| Aquatic products are becoming one of the preferred foods for consumers at domestic and foreign due to their high protein,high nutrition,high unsaturated fatty acids,low fat and delicious taste.etc.At the same time,its quality and safety issues are wildly concerned by the consumers.Drug residues have been a problem for the quality and safety of aquatic products for a long time.There are hidden dangers of illegal fishery drugs and other prohibited drugs in aquaculture and transportation links.Therefore,it is necessary to monitor typical drug residues in aquatic products in aquaculture and circulation links.Rifampicin is a semi-synthetic antibiotic.Our research group found that rifampicin has hidden dangers of illegally used in aquaculture all over the country.In addition,media reports have shown that there is a hidden danger of illegal use of sedative drugs such as diazepam in the circulation of aquatic products.However,the research group showed through data investigation that there is no accurate quantitative determination method for 12 sedative drugs such as rifampin and diazepam in aquatic products.Therefore,this paper developed the detection methods for rifampicin and other 12 sedatives in aquatic products based on QuEChERS technology with the support of the industry standard-setting project such as "Determination of Rifampin Residues in Aquatic Products by Liquid Chromatography-Tandem Mass Spectrometry",and completed the following research work:(1)An isotope dilution high performance liquid chromatography coupled with triple quadrupole mass spectrometry(HPLC-MS/MS)method was established for the determination of rifampicin in aquatic products.The samples were pretreated with QuEChERS(Quick?Easy?Cheap?Effective?Rugged?Safe)method,extracted by 15 m L acetonitrile,and purified by 10 m L hexane.At the same time,the matrix effect was compensated by isotope dilution method.The results showed that the linear relationship was good in the concentration range of 0.5?20 ?/L and the correlation coefficient was 0.9956.At the three spiked levels of 0.5,1.0 and 5.0 ?g/kg,the average recoveries of rifampicin were between 80.39% and 101.5%.The within-day RSD was ranged from 1.21% to 4.83%.The between-day RSD was ranged from 1.39% to 7.18%.The method has good repeatability,high sensitivity,high accuracy and high recovery.It is suitable for the detection of rifampicin in aquatic products and can be used as a standard detection method of rifampicin in aquatic products.(2)A method using HPLC-MS/MS was established for the detection of 12 sedatives in aquatic products,including triazaine,tetracaine,lidocaine,procaine,bupivacaine,quaaludes,niazepam,alprazolam,triazolam,estazolam,diazepam and oxazepam.The sample was pretreated with QuEChERS method,extracted by ultrasonic-assisted salting out extraction,and then low temperature and high speed centrifugation was used to achieve solid-liquid separation.Acetonitrile was used as the extraction solvent.The miture of sodium chloride and anhydrous sodium sulfate was used as salting-out packages.The 12 sedatives was detected by HPLC-MS/MS in MRM mode.The results showed that the linear relationship of 12 tranquilizers was good in the concentration range of 0.5?20 ?g/L,and the correlation coefficients were all higher than 0.9976.Except for procaine,the recoveries of the other 11 compounds were 77.38-118.45% and the RSD was 2.27-8.46%.In general,the method has good recoveries,high precision,good repeatability and meets the requirements of veterinary drug residues detection. |
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