Covalently Bonded HILIC Stationary Phases on Superficially Porous Particles

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Solution Overview

Problem

Conventional HILIC columns using unmodified silica as packing material face instability and poor separation efficiency due to silica dissolution in water-based mobile phases, leading to inconsistent retention times and reduced performance in high-pressure liquid chromatography (HPLC) applications.

Innovation Solution

Development of hydrolytically stable, covalently bonded HILIC stationary phases using native and derivatized cyclofructans, cyclodextrins, macrocyclic antibiotics, and zwitterionic selectors bonded to superficially porous particles (SPPs), which provide enhanced stability and selectivity, and are produced in a range of particle diameters to optimize chromatographic performance.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of manufacture

If unmodified silica is used as packing material in HILIC columns, then the column structure is simple and easy to manufacture, but the column exhibits poor stability due to silica dissolution in water-based mobile phases

Engineering Contradiction:
Improveease of manufactureVSAvoidstability
Core Design Contradiction:
Ease of manufactureVSReliability

Solution Approach 1:

The patent applies composite materials by combining silica core with hydrolytically stable shell materials (such as polymeric coatings or inorganic overlays) to create a core-shell structured packing material. This composite structure maintains the simplicity of silica manufacturing while adding an outer layer that resists dissolution in water-based mobile phases, thereby improving column stability without significantly complicating the manufacturing process.

Inventive Principle:
Principle #40Composite materials

Solution Approach 2:

The patent utilizes porous materials by incorporating a porous shell layer around the silica core. This porous structure provides high surface area for stationary phase coating while maintaining structural integrity in aqueous environments. The porous shell acts as a protective barrier that prevents silica dissolution while allowing analyte access to the stationary phase, thus improving reliability without sacrificing ease of manufacture.

Inventive Principle:
Principle #31Porous materials

2Ease of operation

If conventional HILIC columns are used with aqueous mobile phases, then the operation is simple, but the separation efficiency deteriorates due to inconsistent retention times caused by silica dissolution

Engineering Contradiction:
Improveease of operationVSAvoidseparation efficiency
Core Design Contradiction:
Ease of operationVSManufacturing precision

Solution Approach 1:

The composite core-shell structure with hydrolytically stable shell material ensures consistent retention times by preventing silica dissolution in aqueous mobile phases. This maintains the simplicity of operation while dramatically improving separation efficiency through stable and reproducible chromatographic behavior.

Inventive Principle:
Principle #40Composite materials

Solution Approach 2:

The patent changes the chemical composition parameters of the column packing material by introducing hydrolytically stable shell materials with controlled pore sizes and surface chemistries. This parameter change enables the column to maintain consistent performance in aqueous mobile phases, improving separation efficiency without complicating the ease of operation.

Inventive Principle:
Principle #35Parameter changes

3Productivity

If high flow rates are used in HPLC applications, then the productivity increases, but the performance deteriorates due to poor mass transfer in conventional columns

Engineering Contradiction:
ImproveproductivityVSAvoidchromatographic performance
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The patent employs porous shell materials with optimized pore size distributions that facilitate rapid mass transfer of analytes. The porous structure provides short diffusion paths and high surface area, enabling efficient analyte-stationary phase interactions even at high flow rates. This maintains high chromatographic performance while achieving increased productivity through faster analysis times.

Inventive Principle:
Principle #31Porous materials

Solution Approach 2:

The patent applies local quality by creating a porous shell layer with specific pore size and surface properties optimized for mass transfer. This localized structural modification at the particle surface enhances analyte access and binding efficiency, allowing high flow rates to be used without sacrificing chromatographic performance, thus improving productivity.

Inventive Principle:
Principle #3Local quality

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

The new HILIC columns exhibit higher efficiency and shorter retention times compared to fully porous particle columns, maintaining stability and selectivity even under high flow rates and aqueous mobile phases, thereby improving the overall performance of HPLC separations.

Implementation Method 1

High efficiency, ultra-stable, bonded hydrophilic interaction chromatography (HILIC) matrix on superficially porous particles (SPPs)

Methodology Applied
Scientific EffectHydrophilic interaction chromatography (HILIC): Chromatography

Implementation Method 2

hydrolytically stable, covalently bonded HILIC stationary phases

Methodology Applied
Scientific EffectCovalent bonding: Chemical Bonding

Data Source

PatentUS10265643B2High efficiency, ultra-stable, bonded hydrophilic interaction chromatography (HILIC) matrix on superficially porous particles (SPPS)
Publication Date: 2019.04.23 AZYP LLC
  • US10265643B2 patent drawing
  • US10265643B2 patent drawing
  • US10265643B2 patent drawing

AI summary

The present invention relates to superficially porous particles (SPPs), also called core-shell, porous shell or fused core particles, which are state-of-the-art support materials used in the production of HPLC columns. Hydrolytically stable, highly selective superficially porous particle (SPP) hydrophilic interaction liquid chromatographic (HILIC) stationary phases having higher efficiencies and shorter retention times than analogous stationary phases on fully porous particles (FPP) is provided.