Fast and sensitive method to determine chloroanisoles in cork using an internally cooled solid-phase microextraction...

Area of Science:

• Analytical Chemistry
• Environmental Science
• Food Science

Background:

• Chlorinated anisoles are significant contaminants in cork, impacting food and beverage quality.
• Traditional methods for analyzing these compounds can be time-consuming and lack sensitivity.
• Solid-phase microextraction (SPME) offers a solvent-free approach for sample analysis.

Purpose of the Study:

• To evaluate a new internally cooled solid-phase microextraction (CF-SPME) fiber for determining chlorinated anisoles in cork.
• To compare the performance of CF-SPME with conventional headspace SPME (HS-SPME).
• To optimize extraction conditions for both methods using statistical designs.

Main Methods:

• Utilized an internally cooled SPME fiber (cold fiber) and a commercial polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber for headspace SPME (HS-SPME).
• Coupled both SPME techniques to gas chromatography-time-of-flight mass spectrometry (GC-TOF-MS) for analysis.
• Optimized extraction parameters including incubation time, extraction time, and temperatures using full factorial design and Doehlert matrix.

Main Results:

• Optimized CF-HS-SPME conditions: 10 min incubation, 10 min extraction, 130°C sample, 10°C fiber.
• Optimized HS-SPME conditions: 10 min incubation, 75 min extraction, 85°C sample, 8 ml water, 500 rpm agitation.
• CF-HS-SPME achieved lower quantification limits (0.8–1.6 ng g⁻¹) compared to HS-SPME (4–6 ng g⁻¹).
• CF-HS-SPME demonstrated potential as a non-destructive method with minor modifications.

Conclusions:

• The internally cooled SPME fiber offers a more sensitive and efficient method for analyzing chlorinated anisoles in cork.
• CF-SPME provides significantly lower detection limits than conventional HS-SPME.
• This advanced SPME technique holds promise for improved quality control in cork production and related industries.