Study On Screening Method For Multi-Residues Of 63 Veterinary Drugs In Animal Derived Food By Liquid Chromatography-Mass Spectrometry

In the process of preventing and controlling animal diseases and promoting animal growth and quality,veterinary drugs can easily cause residues in animal derived food,which can contaminate animal derived food and endanger human health.Especially unreasonable and illegal use of veterinary drugs,it is very easy to affect public health security.GB31650-2019 “National Food Safety Standard-Maximum Residue Limits for Veterinary Drugs in Foods” specifies the list of veterinary drugs that are allowed for therapeutic use but not detected and the maximum residue limit(MRL)of approved veterinary drugs in China.The Ministry of Agriculture and Rural Affairs of the People’s Republic of China issued Announcement No.250 on January 6,2020,re-establishing the list of prohibited drugs in animal derived food.Therefore,establishing a screening method for the residues of prohibited drugs and veterinary drugs with food safety risks in animal derived food can better supervise food safety.Nowadays,screening methods for multiple types of veterinary drugs in animal derived food are less,and the pre-treatment is not convenient enough,which can not meet the needs of monitoring veterinary drug residues in animal derived food.In order to achieve the screening of veterinary drug residues in animal derived food,a liquid chromatography-mass spectrometry method for screening 63 veterinary drugs residues in animal derived food was established in this study.In this study,a liquid chromatography-mass spectrometry(LC-MS/MS)method was established for 63 veterinary drugs in eight categories: androgens,progestins,β-agonists,nitroimidazoles,antivirals,sedatives,non-steroidal anti-inflammatory drugs,and glucocorticoids in pig muscle,eggs,and milk.The samples were extracted with 1%acetic acid-acetonitrile,and purified by solid phase extraction(SPE).The pig muscle and milk samples were purified by Oasis PRi ME HLB solid phase extraction cartridges,and the egg samples were purified by SHIMSEN QVet-NM+ cleanup cartridges.After drying under nitrogen,the sample was re-dissolved using acetonitrile/water(20:80,v/v)and detected using LC-MS/MS.Liquid chromatographic analysis was performed on a C18reversed-phase chromatographic column with gradient elution using 0.1% formic acid in water-2mmol/L ammonium formate and methanol,all drugs were completely separated within 25 minutes.Mass spectrometry analysis was performed using electron spray ionization(ESI)with multiple reaction monitoring(MRM)mode,and positive and negative ion scanning.The limits of detection of 63 veterinary drugs in animal derived food,including androgens,progestins,β-agonists,nitroimidazoles,antivirals,sedatives,non-steroidal anti-inflammatory drugs,and glucocorticoids,were 0.1-0.3μg/kg,and the limits of quantification were 0.2-1.0 μg/kg.The recoveries were 40.7%-91.8%,and the coefficients of variation were less than 25%,which met the assessment criteria of the method.The above results indicated that the method established in this study can be used for screening and detecting veterinary drug residues in animal derived food.In this study,the screening method of veterinary drugs in animal derived food was established,which made up for the shortcomings of previous detection methods such as single drug type and complex sample pretreatment.