| Pesticide and veterinary drug residues in bee products will bring human health effects,but also affect the ecology of bee population.This study selected potential influence on human health and bee population agricultural veterinary drugs to establish fast,efficient,sensitive and accurate more residue detection method,and monitor the actual agricultural municipal bee products,to assess the potential risks to human health.1.A detection method based on a new solid phase extraction column combined with ultra-efficient liquid phase-tandem mass spectrometry(UPLC-M S/MS)to detect 25 veterinary drugs and 6 pesticide residues in bee products.Sample pretreatment was based on the new solid phase extraction column(PRIME HLB)method,agricultural and veterinary drug residues in the bee product sample are extracted from 80% acetonitrile water solution(including 0.2% formic acid),directly through the column,1 second,nitrogen blowing concentration,1 m L 10% methanol solution,0.22 μm PTFE microporous membrane after20 S,and quantified by external standard method.The linear range of veterinary drug residues is from 0.1 to 100 ng/m L,The linear range of pesticide residues ranged from 1 to250 ng/m L,The correlation coefficient were all> 0.995;The limit of quantification is0.1～10 μ g / kg(S / N=10);The 31 compounds spiked at 5 to 20 μ g / kg were recovered from 60.3% to 114.2% in honey,relative standard deviation ranged from 0.3% to 13.2%,Recovery in bee pollen ranged from 61.7% to 114.8%,relative standard deviation ranged from 0.4% to 12.1%,recovery rates in royal jelly ranged from 64.1% to 116.7%,The relative standard deviation ranged from 0.7% to 12.3%.2.142 honey samples,51 bee pollen samples and 13 royal jelly samples from 17 districts and counties in Chongqing were analyzed and tested.The data showed that 12 kinds of honey,6 kinds of bee pollen and 1 kind of agricultural and veterinary drug residues of royal jelly were detected respectively.12 veterinary residues were detected in honey samples,The higher detection rate was carbendazim(5.6%),imidacloprid(4.9%),acetamididine(3.5%),the residual mean values were 21.9 μ g / kg,13.2 μ g / kg and 8.9 μ g / kg;Six kinds of agricultural and veterinary drug residues were detected in the bee pollen samples,The higher detection rates were carbendazim(9.8%),imidacloprid(7.8%),acetamididine(5.9%),The residual mean value was 16.0 μ g / kg,16.0 μ g / kg and 12.0 μ g / kg;One veterinary drug residue was detected in the royal jelly samples,The detection rate was 7.7%,the residue value was 19.7 μ g / kg.3.Food safety index method was used to assess the dietary risk of agricultural and veterinary drug residues in bee products on human health.The results showed that enrofloxacin,trimethoprim,lonazole,ciprofloxacin,chloramphenicol,and metronidazole detected in honey were high(IFS> 1),and the dietary risk of agricultural and veterinary residues detected in bee pollen and royal jelly to human health was low.This study established the simultaneous detection of honey,bee pollen,royal jelly,25 kinds of pesticide residue of ultra-efficient liquid phase-tandem mass spectrometry(UPLC-M S/MS)detection method,the method has the characteristics of simple,fast and accurate,collected the 17 counties 142 batches of honey,bee pollen 51 batches,royal jelly13 batches,and the animal residue detection,clear the status of Chongqing bee products,and investigated the potential dietary risk.The research results can provide methods and data support for the risk monitoring of veterinary drug residues and pesticide residues,food safety regulatory agencies,and the bee industry development system. |
