QuEChERS/HPLC-MS/MS method for determination of diazepam and its metabolites in fish feed and bait
A study has established a method for the simultaneous determination of diazepam and its metabolites in fish feed and bait using dispersive solid-phase extraction(QuEChERS)coupled with high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Samples were extracted with ethyl acetate,and the extract was purified with 50 mg of C18 and PSA solid-phase extraction.The extract was concentrated to near dryness under nitrogen at 40 ℃,reconstituted in 1.0 mL of 80％acetonitrile,filtered,and then analyzed using the HPLC-MS/MS method.The target compounds were separated using a Phenomenex Kinetex C18 series chromatographic column(100 mm× 2.1 mm,2.6 pm)with a gradient elution of 0.1％volume ratio aqueous formic acid and acetonitrile as the mobile phase.Detection was performed in electrospray ionization(ESI+)and selected reaction monitoring(SRM)mode,with a matrix-matched internal standard method for qualitative and quantitative analysis.The results showed that the method had a good linear relationship in the range of 0.5～50.0 pg/kg,with correlation coefficients all greater than 0.999,and the limits of detection and quantification were 0.5 pg/kg and 1.0 pg/kg,respectively.At three different spiking levels,the average recovery rates for diazepam and its metabolites were 82.3％～109.4％,with relative standard deviations of 3.62％～6.33％.The study indicates that this method is rapid,accurate,and highly sensitive,capable of meeting the detection requirements for residues of diazepam and its metabolites in fish feed and bait.
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