ADVANTAGES OF HPLC WITH ULTRA STABLE ZR02 BASED PHASES

描述：(改编自申请人的摘要)回应 酸/碱稳定相(pH 1至14)用于生物层析，我们开发了高度 基于单分散3微米微球的稳定的高效液相色谱柱 氧化锆粉。现在很明显，氧化锆提供了一个额外的主要优势。 与传统材料相比：它可以在200摄氏度和 再高一点。我们将利用这种稳定性来探索气相沉积 从具有化学反应的单体(如1，3-丁二烯)制备聚合物 具有改进的传质特性和表面的固定相 对有害的Zr(IV)Lewis酸位的屏蔽会阻碍 刘易斯碱分析物的层析，尤其是多肽和蛋白质。我们 还将调查乙二胺四亚甲基膦的使用 酸衍生物制备RPLC、NPLC和NPLC稳定的单体固定相 手性层析。与之前的所有努力不同，这些努力已经 专注于氧化锆相的合成、表征和用途，我们现在 建议，考虑到氧化锆相较于其他矿物具有极高的稳定性 色谱柱，以探索温度为主要操作方式 高效液相色谱仪中的变量。特别是，我们将同时发展超高速和 超高环境温度下的超选择性分析高效液相色谱。超过 将洗脱液温度从25℃改为25℃，使粘度降低20倍 200摄氏度，分子扩散系数的比例增加，应该允许 更快(10-20倍)的高效液相色谱柱成为常规。它肯定会减少 正常流量下的压力降，允许使用更长的时间(20倍) 柱子和增加的总车牌计数。结合渐变 洗脱，这将提供一个非常需要的增加峰容量的高效液相 用传统的设备。此外，最近的一大部分工作 专注于使用温度作为微调的一种方法 层析选择性和优化分辨率。大大扩展了 氧化锆(至200摄氏度)与二氧化硅载体的温度范围应 大大提高选择性方面可实现的变化。不平凡的 聚丁二烯和碳包覆氧化锆的温度稳定性，以及 它们截然不同的层析选择性，打开了 扩展热调串联柱色谱的激励性概念 给RPLC，带来了我们操纵能力的重大改进 高效液相色谱中的色谱选择性和优化分离。

DESCRIPTION: (adapted from applicant's abstract) Responding to the need for acid/base stable (pH 1 to 14) phases for biochromatography, we developed highly stable HPLC stationary phases based on monodisperse 3 micron spheres of zirconia. It is now clear that zirconia offers an additional major advantage over conventional materials: it can be used at temperatures of 200 C and higher. We will use this stability to explore vapor phase deposition of polymers from chemically reactive monomers (such as 1,3-butadiene) to prepare stationary phases with both improved mass transfer characteristics and surface shielding of the deleterious Zr(IV) Lewis acid sites which can impede the chromatography of Lewis base analytes, especially peptides and proteins. We will also investigate the use of ethylene diamino tetramethylene phosphonic acid derivatives to make stable monomeric stationary phases for RPLC, NPLC and chiral chromatography. In a departure from all previous efforts, which have focused on the synthesis, characterization and use of zirconia phases, we now propose, given the extraordinary stability of zirconia relative to other chromatographic supports, to explore temperature as a principal operating variable in HPLC. In particular, we will develop both ultra-fast and ultra-selective analytical HPLC at super ambient temperatures. The more than 20-fold decrease in viscosity due to changing the eluent temperature from 25 to 200 C, and the proportional increase in molecular diffusivity, should allow much faster (10-20 fold) HPLC to become routine. It will certainly decrease pressure drops at normal flow rates, allowing the use of much longer (20x) columns and increasing total plate counts. In conjunction with gradient elution, this will provide a greatly needed increase in peak capacity of HPLC with conventional equipment. Additionally, a significant body of recent work has focused on the use of temperature as a method of fine "tuning" chromatographic selectivity and optimizing resolution. The greatly extended range in temperature of ZrO2 (to 200 C) vs. SiO2 based supports should considerably enhance the achievable changes in selectivity. The extraordinary temperature stability of both polybutadiene and carbon coated zirconia, and their distinctly different chromatographic selectivities, opens the door to extending the exciting concept of thermally tuned tandem column chromatography to RPLC, bringing about major improvements in our ability to manipulate chromatographic selectivity and optimize separations in HPLC.