Non-Spherical Particles for HPLC

用于 HPLC 的非球形颗粒

基本信息

批准号：
9321117
负责人：
Barry E Boyes
金额：
$ 17.61万
依托单位：
ADVANCED MATERIALS TECHNOLOGY, INC.
依托单位国家：
美国
项目类别：
财政年份：
2013
资助国家：
美国
起止时间：
2013-08-01 至 2018-07-31
项目状态：
已结题

项目摘要

DESCRIPTION (provided by applicant): Extending liquid chromatographic column technology to even higher performance levels has given rise to ultra-high pressure liquid chromatography (UPLC), core-shell particle technology and instrumental developments such as lower volumes for injector and detector hydraulics. In spite of these advances, there is still room for improvement in speed, selectivity and resolution of the liquid chromatographic process. We propose that another level of improvement can be obtained with a change in particle shape by using ellipsoidal particles. These particles offer a reduced pressure drop, a higher mass fraction per unit volume of particles and the possibility to minimize wall effects that are characteristic o packed beds of spherical particles. Furthermore, the possibility of extending this non-spherical particle technology to smaller particle size is important because smaller spherical particles, while offering reduced zone broadening offer larger pressure drops. At some point, the advantage of superficially-porous particle architecture diminishes as particle size is reduced below ≈1.5 µm. If a route to smaller superficially porous non-spherical particles can be devised which minimizes the deleterious pressure drop of spheres, then performance can be increased before the pressure drop causes insurmountable difficulties. New chromatographic particles will be synthesized with a solid ellipsoidal or spherocylinder-like core and then a porous layer will be deposited around the outside for chromatographic retention. We have demonstrated previously in Phase I that there are advantages to this structure with regards to pressure drop and this can be rationalized by bed structures and performance that resemble a monolithic column without the problems of radial inhomogeneity and wall-effect-laden zone broadening that are present in monolithic column technology. We think of the proposed bed structure as that from a "pourable monolith." The current proposal uses synthesis technology and process-scale technology that were discovered and refined during Phase I efforts where it was shown that improved performance can be obtained for larger spherocylinder-like particles that are comparable with smaller spherical particles. In this comparison both the non-spherical and spherical particles used core-shell technology which AMT has pioneered. Phase II will expand on this effort, with the purpose of delivering further improved materials and methods to a broader range of applications in small molecule separations, such as metabolomics, to large molecules, such as proteins, glycoproteins and glycans. The aim here is to not only increase chromatographic resolution, but to make faster separations possible.

描述（由申请人提供）：将液相色谱柱技术扩展到更高的性能水平已经引起了超高压液相色谱（UPLC）、核壳颗粒技术和仪器的发展，例如注射器和检测器液压系统的较小体积。尽管取得了这些进步，但液相色谱过程的速度、选择性和分辨率仍有改进的空间，我们建议通过使用椭球体改变颗粒形状可以获得另一个水平的改进。这些颗粒提供了降低的压降、单位体积颗粒的更高质量分数以及最小化球形颗粒填充床所特有的壁效应的可能性。此外，还可以将这种非球形颗粒技术扩展到更小的尺寸。颗粒尺寸很重要，因为较小的球形颗粒在提供较小的区域展宽的同时会提供较大的压降，在某些时候，当颗粒尺寸减小到小于 1.5 µm 时，表面多孔颗粒结构的优势就会减弱。可以设计非球形颗粒这最大限度地减少了球体的有害压降，然后在压降造成难以克服的困难之前提高性能，将合成具有固体椭圆体或球圆柱状核的新色谱颗粒，然后将形成多孔层。我们之前在第一阶段中已经证明，这种结构在压降方面具有优势，这可以通过类似于整体柱的床结构和性能来合理化，而不会出现径向不均匀性和壁的问题。 -整体柱技术中存在的效应负载区域加宽，我们认为所提出的床结构是“可倾倒整体式”的床结构。第一阶段的工作表明，较大的球柱状颗粒的性能可与较小的球形颗粒相媲美。在本次比较中，非球形和球形颗粒都使用了 AMT 首创的核壳技术。将扩大这一努力，旨在为小分子分离（例如代谢组学）到大分子（例如蛋白质、糖蛋白和聚糖）的更广泛应用提供进一步改进的材料和方法。提高色谱分辨率，但使更快的分离成为可能。