Experimental designs for solid-phase microextraction method development in bioanalysis: A review.

Area of Science:

• Analytical Chemistry
• Method Development

Background:

• Bioanalytical method development relies on robust experimental design.
• Solid-phase microextraction (SPME) is a key technique in bioanalysis.
• Previous reviews highlighted specific trends in experimental design for SPME.

Purpose of the Study:

• To provide an updated review of experimental design strategies in bioanalytical SPME method development.
• To critically analyze the characteristics and application of different SPME approaches.
• To identify trends and gaps in the use of design of experiments (DoE) from 2009 to 2019.

Main Methods:

• Comprehensive literature search of publications from 2009 to 2019.
• Analysis of experimental designs employed in bioanalytical SPME method development.
• Critical discussion of different SPME approaches and their associated designs.

Main Results:

• Two-level full factorial designs (fewer than 5 factors) are most common for initial screening.
• Rotatable central composite and Box-Behnken designs are popular for response surface methodology.
• Advanced designs like definitive screening and D-Optimal designs were not reported.
• Heavy reliance on commercial software for experimental design, analysis, and reporting was observed.

Conclusions:

• The development of bioanalytical SPME methods predominantly utilizes simpler experimental designs.
• There is a notable underutilization of more complex and efficient design of experiments (DoE) methodologies.
• Future research could benefit from exploring and implementing advanced DoE strategies for optimizing SPME methods.