Related Experiment Video
Updated: Jul 16, 2025
06:44
Curtain Flow Column: Optimization of Efficiency and Sensitivity
Published on: June 12, 2016
6.6K
Analytical and preparative chiral supercritical fluid chromatography resolutions using crown ether-derived column
Lei Yue1, Larry Miller2, John Reilly3
1Novartis Institutes for BioMedical Research, Cambridge, Massachusetts, USA.
Chirality
|September 22, 2023
Summary
Crownpak® CR-I (+) columns show superior chiral separation of primary amines using supercritical fluid chromatography (SFC). Adding water enhances peak shape, enabling preparative separations for pharmaceutical applications.
Area of Science:
- Analytical Chemistry
- Chromatography
- Organic Chemistry
Background:
- Chiral separation of primary amines is crucial in pharmaceutical development.
- Supercritical Fluid Chromatography (SFC) offers an efficient separation technique.
- Evaluating novel stationary phases is essential for improving chiral resolution.
Purpose of the Study:
- To evaluate the efficacy of crown ether-derived Crownpak® CR-I (+) columns for chiral separation of primary amines.
- To compare its performance against immobilized polysaccharide-based columns.
- To establish conditions for optimal separation and preparative scale-up.
Main Methods:
- SFC analysis of 12 primary amines using Crownpak® CR-I (+) columns.
- Comparative analysis with eight immobilized polysaccharide-based columns.
- Optimization of mobile phase composition, including water addition.
Main Results:
- Crownpak® CR-I (+) demonstrated a significantly higher success rate in chiral separation compared to polysaccharide columns.
- Addition of 5% water to the mobile phase dramatically improved peak shape for primary amine separations.
- Successful demonstration of the first preparative SFC separations using Crownpak® CR-I (+).
Conclusions:
- Crownpak® CR-I (+) is a highly effective column for the chiral separation of primary amines via SFC.
- Optimized conditions, including water addition, facilitate improved peak shape and preparative resolution.
- This column provides a valuable tool for resolving challenging chiral compounds in the pharmaceutical industry.
Related Concept Videos
01:18Supercritical Fluid Chromatography
275
Supercritical fluid chromatography (SFC) provides a beneficial substitute for gas chromatography (GC) and liquid chromatography (LC) for certain samples because it merges the top attributes of both techniques. SFC allows the separation and analysis of compounds that GC or LC does not easily manage. These compounds are traditionally nonvolatile or thermally unstable, making GC unsuitable and lacking functional groups required for HPLC analysis.
SFC utilizes a supercritical fluid mobile phase,...
SFC utilizes a supercritical fluid mobile phase,...
275
01:13Principles Of Column Chromatography
6.9K
The chromatography technique was first invented in 1901 by Michael S. Tswett, a Russian botanist, to separate plant pigments using organic solvents. Further, in 1941, Archer John Porter Martin and R. L. M. Synge modified the technique by packing silica gel into a column. A mixture of amino acids was then separated on the packed column using chloroform and water mixture as the mobile phase. This was the first report on column chromatography. At present, column chromatography is a widely used...
6.9K
02:36Crown Ethers
5.3K
Crown ethers are cyclic polyethers that contain multiple oxygen atoms, usually arranged in a regular pattern. The first crown ether was synthesized by Charles Pederson while working at DuPont in 1967. For this work, Pedersen was co-awarded the 1987 Nobel Prize in Chemistry. Crown ethers are named using the formula x-crown-y, where x is the total number of atoms in the ring and y is the number of ether oxygen atoms. The term 'crown' refers to the crown-like shape that these ether...
5.3K
01:11High-Performance Liquid Chromatography: Introduction
2.1K
High-performance liquid chromatography(HPLC), formerly referred to as High-pressure liquid chromatography, is a powerful technique used to separate, identify, and quantify components in complex mixtures. The term "high pressure" refers to using high pressure to push the liquid mobile phase through the tightly packed columns.
In HPLC, two phases play a critical role in the separation process:
In HPLC, two phases play a critical role in the separation process:
2.1K
01:05High-Performance Liquid Chromatography: Elution Process
528
In High-Performance Liquid Chromatography (HPLC), the elution process is critical to the separation of analytes and the quality of chromatographic results. Elution describes how compounds move through the column and separate based on their interactions with the mobile and stationary phases. This process determines the resolution, peak shape, and retention times in the chromatogram, which are essential for identifying and quantifying components in complex mixtures. Understanding the elution...
528
01:10Silica Gel Column Chromatography: Overview
1.3K
Silica gel column chromatography is a technique for separating compounds using a column packed with silica gel as the stationary phase. This method relies on differences in the polarity of compounds. Based on their polarities, compounds move between the stationary phase (silica gel) and the mobile phase (the solvent), forming discrete bands in the column.
Polar components tend to bind strongly to the silica gel, causing them to move slowly through the column. In contrast, nonpolar compounds...
Polar components tend to bind strongly to the silica gel, causing them to move slowly through the column. In contrast, nonpolar compounds...
1.3K