Monolithic silica column for in-tube solid-phase microextraction coupled to high-performance liquid chromatography

Area of Science:

• Analytical Chemistry
• Separation Science

Background:

• In-tube solid-phase microextraction (SPME) coupled with capillary liquid chromatography (LC) has been automated.
• Conventional open tubular capillary columns with thick polymer films limit mass transfer efficiency in SPME due to insufficient surface area to volume ratio.

Purpose of the Study:

• To develop a highly efficient SPME column for improved in-tube SPME performance.
• To introduce and evaluate a novel C18-bonded monolithic capillary column for in-tube SPME applications.

Main Methods:

• Fabrication of a C18-bonded monolithic capillary column with a double-pore structure (through-pore and meso-pore).
• Optimization of pore structure for in-tube SPME.
• Connection of the optimized column to an HPLC injection valve for characterization.

Main Results:

• The C18-bonded monolithic capillary column demonstrated excellent pre-concentration efficiency.
• The optimized column significantly improved upon conventional in-tube SPME methods.
• The novel system proved effective, satisfactory, and suitable for SPME.

Conclusions:

• A C18-bonded monolithic capillary column is highly effective for in-tube SPME.
• The double-pore structure optimization is crucial for enhanced mass transfer.
• This novel approach offers a superior method for sample introduction and concentration in SPME.