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Surface Modified Zirconia as Chiral Stationary Phases

表面改性氧化锆作为手性固定相

基本信息

批准号：
7012197
负责人：
CLAYTON VINCENT MCNEFF
金额：
$ 34.85万
依托单位：
ZIRCHROM SEPARATIONS, INC.
依托单位国家：
美国
项目类别：
财政年份：
2001
资助国家：
美国
起止时间：
2001-09-10 至 2008-01-31
项目状态：
已结题

来源：
https://reporter.nih.gov/project-details/7012197
关键词：
beta antiadrenergic agent carbon chemical stability chemical synthesis microcapsule nonsteroidal antiinflammatory agent optics physical separation silicates stereoisomer technology /technique development zirconium

项目摘要

DESCRIPTION (provided by applicant): Our phase I work addressed one of the major current trends in HPLC - the development of materials for improved chiral chromatography. In response, we prepared two new classes of chiral stationary phases (CSPs). We prepared 10 different examples of the class wherein the chiral selector is covalently bonded to the surface of carbon-clad zirconia. Additionally, we prepared 26 different variants of the second class of CSP wherein the chiral selectors is bonded to the surface of zirconia through a Lewis acid/base coordinate covalent anchor group. We found that the second class of phase generally has much better chiral selectivity than the first and was very comparable to commercial phases based on related chiral selectors. Given the very different surface chemistry of zirconia we believe that Bronsted surface acid-base reactions with aminated drugs will be much less serious issues with zirconia based phases compared to silica-based phases. For these reasons phase II work will center on exploiting the newly developed Lewis acid-base anchored CSPs. Our four principal aims in phase II are: to extend our phase I work on 3 micron analytical HPLC particles unto 5, 7,10 and 25-micron particles for semi-prep and prep-scale LC, to scale-up production to the larger batch sizes, to characterize these larger particles made in bigger batches for their critical chromatographic properties (chiral selectivity, loading capacity, efficiency) and last to synthesize a series of Whelk O 1-like and alpha-Burke 2 emulator phases that can be used for rapid chiral selector screening in new HPLC method development to quickly determine the most appropriate type of chiral selector. To accomplish these goals we will subcontract the synthetic efforts to Prof. Tom Hoye of the University of Minnesota an international expert in the area of natural products synthetic chemistry.

描述（由申请人提供）：我们的I期工作解决了HPLC当前的主要趋势之一-开发用于改进手性色谱的材料。为此，我们制备了两类新的手性固定相（CSP）。我们制备了10种不同的实例，其中手性选择剂共价键合到碳包覆氧化锆的表面。此外，我们制备了第二类CSP的26种不同变体，其中手性选择剂通过刘易斯酸/碱配位共价锚基团键合到氧化锆表面。我们发现，第二类相通常具有比第一类更好的手性选择性，并且与基于相关手性选择剂的商业相非常相似。鉴于氧化锆的表面化学性质非常不同，我们认为与二氧化硅相相比，氧化锆相与胺化药物的布朗斯台德表面酸碱反应将是不太严重的问题。由于这些原因，第二阶段的工作将集中在开发新开发的刘易斯酸碱锚定的CSP。我们在第二阶段的四个主要目标是：将我们的I期工作从3微米分析HPLC颗粒扩展到5、7、10和25微米颗粒，用于半制备和制备规模LC，将生产规模扩大到更大的批量，表征这些在更大批量中制备的更大颗粒的关键色谱特性（手性选择性，装载容量，效率），最后合成一系列Whelk O 1-like和alpha-Burke 2模拟器相，可用于新HPLC方法开发中的快速手性选择剂筛选，以快速确定最合适的手性选择剂类型。选择器为了实现这些目标，我们将向明尼苏达大学的Tom Hoye教授提供合成努力，他是天然产物合成化学领域的国际专家。