Cleanup and Separation

Sample extracts often contain impurities that can interfere with subsequent analytical measurements. Cleanup procedures are therefore employed to separate and isolate the analyte of interest from other matrix components prior to analysis. Common techniques used include liquid-liquid partitioning, solid-phase extraction, precipitation, electrophoretic separations, and chromatography. Efficient cleanup ensures pure analyte fractions with minimal interferents are presented to analytical instruments.

Concentration and Volume Adjustment

Depending on analyte concentration levels in the original sample Sample Preparation and detection limits of the specific analytical instrument, it may be necessary to concentrate the extracts or dilute them to fall within the calibrant range. Solvent exchange with evaporation, freeze-drying, or dilution are standard volume adjustment techniques. Care must be taken to avoid analyte loss during these processes. Internal standards can monitor method performance across extractions of varying sample amounts.

Derivatization

Certain analytes may require chemical modification via derivatization prior to analysis to improve volatility, chromophore development, stability, or ionization efficiencies as required by the analytical methodology. Derivatization conditions with regards to reagents, temperature, time etc. need to be optimized to achieve consistent and quantitative conversions. Unreacted reagents should be removed before analysis.

Automation and Miniaturization

Manual sample preparation methods are laborious, time-consuming, and prone to human errors affecting accuracy and precision. Automated liquid handling workstations can conduct multi-step sample preparations on a much larger scale with improved reproducibility compared to manual processing. Miniaturized microfluidic sample preparation systems further increase portability, speed, and throughput while reducing sample and reagent volumes. Automation standards validation becomes necessary.

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