Multiple headspace solid-phase microextraction after matrix modification for avoiding matrix effect in the...

Area of Science:

• Analytical Chemistry
• Food Safety Analysis

Background:

• Solid-phase microextraction (SPME) is widely used for analyte quantification.
• Traditional SPME methods can suffer from matrix effects and incomplete analyte recovery.
• Quantifying contaminants in solid food matrices presents unique challenges.

Purpose of the Study:

• To develop and validate a multiple headspace solid-phase microextraction (HS-SPME) method for ethyl carbamate (EC) determination in bread.
• To address and overcome the challenge of water adsorption in fresh bread samples affecting EC quantification.
• To introduce a novel, high-performance extraction fiber for improved analytical performance.

Main Methods:

• Utilized multiple HS-SPME coupled with gas chromatography-flame ionization detection (GC-FID).
• Developed and tested a novel polyethylene glycol/hydroxy-terminated silicone oil fiber.
• Incorporated anhydrous sodium sulphate to mitigate water adsorption interference.

Main Results:

• The developed method demonstrated excellent linearity (0.15-1500 μg g⁻¹), precision (1.6%), and a low limit of detection (0.041 μg g⁻¹).
• Achieved high recovery rates (92.5–103.4%) across different spiking levels.
• Successfully applied the method to analyze 14 real bread samples.

Conclusions:

• Multiple HS-SPME provides complete analyte recovery, effectively eliminating matrix effects.
• The novel fiber and anhydrous sodium sulphate addition successfully resolved water adsorption issues in bread analysis.
• This validated method offers a cost-effective, time-efficient, and reliable approach for analyzing multiple solid samples.