| Egg is an inexpensive and high quality animal protein food,with high protein,low fat,low calorie and high absorption rate,high conversion rate,etc.,which has made an important contribution to the protein nutrition needs of our residents.The quality and safety supervision of eggs has become one of the important tasks of the food safety supervision system.In this study,an EMR-Lipid matrix dispersive solid phase extraction cleanup(d SPE)technique was established to rapidly and accurately detect the contents of typical veterinary drugs(169),pesticides and their metabolites(295)and dioxins and their analogues(29)in eggs.Data on the levels of typical contaminants in eggs from a region were obtained,and dietary exposure analysis was conducted in conjunction with data from the Fourth China Total Diet Study.The main findings were as follows.(1)Based on the novel EMR-lipid removal material as the purification material,the sample pretreatment method and the instrumental detection method of 169 kinds of veterinary drugs in eggs are developed.The experimental results showed that the method was effective in removing lipid impurities in the sample matrix,and had a high recovery rate for the target analyte,which could realize the simultaneous analysis of multiple residual components.Among them,the spiked recovery rates of 15 nonsteroidal anti-inflammatory veterinary drug residues ranged from 82% to 124%,and the RSD ranged from 2% to 26%,the LOD was 0.07-1.42 μg/kg.The recoveries of 9β-agonist residues were 78%-116%,the RSD were 3%-16%,and the LOD was 0.01-0.37 μg/kg.The recoveries of 8 hormonal veterinary drugs were 57%-124%,the RSD was 4%-31%,and LOD was 0.09-1.80 μg/kg.The recoveries of 21 anti-parasitic veterinary drugs were 75%-124%,the RSD was 1%-26%,and the LOD was 0.01-3.81μg/kg.The recoveries of 14 anticoccidial veterinary drugs were 67%～117%,the RSD was 2%～30%,and the LOD was 0.01～2.52 μg/kg.The recoveries of 74 antibiotic residues were 57%-127%,the RSD was 3%-31%,and the LOD was 0.01-2.03 μg/kg.The recoveries of 12 pesticide residues were 67.3%-118%,the RSD was 1%-28%,and the LOD was 0.02-2.75 μg/kg.The recoveries of 16 other veterinary drugs were64%～121%,the RSD was 2%～30%,and the LOD was 0.01～2.43 μg/kg.The linearity,accuracy and precision of the method were in accordance with the requirements of the indicators in GB/T 27417-2017 Guide for the Validation and Verification of Chemical Analytical Methods.This method was used to detect quinolones,amantadine,rimantadine and ribavirin,chloramphenicol,metronidazole,flufenicol,flufenicomide and tetracycline in eggs.Some of the veterinary drugs tested in this study were detected in the egg samples collected.Combined with the dietary consumption data on eggs in the Fourth China Total Diet Study(37.25 g/d),the intake was calculated according to the standard people(adult male light manual workers,weighing 63 kg).The health risk of consuming veterinary drugs through eggs is low for residents.By using EMR-lipid material,egg samples are pretreated with GC-MS/MS(62kinds)and UHPLC-MS/MS(233 kinds)respectively.295 pesticide residues are rapidly and accurately determined.The method had good precision,accuracy and linearity.The recoveries of 16 carbamate pesticide residues were 58.1%～119%,the RSD ranged from 2.1% to 29%,and LOD was 0.01～6.26 μg/kg.The recoveries of 17 pyrethroid insecticides were 59.2%-124%,the RSD was 7.2%-18%,and the LOD was0.24-9.75 μg/kg.The recoveries of 15 organochlorine pesticide residues were54.1%～125%,the RSD was 4.3%～22%,and the LOD was 0.07～5.16 μg/kg.The recoveries of 88 organophosphate pesticide residues ranged from 50.3% to 133%,the RSD ranged from 1.2% to 34%,and the LOD ranged from 0.01 to 4.79 μg/kg.The recoveries of 58 pesticide residues were 55.1%-128%,the RSD was 3%-33%,and the LOD was 0.01-6.99 μg/kg.The recoveries of 15 pesticide residues were 54.1%-124%,the RSD was 4.6%-30%,and the LOD was 0.01-7.16 μg/kg.The spiked recoveries of18 unclassified pesticides were 62.4%-126%,the RSD was 1.3%-30%,and the LOD was 0.01-2.32 μg/kg.The recoveries of 59 herbicide were 51.7%-132%,the RSD was1.2%-34%,and the LOD was 0.01-2.65 μg/kg.The recoveries of 9 other pesticide residues were from 61.6% to 125%,the RSD was from 1.1% to 26%,and the LOD was from 0.01 to 1.57 μg/kg.The method was used to detect fipronil and its metabolites in egg samples.Only two samples of fipronil sulfone were detected.Combined with the data from the Fourth China Total Diet Study,the results showed that the health risk of fipronil ingestion through eggs was low for residents.(3)We detected and analyzed 29 dioxins and their analogs(dioxin like compounds,DLCs)in chicken egg samples based on high-resolution gas chromatography-highresolution double-focusing magnetic mass spectrometer.The precision,accuracy,detection limit and recovery rate of this method met the requirements.We provided the first systematic risk assessment of the content and toxic equivalent levels(TEQs)of DLCs in eggs.The findings indicated that the TEQs levels of some egg samples exceeded the limited value of the European Union.The TEQs of DLCs in eggs were found to be at the middle-range level.Comparing the dietary intake of DLCs in eggs by inhabitants with the limits set by JECFA and related studies,we found that inhabitants have a low health risk of ingesting DLCs through eggs. |
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