ADVANTAGES OF HPLC WITH ULTRA STABLE ZR02 BASED PHASES

具有超稳定 ZR02 基相的 HPLC 的优点

• 批准号: 6181189
• 负责人: PETER W CARR
• 金额: $ 22.43万
• 依托单位: UNIVERSITY OF MINNESOTA
• 依托单位国家: 美国
• 财政年份: 1996
• 资助国家: 美国
• 起止时间: 1996-08-01 至 2003-07-31
• 项目状态: 已结题
• 来源: https://reporter.nih.gov/project-details/6181189
• 关键词: acidity /alkalinity; biomedical equipment development; high performance liquid chromatography; surface coating; surface property; thermostability; zirconium

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.

描述：（改编自申请人的摘要） 酸/碱稳定（pH 1至14）相的生物色谱，我们开发了高度 稳定的HPLC固定相，基于单分散3微米球， 氧化锆。现在很清楚，氧化锆提供了一个额外的主要优势 超过传统材料：它可以在200 ℃的温度下使用， 高我们将利用这种稳定性来探索气相沉积 由化学反应性单体（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 屏蔽有害的Zr（IV）刘易斯酸位点，其可阻碍 刘易斯碱分析物，特别是肽和蛋白质的色谱法。我们 还将研究使用亚乙基二氨基四亚甲基膦酸 酸衍生物，使稳定的单体固定相的RPLC，NPLC和 手性色谱法与以往的所有努力不同， 专注于氧化锆相的合成，表征和使用，我们现在 建议，鉴于氧化锆相对于其他材料的非凡稳定性， 色谱支持，探索温度作为主要操作 HPLC中的变量。特别是，我们将开发超高速和 超环境温度下的超选择性分析HPLC。多 20-由于将洗脱液温度从25 ℃改变到25 ℃， 200 ℃，分子扩散率成比例增加，应允许 更快（10-20倍）的HPLC成为常规。它肯定会减少 正常流速下的压降，允许使用更长的时间（20倍） 柱和增加的总板数。结合梯度 洗脱，这将大大增加HPLC的峰容量 用常规设备。此外，最近的一项重要工作 已经专注于使用温度作为一种精细“调整”的方法， 色谱选择性和优化分离度。大大扩展了 ZrO 2相对于SiO2基载体的温度范围（至200 ℃）应 显著增强了可实现的选择性变化。的非凡 聚丁二烯和碳涂覆的氧化锆的温度稳定性，以及 他们明显不同的色谱选择性，打开了大门， 扩展热调谐串联柱色谱的令人兴奋的概念 到RPLC，带来了我们操纵能力的重大改进， 色谱选择性和优化HPLC分离。