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Related Concept Videos

Size-Exclusion Chromatography01:08

Size-Exclusion Chromatography

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In size-exclusion chromatography (SEC), also known as molecular-exclusion or gel-permeation chromatography, molecules are separated based on their sizes. This technique is important for separating large molecules such as polymers and biomolecules. The two classes of micron-sized stationary phases encountered in SEC are silica particles and cross-linked polymer resin beads. Both materials are porous, but their pore sizes vary significantly.
Silica particles offer advantages such as rigidity,...
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Related Experiment Video

Updated: Apr 6, 2026

Preparation and Characterization of Nanoliposomes for the Entrapment of Bioactive Hydrophilic Globular Proteins
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Solid Phase Extraction as an Innovative Separation Method for Measuring Free and Entrapped Drug in Lipid

Alexis Guillot1,2,3, Anne-Claude Couffin4,5, Xavier Sejean4,5

  • 1PHAST GmbH, Kardinal-Wendel-Str. 16, D-66424, Homburg, Germany. alexis.guillot@phast.com.

Pharmaceutical Research
|July 24, 2015
PubMed
Summary

Solid Phase Extraction (SPE) offers a validated method for quantifying free and entrapped drugs in nanopharmaceuticals. This technique revealed limited shelf-life for lipid nanoparticles, highlighting its value in quality control.

Keywords:
cyclosporinelipid nanoemulsionnanoparticlesseparation techniquessolid-phase extraction

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Area of Science:

  • Pharmaceutical Sciences
  • Analytical Chemistry
  • Nanotechnology

Background:

  • Characterizing nanopharmaceuticals often focuses on physical properties like size and shape.
  • Quantifying drug encapsulation efficiency (free vs. entrapped drug) in nanocarriers is analytically challenging for routine use.

Purpose of the Study:

  • To investigate Solid Phase Extraction (SPE) as a viable technique for quantifying free and entrapped drugs in nanopharmaceutical formulations.
  • To overcome the limitations of existing methods for drug quantification in nanomedicines.

Main Methods:

  • Developed and validated a Solid Phase Extraction (SPE) protocol coupled with High Performance Liquid Chromatography (HPLC) for drug quantification.
  • Applied the validated SPE-HPLC method to characterize cyclosporine A-loaded lipid nanoparticles (LNPs).
  • Assessed colloidal stability of LNPs using Dynamic Light Scattering (DLS).

Main Results:

  • The SPE-HPLC method demonstrated excellent linearity, repeatability, accuracy, and specificity for quantifying free, entrapped, and total drug.
  • Analysis revealed a limited shelf-life for the lipid nanoparticles when stored in aqueous buffer, particularly at elevated temperatures.
  • Dynamic Light Scattering confirmed nanoparticle stability within the concentration range used during SPE analysis.

Conclusions:

  • Validated Solid Phase Extraction (SPE) is a powerful and transferable analytical tool for drug development and quality control of lipid-based nanopharmaceuticals.
  • The findings underscore the importance of stability assessment for nanopharmaceutical formulations.
  • SPE facilitates robust characterization crucial for industrial nanomedicine applications.