Optimization and Evaluation of an Automated Generic Solid Phase Extraction
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Authors
Farrell, Paige E.
Issue Date
2001
Type
Thesis
Language
en_US
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Abstract
Sample preparation and analysis are necessary at every stage of the drug development process. Solid phase extraction (SPE) is a common sample clean up technique used in the pharmaceutical industry. Mass spectrometry is often used to analyze samples for identification of unknowns or quantification of known compounds. The efficiency of these processes is greatly dependent on time limitations. The use of generic processes and automated procedures is becoming more widespread as a means to increase throughput and efficiency.
The purpose of this experiment was to optimize and evaluate the extraction process through the automation of a generic solid phase extraction. In order to test the method, seven compounds of varying structure were assayed with this experiment and the extracts were analyzed using liquid-chromatography/mass spectrometry.
A successful extraction experiment would allow for a wash solution that would remove impurities and an eluting solution that would efficiently remove the drug from the column. The automation of the solid phase extraction experiment greatly increased time efficiency. However, the effectiveness of the completely generic SPE with Waters Oasis hydrophilic-lipophilic balanced (HLB) plates was not as high. The success of the experiment decreased dramatically when samples were prepared in plasma as opposed to saline. Only one of seven compounds showed an optimal wash and elution solution. The others could not be successfully extracted using the HLB extraction plate. The interactions of the plasma salts and proteins play a critical role in the efficiency of the SPE-columns, explaining some of the differences encountered between saline and plasma. However, new generic approaches are recently becoming available. It is likely that these techniques along with automated procedures will continue to gain popularity in many areas of laboratory research.
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