A Microwave‐assisted Headspace Solid‐phase Microextraction for Rapid Determination of Synthetic Polycyclic and Nitro‐aromatic Musks in Fish Samples

Rapid solvent‐free microwave‐assisted headspace solid‐phase microextraction (MA‐HS‐SPME) coupled with gas chromatography‐mass spectrometry (GC‐MS) was developed to determine synthetic polycyclic and nitro‐aromatic musks in fish samples. Four commonly used synthetic musks, galaxolide (HHCB), tonalide (AHTN), musk xylene (MX) and musk ketone (MK) were employed in the method development and validation. The parameters (microwave irradiation time, irradiation power, amount of water addition, pH value and addition of NaCl) affecting the extraction efficiency of analytes from fish slurry were systematically investigated and optimized. The best extraction conditions were achieved when the fish sample 2‐g mixed with 4‐mL methanol and 15‐mL deionized water (containing 4 g of NaCl, pH 2.0 in a 40‐mL sample‐vial) was microwave irradiated at 80 watt for 5 min. The limits of quantification (LOQ) were 0.4 to 1.2 ng/g in 2‐g of wet tissue. The precision for these analytes, as indicated by relative standard deviations, were less than 9% for both intra‐ and inter‐day analysis. Accuracy, expressed as the mean extraction recovery, was between 80 to 92%. A standard addition method was used to quantitate these four synthetic musks, and the total concentrations ranged from 2.1 to 23.1 ng/g in various fish samples.