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Fast separations on monolithic silica columns: method transfer, robustness and column ageing for some case studies.
A M van Nederkassel1, A Aerts, A Dierick
1Pharmaceutical and Biomedical Analysis, Pharmaceutical Institute, Vrije Universiteit Brussel, ChemoAC, Laarbeeklaan 103, B-1090 Brussels, Belgium.
Journal of Pharmaceutical and Biomedical Analysis
|May 24, 2003
Summary
High performance liquid chromatography (HPLC) methods successfully transferred to monolithic silica columns, enabling faster separations. Monolithic columns demonstrated robustness and minimal ageing even at high flow rates.
Area of Science:
- Analytical Chemistry
- Chromatography
Background:
- Conventional silica high performance liquid chromatography (HPLC) columns are widely used.
- Monolithic silica columns offer potential advantages in speed and efficiency.
Purpose of the Study:
- To evaluate the transferability of established HPLC methods to monolithic silica columns.
- To assess the performance and robustness of monolithic columns under accelerated conditions.
Main Methods:
- Six separation methods were transferred from conventional HPLC to monolithic silica columns (5 and 10 cm).
- Methods included alkylbenzene mixtures, drug-impurity separations (nimesulide, tetracycline, phenoxymethylpenicillin, erythromycin), and green tea extract analysis.
- Flow rates were increased up to 9 ml/min where feasible.
Main Results:
- Successful transfer was achieved for alkylbenzene and two drug-impurity separations.
- Analysis times were significantly reduced (e.g., 48 s for alkylbenzene, 1.8 min for nimesulide).
- Monolithic columns exhibited robustness, repeatability, and minimal ageing despite high flow rates and mobile phase variations.
Conclusions:
- Monolithic silica columns can successfully accommodate transferred HPLC methods, offering accelerated analysis times.
- These columns maintain performance and stability under demanding conditions, indicating their suitability for rapid chromatographic separations.