| In recent years,the irrational use and abuse of fluoroquinolones by humans has become increasingly serious,resulting in excessive levels of residues in animal-source foods.If you eat livestock and poultry products that contain excessive drug residues for a long period of time,it can lead to a series of problems such as dizziness,vomiting,and diarrhea.Therefore,for the residue detection of such drugs in livestock and poultry products,it is necessary to develop a rapid and accurate detection technology in order to detect the content of its drugs in foods,provide protection for people's health,and provide strong technical support for China's trade.This study mainly includes 3 aspects:1.By using enzyme-linked immunosorbent assay,120 samples of chicken and 200 samples of chicken eggs collected were tested from five cities in Ningxia.The results showed that none of the samples involved in the trial contained quinolones.The method has a simple test procedure and can be applied to the rapid detection of a large number of samples.2.Establish a method for the determination of four fluoroquinolones residue in chicken by solid phase extraction combined with ultra performance liquid chromatography.The sample was extracted with a phosphate solution.The extract was purified with a C18 solid phase extraction column and eluted with a mobile phase.The assay was performed using a high performance liquid chromatograph.The linear relationship between the four drugs at 0.005?g/mL-0.5?g/mL was good,and the correlation coefficient R was greater than 0.99994.At the concentrations of 20?g/kg,100?g/kg and 200?g/kg,the average recovery of the method was between 40.0%and 94.8%with relative standard deviations of 1.5%-17.4%.The method detection limit was 20?g/kg,the quantification limit was 100?g/kg.According to the method established in this study,120 chicken samples collected from 5 cities in Ningxia were tested in 2017.None of the four fluoroquinolones were detected.3.A solid phase extraction combined with high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)was developed for the determination of seven fluoroquinolones in eggs.The sample was extracted with EDTA-Mcllvaine solution and degreased with n-hexane.The extract was purified by an HLB extraction column,dried with nitrogen,concentrated by mobile phase,and analyzed by HPLC with tandem mass spectrometry.The linear relationship was good between 5 ?g/kg and 100?g/kg for 5 drugs,and the linear relationship between ciprofloxacin and oxolinic acid was 6 ?g/kg to 100 ?g/kg and 0.25 ?g/kg to 10 ?g/kg,respectively.The coefficients were all greater than 0.9959.When the amounts were 100?g/kg,200?g/kg,and 500?g/kg(Equivalent to upper machine concentration 20?g/kg,40?g/kg,100?g/kg),the average recoveries were 61.9%?106.2%and the relative standard deviations were 1.3%?10.1%.The detection limits of ciprofloxacin and oxolinic acid in this method were 1.2 pg/kg and 0.05 ?g/kg,the quantitation limits were 24 pg/kg and 1 ?g/kg.The detection limits of the other five drugs were 0.5 ?g/kg and the quantitation limits were 10 ?g/kg.According to the method established in this study,200 samples of eggs collected were tested in 5 cities of Ningxia in 2017.None of the 7 fluoroquinolones were detected.The two methods established in this paper have a simple pretreatment process,high sensitivity,and a short detection time.The detection results meet the requirements of domestic regulations and can be applied to the residue detection of fluoroquinolones in animal foods. |
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