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气质联用仪在槐花等分析中的应用

Analysis in Sophora Japonica L, Etc by Gas Chromatography/Mass Spectrometry

【作者】 王丽艳

【导师】 李继平; 由万胜;

【作者基本信息】 辽宁师范大学 , 无机化学, 2008, 硕士

【摘要】 本文开始介绍了气相色谱-质谱联用(GC/MS)技术概况及其在各个领域的应用,对GC/MS联用仪的分析特点、仪器配置、基础知识作了概括。作为最主要的分析手段之一—GC/MS联用仪的应用范围极为广泛,本文从食品安全、天然产物、环境保护、法庭科学这四个领域进行综述。本文主要内容分三部分。首先,选取天然产物槐花进行GC/MS分析。从GC/MS联用仪对天然产物分析侧重于某一类物质的分析出发,本文重点研究槐花的挥发油和脂肪酸的组成,主要从样品的前处理和气相色谱-质谱条件的选择两方面进行研究。实验结果是,从槐花中,鉴定出挥发油30种成分,占挥发油总量的84.41%;鉴定出脂肪酸13种,这13种脂肪酸相似度都在90%以上。然后,利用GC/MS联用仪对茶饮料中咖啡因进行定性分析、定量分析两方面研究。在定性分析中,主要是分析样品的制备和气质联用分析条件的选择,采用和标准谱图对照的方法定性确定咖啡因。在定量分析中,采用外标法对茶饮料中的咖啡因的含量进行分析。自动进样器的使用解决了外标法需要的进样量准确、重复性好的实验要求;质谱扫描方式选择全扫描和选择离子两种扫描方式,选择离子扫描选取m/z为67、82、109、194四种离子。定性结果准确,与谱库标准谱图相似度达99%;定量方法可行,回收率、精密度均在限定范围内。最后,对海参提取液中的脂肪酸进行了GC/MS分析,通过甲酯化条件的探索,找到最佳的实验条件,实验结果共鉴定出31种脂肪酸,占总馏出组分的80.33%。

【Abstract】 In this thesis, at first, gas chromatography/mass spectrometry (GC/MS) technology and its applications in various fields, its analysis characteristics、equipment configurations and relevant basal knowledge have been introduced. As one of the most important means—GC/MS has been applied extensively, the thesis summarized its applications in the four areas, namely food security、natural products、environmental protection and the court science.The main content has been divided into three parts. In first part, the chemical components in Sophora japonica L were analyzed by GC/MS. We focused attention on the analysis of the volatile oil and fatty acid components in Sophora japonica L. The samples processing and GC/MS conditions choice were studied. As a result, 30 components of the volatile oil were identified, which represented 84.41% of the total GC peaks of the volatile oil; 13 kinds of fatty acids were identified, and similarity of 13 species fatty acids all were more than 90%.In second part Caffeine in tea beverage was measured from the qualitative analysis and quantitative analysis with GC/MS. In qualitative analysis, the key step was sample preparation and the GC/MS analysis conditions choice. The qualitative method was compared with the caffeine standard spectrum. In quantitative analysis, the external standard method has been used to determine the caffeine concentration in tea beverage, using automatic sampling to solve the accurate sample volume in the external standard method. MS scan mode included Full-scan and SIM scan choice, in SIM scan, m/z 67、82、109 and 194 four ions was selected. Qualitative results were accurate, and standard spectrum similarity was 99 percent. Quantitative method was feasible, the recovery rate and precision were acceptable.Finally, the fatty acids of the sea cucumber extract was analyzed by GC/MS. The best experimental conditions were found. As a result, 31 kinds of fatty acids were identified. The components of fatty acids represent 80.33 % of the total fraction

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