液相色谱柱基础解析.ppt

Agenda 2013 Lab Water China Marketing Plan| 20 Feb. 2013 * 为什么要了解色谱柱 1 2 如何成为色谱柱专家 在LC实验室中寻找销售机会 3 色谱柱使用寿命一年左右： 水质对色谱柱的累积作用 Particles Bacteria Other。。。。。。 Bottle water HPLC实验室 色谱柱的使用寿命平均在3-6个月： 溶剂对实验结果的影响 UPLC实验室 Organics Ion Bottle water Other。。。。。。 问题? * A Basic Method Development Strategy Rev. 27807 3: * of 46 * * * Here we see the same procedure adapted to give a silicon-carbon hybrid particle. This is a cartoon depicting this particle known as XTerra in which we have now incorporated carbon into our silica gel matrix providing high pH stability. So you can see that the methyl group is actually incorporated into the matrix of our particle. This is very different from a traditional silica gel column in which surface modifications have been made to add carbon through siloxane bonded alkyl groups to the surface such as an endcapping reagent as well as the primary ligand to to give us our bonded phases. This particle is a very different material in that the methyl group is not just a surface modification. The methyl groups are incorporated into the entire particle and the bond is a silicon-carbon bond-not a weaker siloxane bond. Note this is a patent pending new technology from Waters, and has just received the R+D 100 award. This is an award that recognises the 100 most technologically products brought sucessfully to market in 1999 * * * * * * * 残留硅羟基 端基封口基团 C18 填料的合成—2. 端基封口 四乙氧基硅烷 TEOS 硅甲基嵌入型聚乙氧基硅烷 MPEOS 甲基三乙氧基硅烷 MTEOS 第一代杂化颗粒的合成过程 为何杂化颗粒柱可增加在高pH下的柱寿命？ 硅胶快速溶解 严重的柱失效 柱寿命短暂 Surface modified Silica Particles 因嵌入硅甲基的阻挡, 颗粒表面溶解速度明显减缓 柱寿命大大延长 XTerra? Hybrid Particles 普通硅胶柱 基于杂化颗粒的Xterra 柱 XBridge:第二代杂化填料的合成 硅胶基体中插入的桥式乙基 美国专利号 6,686,035 B2 Tetraethoxysilane TEOS Bis triethoxysilyl ethane BTEE + 4 Polyethoxysilane BPEOS 挑战性流动相: 0.02N NaOH pH 12.3 , 50°C 测试时的流动相: 50/50 v/v 乙腈/水 , 50°C 标准测试物: 苯癸酮 0 10 20 30 40 50 XBridge? C8 XBridge? C18 XBridge? Phenyl XBridge? Shield RP18 XTerra? MS C18 Symmetry? C18 要使柱效降低一半, 需将色谱柱曝露在 0.02N NaOH pH 12.3 和 50℃