Solid‐phase microextraction combined with gas chromatography/triple quadrupole tandem mass spectrometry for determination of nitrated polycyclic aromatic hydrocarbons in sediments

Abstract

Nitro‐polycyclic aromatic hydrocarbons have been detected in various environmental media. However, determination in sediment matrix is challenging due to the lack of a suitable method. In this study, a reliable method for determining 15 nitro‐polycyclic aromatic hydrocarbons in sediments was developed based on accelerated solvent extraction and solid‐phase microextraction coupled with gas chromatography–tandem mass spectrometry. The accelerated solvent extraction and solid‐phase microextraction are sample pre‐treatment techniques that have advantages, such as rapid operation and minimal sample volume. Initially, the solid‐phase microextraction was optimized using five commercial fibers and from that 65 μm polydimethylsiloxane/divinylbenzene fiber was selected as the best fiber. Further, the accelerated solvent extraction conditions were optimized by Taguchi experimental design, such as extraction temperature (120℃), extraction solvent (dichloromethane), number of cycles (two), static extraction period (4 min), and rinse volume (90%). The method parameters, such as limits of quantitation, and intraday and interday accuracy and precision, were in the range of 0.067–1.57 ng/g, 75.2–115.2%, 69.9–115.4%, and 1.0–16.5%, respectively. Upon meeting all the quality criteria, the method was applied successfully to analyze real sediment samples. Therefore, our study creates a new prospect for the future application of direct immersion solid‐phase microextraction in sediment analysis.