ………………………………………………………………9

2.2.2角鲨烯标准曲线的绘制……………………………………………………………9

2.2.3强碱浓度对皂化-甲酯化反应的影响……………………………………………10

2.2.4温度对皂化-甲酯化反应的影响…………………………………………………10

2.2.5皂化-甲酯化反应时间曲线………………………………………………………11

2.2.6不同溶剂对角鲨烯得率的影响 …………………………………………………11

2.2.7不同产地山茶油中角鲨烯的测定 ………………………………………………11

1. 实验结果与讨论 …………………………………………………………………12

3.1角鲨烯标准曲线………………………………………………………………………12

3.2皂化-甲酯化条件优化 ………………………………………………………………13

3.3本章小节………………………………………………………………………………16

1. 结论与展望…………………………………………………………………………18

参考文献………………………………………………………………………………………20

致谢 ……………………………………………………………………………………………22

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