Study On Detection Method Of Drug Residues In Poultry Eggs

Poultry eggs are one of the essential foods on the table of Chinese residents and are widely welcomed because of their high nutritional value.China’s poultry egg production has grown steadily and ranked first in the world,with an annual output of more than 30 million tons since 2015,becoming one of the main poultry products consumed in China.Drugs are used to prevent or treat various diseases during the laying hen feeding process,but improper use will cause drugs to remain in poultry eggs,which will affect human health.Therefore,it is of great significance to establish a rapid and efficient method for detecting multiple types of drug residues in poultry egg products to ensure the quality and safety of poultry egg products and reduce the risk of consumption.In this paper,289 drug residue screening and identification methods were established based on Qu ECh ERS pretreatment technology by liquid chromatography-triple quadrupole tandem mass spectrometry,which provided technical means for the rapid detection of cross-class drug residues in poultry eggs.The main research contents and results are as follows:A liquid chromatography-triple quadrupole tandem mass spectrometry method for simultaneous determination of 289 drugs residues in poultry eggs was established based on Qu ECh ERS method.Includingβ-agonists,tetracycline,macrolides,sulfonamides,quinolones and other 17 classes of drugs.Methods Acetonitrile and acid acetonitrile were extracted in the condition of citric acid-sodium citrate buffer solution（p H≈4）by vortex oscillation,and were purified by C18,PSA and Na₂SO₄,then concentrated and tested by machine.Primary and secondary mass spectrum databases of 289 drugs in 17 classes were constructed by liquid chromatography-quadrupole time-of-flight mass spectrometry.First,the primary spectrum database was constructed based on the information of drug English name,chemical formula,CAS number and precise molecular weight,etc.Then,the ion information of each compound fragment was collected by liquid chromatography and four-pole time-of-flight mass spectrometry to construct the high resolution secondary mass spectrum database,which was matched with the primary information,and combined with the retention time of chromatographic information,a complete mass spectrum database was obtained.Method evaluation and verification were carried out for the detection of 289 drug residues in poultry eggs.Based on the established pretreatment method and instrumental method,the methodological evaluation experiments of high,medium and low concentrations of eggs and duck eggs were carried out by liquid chromatography-triple quadrupole tandem mass spectrometry,and the results showed that the drug addition concentration was in the range of 0.25～100μg/kg,the linearity was good,the recovery rate ranged between51.07%-117.8%,and the RSD was less than 20%.The results show that the mass spectral fragment information obtained at different concentration levels can be matched with the information in the database,of which 215 drugs have good linear range within 0.25～100μg/kg,the recovery range is 50%～130%,the RSD is less than 20%,and 74 can obtain secondary spectra at 100μg/kg concentration,and the recovery range is 51.79%-Between119.62%,RSD is less than 20%.Finally,the actual detection and application of different kinds of poultry egg samples showed that sulfadiazine was detected in one quail egg,and the sample obtained accurate quantitative results by triple quadrupole tandem mass spectrometry,and the mass spectrometry fragment information was compared and verified by quadrupole time-of-flight mass spectrometry,which proved the accuracy and practicability of the method.