One-step microwave-assisted headspace solid-phase microextraction for the rapid determination of synthetic polycyclic musks in oyster by gas chromatography–mass spectrometry

A rapid, simple and solvent-free procedure was developed for the determination of synthetic polycyclic musks in oyster samples by using one-step microwave-assisted headspace solid-phase microextraction (MA-HS-SPME) and gas chromatography–mass spectrometry (GC–MS). Two commonly used synthetic polycyclic musks, galaxolide (HHCB) and tonalide (AHTN), were selected in the method development and validation. The parameters (microwave irradiation power, extraction time, amount of water added, pH value and addition of NaCl) affecting the extraction efficiency of analytes from oyster slurry were systematically investigated and optimised. The best extraction conditions were achieved when the oyster tissue mixed with 10-mL deionised water (containing 3 g of NaCl in a 40-mL sample-vial) was microwave irradiated at 80 W for 5 min. The limit of quantification (LOQ) was 0.1 ng/g in 5-g of wet tissue. The good precision and accuracy of one-step MA-HS-SPME coupled with GC–MS for the determination of trace level of AHTN in oyster samples was also demonstrated.