Characterization of hydroxypropylmethylcellulose (HPMC) using comprehensive two-dimensional liquid chromatography
Andreas Greiderer1, Linda Steeneken, Tom Aalbers
1Van't Hoff Institute for Molecular Sciences, Faculty of Science, University of Amsterdam, Science Park 904, 1098 XH Amsterdam, The Netherlands.
Journal of Chromatography. A
|July 23, 2011
Summary
This study characterizes hydroxyl-propylmethylcellulose (HPMC) polymers using advanced two-dimensional liquid chromatography (LC×LC). Temperature-dependent thermal gelation provides unique insights into HPMC composition and properties.
Area of Science:
- Polymer Chemistry
- Analytical Chemistry
- Chromatography
Background:
- Hydroxyl-propylmethylcellulose (HPMC) is a versatile polymer with applications in various industries.
- Characterizing HPMC's complex size and compositional distributions is crucial for understanding its properties.
- Existing methods may not fully resolve the intricate details of HPMC polymer structures.
Purpose of the Study:
- To develop and apply a comprehensive two-dimensional liquid chromatography (LC×LC) method for detailed HPMC characterization.
- To investigate the influence of temperature on HPMC retention behavior and thermal gelation.
- To correlate chromatographic observations with inherent polymer properties like cloud point.
Main Methods:
- Utilized comprehensive two-dimensional liquid chromatography (LC×LC) combining reversed-phase (RP) and aqueous size-exclusion chromatography (aq-SEC).
- Employed a two-position ten-port switching valve for seamless LC×LC system integration.
- Employed charged aerosol detection (CAD) for sensitive HPMC detection and Matlab for data analysis.
- Investigated the impact of column temperature control on HPMC separation and thermal gelation.
Main Results:
- Successfully separated and characterized HPMC polymers based on size and compositional distributions (methoxyl and hydroxyl-propoxyl substitution).
- Demonstrated the significant influence of temperature on HPMC retention, enabling monitoring of thermal gelation.
- Established a correlation between the temperature of half-gelation and the polymer's cloud-point temperature.
- Showcased temperature-responsive LC×LC as a powerful tool for distinguishing modified cellulose properties.
Conclusions:
- LC×LC, particularly with temperature control, offers a powerful approach for detailed HPMC polymer analysis.
- Thermal gelation phenomenon provides specific compositional information and can be monitored chromatographically.
- The method allows for the characterization of inherent cloud points, adding a new dimension to HPMC analysis.
- This technique enhances the ability to differentiate and understand modified cellulose polymers.
More Related Videos
07:502D-HPLC-MS Technology Combined with Molecular Network for the Identification of Components in Tibetan Medicine Aconitum pendulum
Published on: December 8, 2023
11:09An HS-MRM Assay for the Quantification of Host-cell Proteins in Protein Biopharmaceuticals by Liquid Chromatography Ion Mobility QTOF Mass Spectrometry
Published on: April 17, 2018
Related Concept Videos
01:11High-Performance Liquid Chromatography: Introduction
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:
00:57High-Performance Liquid Chromatography: Instrumentation
High-performance liquid chromatography, or HPLC, is an analytical technique that separates liquid samples under high pressures. An HPLC instrument consists of glass bottles for storing solvents called mobile phase reservoirs. HPLC-grade solvents are used to maintain high purity, and the dissolved gases are removed using a degasser, such as a vacuum pumping system or sparging with helium. The solvents are then pumped into the analytical column using a screw-driven syringe or reciprocating pumps.
01:05High-Performance Liquid Chromatography: Elution Process
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...
01:15High-Performance Liquid Chromatography: Types of Detectors
The role of the detectors in High-Performance Liquid Chromatography (HPLC) is to analyze the solutes as they exit from the chromatographic column. The detector recognizes the solute's property and generates corresponding electrical signals, which are converted into a readable graph of the detector's response versus elution time called a chromatogram at the computer. There are several types of HPLC detectors, each with its own advantages and limitations, depending on the analyte properties and...
01:18Supercritical Fluid Chromatography
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,...
01:192D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)
Heteronuclear single-quantum correlation spectroscopy (HSQC) is a 2D NMR technique that reveals one-bond correlations between hydrogen and a heteronucleus. The HSQC experiment is similar to the heteronuclear correlation experiment (HETCOR) but is more sensitive. In the HSQC spectrum, the proton chemical shift is plotted on the horizontal F2 axis, while the 13C chemical shift is plotted on the vertical F1 axis. The corresponding proton and 13C spectra are also shown. The HSQC contour plot does...