【作者】 金宏；

【导师】 吕志华；

【作者基本信息】 中国海洋大学 ， 生药学， 2006， 硕士

【摘要】 本文通过正交实验获取水蒸气蒸馏法提取丁香挥发油的最佳提取工艺：将丁香干燥花蕾粉碎，室温浸泡24小时，再超声波处理30min，然后水蒸气蒸馏5小时，馏出液静置分层，分离出下层油层，用无水Na₂SO₄脱水即得丁香挥发油纯品。 GC-MS分析条件：色谱柱为SGE-30QC3＼AC225（0.32mm×30m，0.25μm）弹性石英毛细管柱：柱初始温度为70℃，以6℃·min^-1升至160℃，再以3℃·min^-1升至190℃；进样量0.5μL；柱前压60kpa；流速1.0ml·min^-1。并分别对仪器的精密度、重复性、稳定性和10批次丁香挥发油特征指纹图谱做了考察。 实验结果显示，通过正交实验获取水蒸气蒸馏法提取丁香挥发油的提取工艺，产率较高，简便易行。在色谱分析时，主成分峰相对保留时间和相对峰面积的RSD值均小于3％，说明仪器精密度、重复性、样品稳定性好，并利用Microsoft Office办公软件系列中的Excel 2002中的数据处理等功能进行相似度计算，建立丁香挥发油的共有指纹图谱，10批次丁香挥发油的相似度都在0.99以上，符合指纹图谱的要求。 本文全方位优化条件，获得了供试液前处理方法和高灵敏度的色谱条件，所建立的GC-MS分析条件研究丁香挥发油指纹图谱的方法有较好的重现性、精密度和稳定性，再加上GC-MS法具有多成分同时定性的优势，所建立的丁香挥发油的GC-MS指纹图谱为其质量控制提供参考，同时也为中药标准指纹图谱库的建立提供基础。更多还原

【Abstract】 Clove volatile oil is extracted by steam distillation in the research by orthogonal test. The concrete method is described below : The dry buds of cloves are broken into pieces, then dipped in water at room temperature for 24 hours, and then extracted by ultrasonic wave for 30 minutes. The extract is distilled with steam for 5 hours and the distilled solution is left to delaminate for some minutes. The nether layer of oil is isolated and pure volatile oil of clove is obtained after dehydration by anhydrous Na₂SO₄.Conditions of GC-MS are described below: the chromatographic column is SGE-30QC3\AC225（0. 32mm × 30m, 0. 25 μ m）. The column temperature is programmed from 70℃ to 160℃ at 6℃ ? min^-1 and then to190℃ at 3℃ ? min^-1. The injected volume is 0. 5 μL. The pressure before column is 60kpa. They explore the accuracy, fidelity and stability of instrument and analyze the fingerprint spectrum of volatile oil extracted from ten batches of cloves.The accuracy, fidelity and stability of instrument are very good in the tests with the RSD of the relative retention time and area of common peaks smaller than 3%. They match the spectrum and peaks , and calculate the similarity by data processing function of Excel 2002 which is one of the office software of Microsoft Office, and establish the common fingerprint spectrum of clove volatile oil and it meets the requirement of fingerprint spectrum that the similarity of ten batches of cloves is more than 0. 99 .They optimize the conditions and acquire the chromatogram conditions with high sensitivity and proper pre-treatment method . The analysis method of clove volatile oil established by GC-MS has good fidelity, accuracy and stability, and at the same time, the method of GC-MS has the advantage in qualitative analysis of various components simultaneously. As a result, the fingerprint spectrum established here can offer a reference for quality control of clove and make a basis for Chinese traditional medicine fingerprint spectrum establishment.更多还原