Study On Rapid Screening Methods For Various Hormones And Antibiotics In Aquatic Products

Aquatic products are rich in nutrients,with high protein,low fat,rich in vitamins and active substances,and are indispensable quality protein sources for the residents' dietary structure.However,in order to the pursuit of economic benefits,some aquaculture farmers have abused antibiotics and used hormones illegally,causing serious security risks.Therefore,the safety issues of aquatic products have receiving increasing attention.This article was based on UPLC-QTOF technology to establish a rapid and effective screening method for various hormones and antibiotic residues in aquatic products.An analytical method was established for rapid screening of 16 hormones residues in aquatic product by modified QuECHERS combined with ultra performance liquid Chromatography-quadrupole time of flight mass spectrometry(UPLC-QTOF-MS).The homogenized sample were extracted with 1%acetic acid acetonitrile,salting out with sodium chloride and anhydrous magnesium sulfate,and defatted with n-hexane,then cleaned-up by Cl8.Analysis were separated on an BEH C18 column using water with 0.1%formic acid and methanol as mobile phase by gradient,analyzed by MS under ESI positive ionization mode.The linear range was 1?100?g/L for each compound with the correlation coefficients of more than 0.9906.At the different spiked level,the recoveries were ranged from 53.6%to 135.2%,with relative standard deviations(RSDs)ranged from 0.93%to 10.93%in Penaeus vannamei,Pseudosciaena crocea,Grass Carp and Swimming crab matrices?The limits of detection(LODs)(S/N=3)were 0.2?2.7 ?g/kg and the limits of quantification(LOQs)(S/N=10)for the analytes were 0.8?9.0 ?g/kg.A rapid screening method for 49 kinds of antibiotics in aquatic products(fish,shrimp,crab)was established by improving QuEChERS method combined with UPLC-QTOF technology.The homogenized sample were extracted with 3%acetic acid acetonitrile,salting out with sodium chloride and anhydrous magnesium sulfate,and cleaned-up by C18 and PSA.Analysis were separated on an BEH C18 column using water with 0.1%formic acid and methanol as mobile phase by gradient,analyzed by MS under ESI positive ionization mode.The linear range was 1?100 ?g/L for each compound with the correlation coefficients of more than 0.9851.At the different spiked level,expect for Lincomycin hydrochloride,the recoveries were ranged from 60.6%to 117.9%,with relative standard deviations(RSDs)ranged from 1.6%to 14.00%in Grass Carp,Penaeus vannamei and Scylla serrata matrices.The limits of detection(LODs)(S/N=3)were 0.05?2.40 ?g/kg and the limits of quantification(LOQs)(S/N=10)for the analytes were 0.16?8.00?g/kg.Screning database of 65 compound was developed using UPLC-QTOF technology and Masslynx software,and then the database was used to screening aquatic products samples.The result showed that a few compounds,including hydrocortisone and difluoxacin hydrochloride were detected in the real samples,however,after further quantitative detection found that there was no compound detected and quantitated that would exceed the MRL established in the Ministry of Agriculture 235 announcement.