Study On High-throughput Screening Methods For Hundreds Of Veterinary Drug Residues In Animal-derived Food

In this paper,an information database of 10 kinds of 103 kinds of veterinary drugs,such as?-receptor hormones,quinolones,antibiotics,nitroimidazoles,sulfonamides,steroid hormones,benzimidazoles,etc.,was established to determine the optimal screening parameters.The database includes key information such as Chinese name,English name,CAS,molecular formula,ionization type,retention time,precursor ion,product ion,collision energy,etc.,which lays a foundation for high-throughput screening methods for veterinary drug residues.QuEChERS extraction method was combined with LC-MS/MS,comprehensive consideration of the physical and chemical properties of various veterinary drugs,optimized the pretreatment method for pork and fish sample screening,and established a total of 10kinds of 103 kinds of veterinary drug residues high-efficiency liquid analytical detection methods for high-throughput screening by phase chromatography-mass spectrometry/mass spectrometry(LC-MS/MS):extraction with 1%formic acid acetonitrile and purification with EMR-Lipid,and finally reconstituted with 5%acetonitrile-water solution;and the method was carried out by gradient elution with acetonitrile(0.2%formic acid)-water(0.2%formic acid)system using an Agilent Eclipse Plus C18 column(3.0 x 150 mm,1.8?m)for dynamic-multiple reaction monitorin(d-MRM)mode screens 10 kinds of 103 drugs in pork and fish tissue within 20 minutes.The results showed that the linearity of 103 veterinary drugs in the range of 0.05~100.0?g/kg,0.25~100.0?g/kg or 0.50~100.0?g/kg was good,and the correlation coefficient R~2was greater than 0.99.The detection limit of this method is 0.10~10.0?g/kg,and the limit of quantification is 0.30~30.0?g/kg.The average recovery rate of 103 veterinary drugs in pork matrix at high,medium and low concentrations(1,10,100?g/kg)was 60.40%~132.91%,relative standard deviation was 0.77%~25.24%;the average recovery rate in fish matrix was61.88%~128.59%,relative standard deviation 1.13%~24.83%.The precision of 103veterinary drugs in pork matrix is 0.49%~12.26%,and the precision in fish meat matrix is2.96%~11.51%.The method has high sensitivity and good accuracy,meets the screening and testing requirements of various veterinary drug residues,and can be used for rapid screening of large quantities of samples.Using established methods to detect 103 veterinary drug residues in pork and fish,21cases of hydrocortisone were detected in 30 pork samples;7 cases of hydrocortisone were detected in 30 fish samples.There were 13 cases of enrofloxacin and 1 case of metronidazole.