This application note details a quick and effective analytical method for the determination of low and trace level polycyclic aromatic hydrocarbons (PAHs) in fish samples as an alternative to procedures involving more time consuming and complex techniques. A simplified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method with dispersive solid phase extraction (dSPE) provided sufficient sample matrix cleanup while preserving low level analyte detection. A pressure controlled tee was installed post column to implement the use of automated backflush to diminish residual sample carryover and reduce instrument cycle times. The Agilent J&W DB-5ms Ultra Inert (UI) 20 m × 0.18 mm , 0.18 µm column effectively resolved the 16 targeted PAHs. A GC/MS method employing selective ion monitoring (SIM) was calibrated at the 10, 25, 50, 100, 250, 500, and 1000 ng/mL PAH levels, yielding excellent linearity and reproducibility. The spiked levels for recovery determinations were 25, 250, and 500 ng/mL. Recoveries ranged from 80% and 139% with RSD below 6%.
This document details an analytical method for determining low and trace level polycyclic aromatic hydrocarbons (PAHs) in fish samples. The method utilizes Agilent Bond Elut QuEChERS dispersive solid phase extraction (dSPE) for sample preparation, offering a simplified alternative to more complex and time-consuming techniques. The approach allows for the processing of up to 60 samples in an eight-hour shift.
The analysis employs an Agilent J&W DB-5ms Ultra Inert (Ul) 20 m x 0.18 mm, 0.18 µm column to effectively resolve the 16 targeted PAHs. The method uses a GC/MS system equipped with selective ion monitoring (SIM) and automated backflush capabilities to reduce residual sample carryover and instrument cycle times.
| Carrier Gas | Helium, constant flow 1.7 mL/min |
|---|---|
| Injection Mode | 0.5 µL splitless |
| Oven Program | 50 °C (0.4 min), 25 °C/min to 195 °C (1.5 min), 8 °C/min to 265 °C, 20 °C/min to 315 °C (1.25 min) |
| Method Limit of Quantitation | 10 ppb |
| Calibration Range | 10 to 1000 ng/mL |
The method uses a QuEChERS approach followed by dispersive solid phase extraction (dSPE).
Up to 60 samples can be processed in one eight-hour shift.
The method limit of quantitation is 10 ppb for benzo[a]pyrene.