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Development of a solid phase extraction method for simultaneous determination of corticoids and tranquilizers in
M Carmen Quintana1, Lourdes Ramos, M Jose González
1Departamento de Química Analítica y Análisis Instrumental, Facultad de Ciencias, Universidad Autónoma de Madrid, Cantoblanco 28049, Madrid, Spain.
Journal of Separation Science
|September 1, 2004
Summary
A new solid phase extraction (SPE) method efficiently isolates phenothiazines and glucocorticoids from serum. This technique simplifies analysis using high-performance liquid chromatography (HPLC) with UV-Vis detection.
Area of Science:
- Analytical Chemistry
- Pharmacology
Background:
- Accurate quantification of phenothiazines and glucocorticoids in biological matrices is crucial for therapeutic drug monitoring and pharmacokinetic studies.
- Existing methods for sample preparation can be time-consuming and complex, potentially affecting analyte stability and recovery.
Purpose of the Study:
- To develop a simple, fast, and efficient solid phase extraction (SPE) method for the simultaneous preconcentration and clean-up of phenothiazines and glucocorticoids from human serum.
- To enable direct analysis of the extracted fractions using high-performance liquid chromatography with UV-Vis detection.
Main Methods:
- Development of a solid phase extraction (SPE) protocol for serum sample preparation.
- Separate elution of phenothiazine and glucocorticoid fractions.
- Analysis of eluted fractions using high-performance liquid chromatography with UV-Vis detection (HPLC-UV/Vis).
- Confirmation of results using liquid chromatography-mass spectrometry (LC-MS).
Main Results:
- The developed SPE method achieved satisfactory preconcentration and clean-up for both drug classes.
- High-performance liquid chromatography with UV-Vis detection allowed direct analysis without further sample treatment.
- Overall recoveries ranged from 64-85% for most analytes, with phenylbutazone at 20%.
- Repeatability, assessed by relative standard deviation, was generally below 12%.
Conclusions:
- The developed SPE method offers a robust and efficient approach for the simultaneous analysis of phenothiazines and glucocorticoids in serum.
- This method simplifies sample preparation, reduces analysis time, and provides reliable results for clinical and research applications.
- Further optimization may be needed for specific analytes like phenylbutazone to improve recovery rates.