基于通过型固相萃取净化法快速测定鱼肉中地西泮残留量的研究OA

A rapid,convenient,and quantitative analysis method using pass-through solid phase extraction(SPE)purification has been developed for detecting diazepam residues in fish meat.The fish meat samples were extracted with a small amount of acetonitrile,and the extract was purified using a neutral alumina SPE column.The purified ex-tract was then evaporated to dryness under reduced pressure,dissolved in an acetonitrile-water solution,and brought to volume.Quantitative analysis was performed using high-performance liquid chromatography-tandem mass spec-trometry(HPLC-MS/MS).The results showed that diazepam exhibited a good linear relationship in the range of 0.20-50.00 ng/mL.And the standard curve linear regression equation is y=51 600x-14 500,with correlation coefficients(r)of 0.999 8.The method's detection limit was 0.10 μg/kg,and the quantification limit was 0.25 μg/kg.A recovery experiment was conducted with 3 levels of 0.25,1.50,and 2.50 μg/kg,with the average recov-ery rates of diazepam being 91.2%,92.0%,and 93.6%,respectively,and the relative standard deviations being 7.6%,9.0%,and 6.0%.In summary,this method has many advantages of rapid and simple sample preparation,low detection limits,high accuracy,and strong practicality,which suitable for large-scale rapid quantitative detec-tion of diazepam residues in fish meat samples.[Chinese Fishery Quality and Standards,2025,15(1):19-25].