高速逆流色谱原及理应用.ppt

高速逆流色谱技术 在天然香料分离中的应用 Evaluation only.Evaluation only. Created with Aspose.Slides for .NET 3.5 Client Profile .Created with Aspose.Slides for .NET 3.5 Client Profile . Copyright 2004-2011 Aspose Pty Ltd.Copyright 2004-2011 Aspose Pty Ltd. 2 目录 高速逆流色谱发展 1 高速逆流色谱原理 2 高速逆流色谱特点 3 4 高速逆流色谱应用 Evaluation only.Evaluation only. Created with Aspose.Slides for .NET 3.5 Client Profile .Created with Aspose.Slides for .NET 3.5 Client Profile . Copyright 2004-2011 Aspose Pty Ltd.Copyright 2004-2011 Aspose Pty Ltd. 3 Copyright 2012 Andy Guo. All rights reserved。 /9ippt 一、高速逆流色谱发展 高速逆流色谱发明人 Yiochiro Ito博士 我国张天佑教授等人于80年 代引入该技术 Evaluation only.Evaluation only. Created with Aspose.Slides for .NET 3.5 Client Profile .Created with Aspose.Slides for .NET 3.5 Client Profile . Copyright 2004-2011 Aspose Pty Ltd.Copyright 2004-2011 Aspose Pty Ltd. 4 一、高速逆流色谱发展 多极萃取设备庞大复杂、易碎、溶剂体系容易乳化，溶剂耗量 大，分离时间长。 1. 多极萃取技术 Evaluation only.Evaluation only. Created with Aspose.Slides for .NET 3.5 Client Profile .Created with Aspose.Slides for .NET 3.5 Client Profile . Copyright 2004-2011 Aspose Pty Ltd.Copyright 2004-2011 Aspose Pty Ltd. 5 一、高速逆流色谱发展 2、20世纪70年代， 液滴逆流色谱（DCCC） 3、20世纪70年代 离心分配色谱（CPC） 4、20世纪80年代高速逆流色谱 Evaluation only.Evaluation only. Created with Aspose.Slides for .NET 3.5 Client Profile .Created with Aspose.Slides for .NET 3.5 Client Profile . Copyright 2004-2011 Aspose Pty Ltd.Copyright 2004-2011 Aspose Pty Ltd. 6 二、高速逆流色谱原理 原理：作为流动相，在连续洗脱的过程中能保留大量固 定相它利用两相溶剂体系在高速旋转的螺旋管内建立起 一种特殊的单向性流体动力学平衡，当其中一相作为固 定相，另一相。 Ito Y. Journal of Chromatography A, 2005. 1065(2): p. 145-168. Evaluation only.Evaluation only. Created with Aspose.Slides for .NET 3.5 Client Profile .Created with Aspose.Slides for .NET 3.5 Client Profile . Copyright 2004-2011 Aspose Pty Ltd.Copyright 2004-2011 Aspose Pty Ltd. 7 二、高速逆流色谱原理 通过公转、自转（同步行星式运动）产生的二维力场，保留两 相中的其中一相作为固定相 齐誉. 数理医药学杂志, 2011(06): p. 721-724. Evaluation only.Evaluation only. Created with Aspose.Slides for .NET 3.5 Client Profile .Created with Aspose.Slides for .NET 3.5 Client Profile . Copyright 2004-2011 Aspose Pty Ltd.Copyright 2004-2011 Aspose Pty Ltd. 8 二、高速逆流色谱原理 两个不同的区域：1、两相的激烈混合(混合区) 2、两溶剂相分成两层(静置区) 齐誉. 数理医药学杂志, 2011(06): p. 721-724. Evaluation only.Evaluation only. Created with Aspose.Slides for .NET 3.5 Client Profile .Created with Aspose.Slides for .NET 3.5 Client Profile . Copyright 2004-2011 Aspose Pty Ltd.Copyright 2004-2011 Aspose Pty Ltd. 9 二、高速逆流色谱原理 齐誉. 数理医药学杂志, 2011(06): p. 721-724. Evaluation only.Evaluation only. Created with Aspose.Slides for .NET 3.5 Client Profile .Created with Aspose.Slides for .NET 3.5 Client Profile . Copyright 2004-2011 Aspose Pty Ltd.Copyright 2004-2011 Aspose Pty Ltd. 10 二、高速逆流色谱原理 Evaluation only.Evaluation only. Created with Aspose.Slides for .NET 3.5 Client Profile .Created with Aspose.Slides for .NET 3.5 Client Profile . Copyright 2004-2011 Aspose Pty Ltd.Copyright 2004-2011 Aspose Pty Ltd. 11 二、高速逆流色谱原理 HSCCC 系统连接工作图 Evaluation only.Evaluation only. Created with Aspose.Slides for .NET 3.5 Client Profile .Created with Aspose.Slides for .NET 3.5 Client Profile . Copyright 2004-2011 Aspose Pty Ltd.Copyright 2004-2011 Aspose Pty Ltd. 12 二、高速逆流色谱原理 Evaluation only.Evaluation only. Created with Aspose.Slides for .NET 3.5 Client Profile .Created with Aspose.Slides for .NET 3.5 Client Profile . Copyright 2004-2011 Aspose Pty Ltd.Copyright 2004-2011 Aspose Pty Ltd. 13 三、高速逆流色谱特点 Evaluation only.Evaluation only. Created with Aspose.Slides for .NET 3.5 Client Profile .Created with Aspose.Slides for .NET 3.5 Client Profile . Copyright 2004-2011 Aspose Pty Ltd.Copyright 2004-2011 Aspose Pty Ltd. 14 四、高速逆流色谱应用 Evaluation only.Evaluation only. Created with Aspose.Slides for .NET 3.5 Client Profile .Created with Aspose.Slides for .NET 3.5 Client Profile . Copyright 2004-2011 Aspose Pty Ltd.Copyright 2004-2011 Aspose Pty Ltd. 15 四、高速逆流色谱应用 余汉谋. 香料香精化妆品, 2012(01): p. 50-55. Evaluation only.Evaluation only. Created with Aspose.Slides for .NET 3.5 Client Profile .Created with Aspose.Slides for .NET 3.5 Client Profile . Copyright 2004-2011 Aspose Pty Ltd.Copyright 2004-2011 Aspose Pty Ltd. 16 四、高速逆流色谱应用 王美玲. 安徽农业科学, 2010(27): p. 14828-14830. Evaluation only.Evaluation only. Created with Aspose.Slides for .NET 3.5 Client Profile .Created with Aspose.Slides for .NET 3.5 Client Profile . Copyright 2004-2011 Aspose Pty Ltd.Copyright 2004-2011 Aspose Pty Ltd. 17 四、高速逆流色谱应用 实例1、木香中的木香烃内酯和去氢木香内酯（内酯 类化合物） HSCCC条件： 溶剂体系：正己烷-乙酸乙酯-甲醇-水(2 : 0. 5 : 2 : 1) 固定相流速：10mlmin-1，流动相流速:：2.0 mlmin-1 进样量100mg，下相溶样 主机转速：850 rpm 工作温度：28 分离时间：4h 机型：TBE-300 固定相保留率：80. 3% 李躬行. 华西药学杂志, 2009(05): p. 526-528. Evaluation only.Evaluation only. Created with Aspose.Slides for .NET 3.5 Client Profile .Created with Aspose.Slides for .NET 3.5 Client Profile . Copyright 2004-2011 Aspose Pty Ltd.Copyright 2004-2011 Aspose Pty Ltd. 18 四、高速逆流色谱应用 实验结果： 100mg粗样品：木香烃内酯 34. 6mg ，去氢木香内酯： 44. 3mg 检测纯度：均大于98% 李躬行. 华西药学杂志, 2009(05): p. 526-528. Evaluation only.Evaluation only. Created with Aspose.Slides for .NET 3.5 Client Profile .Created with Aspose.Slides for .NET 3.5 Client Profile . Copyright 2004-2011 Aspose Pty Ltd.Copyright 2004-2011 Aspose Pty Ltd. 19 四、高速逆流色谱应用 大孔吸附树脂柱色谱分离： 乙酸乙酯相100g，25%乙醇水溶液溶解后经 D2040大孔吸附树脂柱色 谱层析，分别用25%乙醇除去水溶性杂质，50%乙醇洗脱，得到25g油 状物质。 HSCCC条件： 溶剂体系：石油醚 -乙酸乙酯-甲醇-水(1 : 1.6 : 1 : 1.6) 固定相流速：25 mlmin-1 主机转速：800 rpm 机型：TBE-300A 进样量2050mg 实例2、生姜中的6-姜酚（高速逆流色谱与大孔吸附树脂柱 色谱结合）（酚类化合物） 乔庆亮 . 食品科技, 2010(10): p. 208-210. Evaluation only.Evaluation only. Created with Aspose.Slides for .NET 3.5 Client Profile .Created with Aspose.Slides for .NET 3.5 Client Profile . Copyright 2004-2011 Aspose Pty Ltd.Copyright 2004-2011 Aspose Pty Ltd. 20 四、高速逆流色谱应用 乔庆亮 . 食品科技, 2010(10): p. 208-210. Evaluation only.Evaluation only. Created with Aspose.Slides for .NET 3.5 Client Profile .Created with Aspose.Slides for .NET 3.5 Client Profile . Copyright 2004-2011 Aspose Pty Ltd.Copyright 2004-2011 Aspose Pty Ltd. 21 四、高速逆流色谱应用 实例3、芫荽中的芫荽异香豆精、二氢 芫荽异香豆精、芫荽异香豆酮A 和B（高速逆流色谱与超临界CO2流