Simultaneous determination of polycyclic musks in blood and urine by solid supported liquid–liquid extraction and gas chromatography–tandem mass spectrometry

• The sample preparation time was greatly shorten (∼15 min) by SLE compared with present methods in literature.
• The sensitivity and selectivity were improved and analytical time was shortened by employing gas chromatography–tandem mass spectrometry (GC–MS/MS).
• The developed method was proved to be rapid, precise and accurate.
• The developed method has potential for high-throughput analysis of PCMs in biological fluids for health impact assessment.

A rapid, precise and accurate method for the simultaneous determination of 5 polycyclic musks (PCMs) in biological fluids was developed by solid supported liquid–liquid extraction (SLE) coupled with gas chromatography–tandem mass spectrometry (GC–MS/MS). All parameters influencing SLE-GC–MS performance, including electron energy of electron-impact ionization source, collision energy for tandem mass spectrometer when operated in selected-reaction monitoring (SRM) mode, type and volume of elution reagent, nitrogen evaporation time, pH and salinity of sample have been carefully optimized. Eight milliliter of n-hexane was finally chosen as elution reagent. Blood and urine sample could be loaded into SLE cartridge without adjusting pH and salinity. Deuterated tonalide (AHTN-d3) was chosen as internal standard. The correlation coefficient (r2) of the calibration curves of target compounds ranged from 0.9996 to 0.9998. The dynamic range spanned over two orders of magnitude. The limit of detection (LOD) of target compounds in blood and urine ranged from 0.008 to 0.105 μg L−1 and 0.005 to 0.075 μg L−1, respectively. The developed procedure was successfully applied to the analysis of PCMs in human blood and urine obtaining satisfying recoveries on low, medium and high levels. The method was compared with SLE-GC–MS and shown one to two orders of magnitude improvement in sensitivity.