| With the improvement of people’s living standards,the quality and safety of aquatic products has attracted more and more attention.Therefore,this study focuses on the actual demand of detection technology of quality and safety in seafood,and the problems of existing detection technology have been too complex for residuals sedatives,sulfonamides,and quinolones in seafood.Meanwhile in the study,a novel cheap analytical filtration syringe(CAFS)clean-up column was developed in combination with reversed-dispersive solid-phase extraction(r-DSPE)clean-up technology.The developed method has been applied to analysis of the HPLC coupled with triple quadrupole-linear ion trap MS/MS(HPLC-QTRAP-MS/MS)for sedatives,quinolones and sulfonamides residuals in seafood:(1)Based on the Qu ECh ERS pretreatment method,a fast,simple and convenient detection method combined with a novel CAFS-clean-up column and high-performance liquid chromatography/quadrupole-linear ion trap tandem mass spectrometry(HPLC-QTRAP-MS/MS)was developed for the rapid determination of three sedatives in seafoods.10 m L of acetonitrile solution acetonitrile(containing 0.1%formic acid,V/V)was added to extract the sample.This study optimized the type and amount of clean-up sorbents and used matrix-matched calibration method to avoid the matrix effect.The results showed that when 300 mg of primary/secondary amino was used as clean-up sorbents,the target compounds in different matrix had a good linear relationship(1-50μg/kg)and the correlation coefficient(R~2)of the linear regression was higher than 0.99.With 5.0μg/kg,25.0μg/kg,50.0μg/kg as the sample spiked concentration,the recoveries of the three sedatives were in the range of88.73%～108.72%,and the intra-day relative standard deviations(Inter-day RSD)were in the range of 0.34%～14.67%.The inter-day relative standard deviation(Inter-day RSD)were in the range of 1.50%～12.37%.At the same time the purification performance of CAFS cleanup and r-DSPE methods was compared.The experimental results showed that CAFS cleanup method is more effect and this method has high precision,high efficiency,and can be used as the detection method of three kinds of sedatives in seafood.(2)Based on(1),this study developed a method for the analysis of 3 sedatives and6 quinolones residues in aquatic products.The samples were purified by CAFS clean-up column.The type and amount of clean-up sorbents,the type of extraction solution and the clean-up times were optimized in this study.10 m L of acetonitrile solution(acetonitrile:acetic acid:water=79:1:20,V/V)was added for extraction.The matrix-matched calibration method were used to avoid the matrix effect.With 5.0μg/kg,10.0μg/kg,20.0μg/kg as the sample spiked concentration,the recoveries of the three sedatives were in the range of 99.10%～109.79%,and the inter-day RSD were in the range of 2.02%～7.65%.The inter-day RSD were in the range of 0.55%～6.30%.The limit of detection(LODs)ranged from 0.2 to 1.0μg/kg.The limits of quantification(LOQs)ranged from 1.0 to 5.0μg/kg.Thence,thr CAFS cleanup method has higher recoveries rate,better precision,more and more efficiency,and can be meet relevant test requirements.(3)Based on(1)and(2),a method for the analysis of 17 sulfonamides and trimethoprim residues in seafood was developed by using CAFS clean-up column combined with HPLC-QTRAP-MS/MS.The sample was purified by CAFS clean-up column.Simultaneously,the type and amount of clean-up sorbents,the type of extraction solution and the clean-up times were optimized in this study.10 m L of acetonitrile solution(acetonitrile:water=80:20,containing 0.1%formic acid,V/V)was added for extraction.The results show that all target compoundsthe had a good linear relationship(1-50μg/kg),and the correlation coefficient(R~2)of the linear regression was higher than 0.996.With 10.0μg/kg,20.0μg/kg,50.0μg/kg as the sample spiked concentration,the recoveries were in the range of 81.39%～119.62%,The inter-day RSD were in the range of 1.72%～13.96%and the he inter-day RSD were in the range of2.23%～3.09%.The results show that this method could be used for the detection of 18target compounds residues in seafood. |
PDF Full Text Request