Straightforward SPE Method Development: Avoiding Common Pitfalls with a Simple Approach

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Ziling Lu, Diane M. Diehl, Claude Mallet, Jeffrey R. Mazzeo [Waters]
Pittcon 2004
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SPE Format:
Oasis HLB 96-well Plate Oasis MCX 96-well Plate Oasis MAX 96-well Plate Oasis WCX 96-well Plate
Valethamate, Protriptyline
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In today’s highly competitive chemical markets, high sample throughput has become the norm. Faster analyses require a high level of automation and fast method development. And, as formulations become more potent, additional emphasis has been directed on sample preparation for sub ng/mL levels of components. Classical extraction techniques, such as liquid-liquid extraction (LLE) or protein precipitation (PPT), are not often suitable procedures for high throughput. More importantly, the extracts from LLE and PPT are often not clean enough to be able to achieve the low limits of detection now required. Therefore, solid phase extraction (SPE) has become the sample preparation tool of choice. However, many chemists feel that SPE method development is too time consuming or too difficult. To address these issues, we took a systematic approach to SPE method development and outlined all the steps including sample pretreatment, sample solubility, SPE sorbents, wash steps and solvents, elution solvents, calculation of recovery and method reproducibility. We used a variety of sample probes to cover acids, bases and neutrals, as well as the range from polar to nonpolar analytes. We used a variety of sorbents in the 96-well plate format and LC/MS/MS for analysis at ng/mL levels. In this presentation, we outline all the important steps for SPE method development, highlighting the pitfalls and how to avoid them. Based on these data, we then outline a straightforward approach to SPE method development.

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