【作者】 宋明杰；

【导师】 包海鹰；

【作者基本信息】 吉林农业大学 ， 生药学， 2011， 硕士

【摘要】 以北五味子为研究对象,总木脂素为评价指标,通过正交实验设计优选了北五味子的超临界提取工艺,并对压力、温度、提携剂、萃取时间等这些影响萃取率的主要因素进行了系统考察,确定了最佳的提取工艺,即提取压力为25Mpa,提取温度为45℃,提取时间为3小时,提携剂是浓度为90%的乙醇,最高提取率可达到7.92%。与传统提取方法对比,证明超临界萃取的优越性,此方法具有一定的实用价值。利用大气压化学电离质谱和高效液相色谱指纹图谱分析方法对不同产地、不同生长特征的五味子样品的超临界流体萃取产物进行分析。采用液相色谱-大气压化学电离质谱联用技术分析鉴定产物结构。结果表明,此种分析方法可以有效地对中药材进行品质评价。采用DMPO液质联用技术、FRAP法、H2O2/Fe2+/水杨酸检测体系测定五味子清除羟自由基的能力；以紫外分光光度法测定总木脂素含量,Tris-HCL/邻苯三酚反应体系测定五味子清除超氧阴离子自由基的能力。当浓度为14mg/ml时,样品CB7的羟自由基清除率最高,达到83.70%,样品TH4的FRAP值达到902.55；TH17的总木脂素含量为5.42%,超氧阴离子的清除率为86.89%,GZ3的总木脂素含量为8.52%,超氧阴离子的清除率为84.27%。结合高液相色谱法对五味子中五种主要木脂素类有效成分的定量测定结果,对长白地区、通化地区、公主岭地区不同生长特征的五味子进行抗氧化活性的综合评定。结果表明,五味子对羟自由基、超氧阴离子自由基均有较显著的清除能力,并且五味子发挥抗氧化活性与其中所含化学成分的结构及含量直接相关,此活性测定方法可应用于对五味子的品质评价。研究并建立了一种超高液相色谱-三重四级杆联用技术检测五味子中农药残留的分析方法,采用超声波法脱除农药残留,在25℃、40min条件下的效果较好,并且总木脂素含量损失较小,该方法具有操作简单、灵敏度高、分离效果好、重复性好的特点,是一种实用性强、快速、简便、廉价的检测手段,能满足五味子中农药残留检测的要求。更多还原

【Abstract】 In this study, the orthogonal test was used to optimize CO2-SFE process of the lignans in Schisandra chinensis fruits with the content of total lignan as index. According to the systematic study on different factors to CO2-SFE, such as pressure, temperature, time and alcohol concentration, the optimal extraction procedure was as follows:the extraction pressure was 25 Mpa, the extraction temperature was 45℃, the extraction time was 3 hours and the alcohol concentration was 90%, and the maximum extraction rate was 7.92%. Compared SFE with traditional methods, the optimum extraction procedure is excellent and valuable.The APCI-MSn and HPLC fingerprints analytical methods had been utilized to analyze the constituents in CO2-Supercritical fluid extraction of Fructus Schisandrae from different planting area, of different characteristics and growth years. The extraction products were analyzed by using HPLC-APCI-MS" technique, The structures of extraction products were confirmed. The results demonstrated that this analytical methods are powerful and reliable tools for quality evaluation of Chinese medicinal materials.The detection of the DMPO technology, the FRAP assay and H2O2/Fe2+/salicylic acid method could indicate the change of·OH concentration. Detecting the content of total lignan by UV spectrophotometry. Using Tris-HCL/pyrogallic acid system to detect the decrease percentage of superoxide anion. When the concentration was 14mg/ml, the highest·OH decrease percentage of CB7, reaching 83.70%, the FRAP value could reach 902.55; for TH17, the content of total lignan was 5.42% and the decrease percentage of superoxide anion was 86.89%; for GZ3, the content of total lignan was 8.52% and the decrease percentage of superoxide anion was 84.27%. Combined with the results of HPLC analytical methods to such samples. The results demonstrated that Fructus Schisandrae have excellent antioxidant activities and the activities were correlated with the structure and contents of chemical components and this HPLC-ESI-MS method could be used to evaluate the quality of Schisandra chinensis fruits.The analysis of UPLC-MS technology on pesticide reference compounds. At 25℃、40min conditions, removal of pesticide with smaller loss in the total lignan content by ultrasonic. The method is simple, sensitive, good separation and good repeatability. It is a practical, fast, easy, inexpensive detection in Chinese herbal medicine.更多还原