Comparison of Sample Preparation and Detection Methods for the Quantification of Synthetic Musk Compounds (SMCs) in Carp Fish Samples

Abstract

This study deals with the separation and detection methods for 12 synthetic musk compounds (SMCs), which are some of the emerging contaminants in fish samples, are widely present in environmental media, and can be considered serious risks due to their harmful effects. For the separation of co-extracted substances and the target SMCs in fish samples after ultrasonic extraction, four solid-phase extraction (SPE) sorbents were investigated. The recoveries of SMCs from 10 mL of eluent, as optimized by the elution profile, were within the acceptable range of 80–120% in all SPE types, and it was found that nitro musk and polycyclic musk compounds were separated more clearly in Florisil SPE than others (Aminopropyl, Alumina-N, PSA). Furthermore, the results of measuring the matrix effects by each SPE through the spiking experiments showed that Florisil SPE was superior. The comparison of a gas chromatograph-single quadrupole mass spectrometer (GC-SQ/MS) with selected ion monitoring (SIM) mode and GC-triple quadrupole mass spectrometer (GC-QqQ-MS/MS) with multiple reaction monitoring (MRM) modes regarding the detection method of SMCs showed that the method detection limits (MDLs) of SMCs were on average ten times lower when GC-QqQ-MS/MS with MRM mode was used. The differences between the two methods can provide essential information for selecting an analytical method in related research fields that require appropriate detection levels, such as risk assessment or pollution control.

Keywords

• synthetic musk compounds (SMCs)
• solid-phase extraction (SPE) cleanup
• gas chromatograph-single quadrupole mass spectrometer (GC-SQ/MS)
• gas chromatograph-triple quadrupole mass spectrometer (GC-QqQ-MS/MS)
• carp fish samples