Technology Forum: Sample Prep

It has been said that the foundation of all chromatographic research can be found in the sample preparation. An assay can be doomed before it starts if not prepared properly, while conversely, the new solvents and techniques being developed today can lead to better, more accurate results.

This month, Chromatography Online's Technology Forum looks at the topic of Sample Prep and the trends and issues surrounding it. Joining us for this discussion is Dennis D. Blevins, Ph.D., of Agilent Technologies, Inc., Elena Gairloch of Biotage, and Jeffrey Zonderman of Thermo Fisher Scientific.

What trends do you see emerging in Sample Prep?

Blevins: I see processing smaller samples using reduced solvent volumes, simplifying rugged methods, and making environmentally conscious solvent choices as emerging trends in sample prep.

Gairloch:Trends for sample prep are being driven largely by the need to balance cost and results. In some areas, low-cost protein precipitation or dilution is adequate to obtain desired results. However, the drive to eliminate ion-suppression and ion-enhancement requires more effective sample clean-up, which is achieved by techniques such as supported liquid extraction (SLE) and solid phase extraction (SPE).

Great advances have been made recently in the production of SLE plates, which can provide reliable and rugged performance from well-to-well. Supported liquid extraction is cost-effective, offers easy method development, and often results in extremely clean samples for mass spec.

Recent trends in SPE include the use of mixed-mode, polymer-based materials to achieve the high levels of selectivity and extract cleanliness needed from today's applications.

Zonderman: The trend I see is that labs are looking to remove the sample prep steps. Many times, SPE and SFC do not work well to clean up the biological sample for very complicated matrixes. For many matrices, chemists have to move to liquid-liquid solvent extractions. Second, the market is moving to online sample prep in an attempt to automate the process by integrating with the mass spec detector.Lastly, the need to reduce the overall cost associated with sample prep - labor and material - is a driving factor.

What is the future of Sample Prep?

Blevins: The future of sample prep lies in additional multiplex sample processing tools- past 96-well plates and pipette tips and increased sensitivity to contamination issues - instrument lower detection limits.

Gairloch:The future of sample prep will follow the future of the LC-MS systems currently being developed. Lately we have seen a greater utilization of smaller ID columns. This increases the demand for sample clean-up to prevent column and system plugging.

What is the Sample Prep application that you see growing the fastest?

Blevins: Additional rapid broad spectrum methods targeting food industries are growing the fastest right now.

Gairloch:The fastest growing application right now is Vitamin D analysis and MethyMalonic Acid.

Zonderman:I see the applied markets like food safety and clinical applications growing the fastest.

What obstacles stand in the way of Sample Prep development?

Blevins: Two obstacles that stand in the way of sample prep development are inadequate training of extraction technicians and resistance to market acceptance to new extraction methods.

Gairloch:The biggest obstacle in sample prep is the balance of cost and performance.

Zonderman:The fact that these sample prep technologies do not meet the future requirements of the customer is the biggest obstacle to their development.

What was the biggest accomplishment or news item during the past year for Sample Prep?

Blevins: The expansion of Quechers applications was the biggest accomplishment.

Gairloch:The biggest announcement in the last year has been the availability of a rugged 96-well SLE plate.