Multi-residue Detection Methods For Chloramphenicol,Stilbenes And Resorcylic Acid Lactones In Porcine Muscle

In this test,an immunoaffinity syringe capable of simultaneously extracting chloramphenicol,stilbenes and Resorcylic Acid Lactones lactone drugs was prepared.An immunoaffinity syringe microextraction ultra liquid chromatography tandem mass spectrometry（IA-MEPS-UPLC-MS/MS）and solid phase extraction ultra high performance liquid chromatography tandem mass spectrometry（SPE-UPLC-MS/MS）capable of simultaneously detecting three types of drugs in porcine muscle was established.Immunoaffinity syringes capable of purifying chloramphenicol,stilbenes and resorcylic acid lactones drugs were prepared by immobilizing antibodies on glass beads by non-point covalent binding method.The column capacity of immunoaffinity syringes measurements were performed.Scanning electron microscopy and XPS characterization were performed on the carrier matrix filled with immunoaffinity syringes,and the changes of materials during the modification of silica were observed.The parameters affecting the extraction effect were optimized.The optimization results were as follows:the extraction time was 15 min,the extraction rate was 3.5m L/min,the elution time was 5 min,the eluent was pure methanol,and the eluent volume was 1000μL.The capacity of the three types of drug columns is between 0.40and 11.73 ng/mg,which can meet the needs of residual analysis.An IA-MEPS-UPLC-MS/MS method was developed for the detection of chloramphenicol,stilbenes,and resorcylic acid lactones in porcine muscle.The results showed that the three types of drugs had good linearity in their respective concentration ranges,and the correlation coefficients were greater than 0.99.The detection limits of the method were 0.15 to 0.3 ng/g,and the limits of quantification were 0.5 to 1 ng/g.The recovery test of negative porcine muscle samples was performed.When the immunoaffinity syringe was used for purification,the recovery rate of the three drugs was between 14.6%and 33.3%,the relative standard deviation within the day was 4.7%～19.2%,and the relative standard deviation during the day was between 1.0%～16.5%.The method has good recovery rate and precision,good reproducibility and short detection time,and can meet the detection of chloramphenicol,stilbenes and resorcylic acid lactones in porcine muscle.A SPE-UPLC-MS/MS method was developed for the simultaneous detection of chloramphenicol,stilbenes,and resorcylic acid lactones.Solid phase extraction was used for sample pretreatment.Ether,ethyl acetate,and methyl tert-butyl ether were compared as extraction solvents.HLB solid phase extraction cartridges and C₁₈solid phase extraction cartridges were used as purification means.Effect of Three Classes of Drug Recovery in Porcine muscle.The results showed that when ethyl acetate was used as the extraction reagent and C₁₈solid-phase extraction cartridges were used as the purification means,the three types of drugs had good linearity in their respective concentration ranges,and the correlation coefficients were greater than 0.99.The detection limits of the method were 0.15 to 0.3 ng/g,and the limits of quantification were 0.5 to 1 ng/g.The recovery test of negative porcine muscle samples was performed.When the C₁₈solid phase extraction cartridge was used for purification,the recovery rate of the three drugs was between 42.4 and 97.1%,and the relative standard deviation within the day was 6.1 to 16.9%.The deviation is between 3.7 and18.4%.