Solid phase microextraction Arrow for the determination of synthetic musk fragrances in fish samples.

A novel solid phase microextraction Arrow (SPME Arrow) system has been applied for the first time to determine synthetic musk fragrances in fish samples. The lack of regulation concerning the concentration of musk fragrances in fish along with the risk associated to these compounds has led to an increased development of analytical methods on this topic. This study applies SPME Arrow followed by gas chromatography coupled to tandem mass spectrometry (ion trap) to determine nine musk fragrances and compares this novel technique with its predecessor (SPME). Parameters such as type of coating, extraction time and temperature as well as water addition were optimized to achieve higher sensitivity. Results show that detection limits ranging between 0.5 ng g-1 (for cashmeran, celestolide, phantolide, tonalide and musk ketone) and 2.5 ng g-1 (dry weight) (for musk xylene) when SPME Arrow is used instead of a conventional fibre, with an up to ten-fold increase in sensitivity. Moreover, commercial fish samples were analysed using the method developed and galaxolideand tonalidewere quantified at concentrations ranging from 6.5 ng g-1 to 17.5 ng g-1 (d.w.) and 2.9 ng g-1 and 5.1 ng g-1 (d.w.) in all the species analysed.