Solid-Phase Extraction Combined with Gas Chromatography-Triple Quadrupole Tandem Mass Spectrometry for the Determination of 11 Benzotriazole Ultraviolet Stabilizers in Aquatic Products

In this study, a method for the simultaneous determination of 11 benzotriazole ultraviolet stabilizers (BUVs) in aquatic products was developed using solid-phase extraction combined with gas chromatography-triple quadrupole tandem mass spectrometry. Samples were ultrasonically extracted with 10 mL of acetonitrile-water mixture (4:1, V/V), and added with 2.5 g of sodium chloride for salting out. The supernatant was concentrated after three rounds of freezing for degreasing, and then cleaned up by passing sequentially through PRiME HLB and Florisil solid-phase extraction (SPE) columns. The target compounds were separated using a DB-5MS (30 m × 0.25 mm, 0.25 μm) column, detected in the multiple reaction monitoring (MRM) mode by tandem mass spectrometry, and quantified by the isotope internal standard method. The results showed that good linearity (R² > 0.998) was observed for the 11 BUVs, the limits of detection (LOD) ranged from 0.11 to 1.08 ng/g dry mass, and the limits of quantification (LOQ) ranged from 0.33 to 3.24 ng/g dry mass. At three different spiked concentrations, 2, 10, 50 ng/g, the recovery rates of these BUVs ranged from 71.98% to 119.08% with relative standard deviation (RSD) of less than 19.60%. In two types of aquatic products, a variety of BUV monomers at different concentrations were detected by the proposed method. This method is simple, reproducible and precise, and effectively solves the problem existing in the extraction and purification of BUVs from biological matrices with high fat content, providing effective technical support for the accurate quantitative analysis of BUVs in aquatic products.