Research On High Resolution Mass Spectrometry Detection Technology Of Drug Residues In Animal Derived Foods

Objective:In this research,two method for the determination of sulfonamides,?-agonists and?-blockers in meat products by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry?UPLC-Q-Orbitrap HRMS?was proposed.1.The screening of 23 SAs in meat were performed using QuECHERS followed by a UPLC-Q-Orbitrap HRMS.2.The screening of 22?-agonists,?-blockers and metabolites in meat were performed using QuECHERS followed by a UPLC-Q-Orbitrap HRMS.Methods:1.Extraction of 23 sulfonamide antibacterial medicines and metabolites in meat products with 0.1%acetic acid acetonitrile solution.Anhydrous magnesium sulfate and PSA were used to remove water and impurities from the samples.The upper layer was redissolved in methanol-water?5:95?after being blown dry with nitrogen.23sulfonamides were separated on a WATERS BEH C₁₈ column.Electrospray positive ion mode was used to analyze these antibiotics.Full MS/dd-MS² and AIF scan were used to monitor ions,internal standard method was used for quantification;2.The homogenized meat samples were digested for 2 hours at 37°C,22?-agonist,?-blocker and metabolites were extracted from meat with acetonitrile solution.Sodium chloride was used to salte out stratification.MgSO₄,PSA and C₁₈ absorb were used for dehydration and removing impurity,and the upper layer was redissolved in methanol-water?5:95?after being blown dry with nitrogen.Waters BEH-C₁₈ column was used for separation,electrospray positive ion mode was used to analyze these compounds.Full MS/dd-MS2 and AIF scan were used to monitor ions,internal standard method was used for quantification.Results:1.Establishment the method for determination of 23 sulfonamides in meat products by UPLC-Q-Orbitrap HRMS.This method has a good linear relationship in the concentration range of 0.5-200 ng/mL?r²>0.99?.The recovery rates were 81.3%-113.6%,and the intra-day precision and inter-day precision RSD did not exceed 10%;the LOD of the instrument were 0.1-1.5?g/kg,the LOQ were 0.3-5?g/kg;2.UPLC-Q-Orbitrap HRMS was used for the determination of 22?-agonists,?-blockers and metabolites in meat,the method has a good linear relationship in the concentration range of 0.5-200 ng/mL?r²>0.99?,the recovery rates were 63.2%-103.2%,intra-day precision and inter-day precision did not exceed 7%;the LOD of the instrument were 0.1-1?g/kg,and the LOQ were 0.3-3?g/kg.Conclusion:1.The method of QuECHERS-UPLC-Q-Orbitrap HRMS for the determination of 23 sulfonamides in meat were accurate and suitable for confirmatory analysis sulfonamides drugs and metabolites in meat products;2.The method of QuEChERS-UPLC-Q-Orbitrap HRMS for the determination of 22?-agonists,?-blockers and metabolites in meat were accurate and suitable for confirmatory analysis of?-agonists and?-blocker drugs and metabolites in meat products;...