Preparation Of Immunoaffinity Microextraction By Packed Sorbent And Its Application In Determination Of Quinolones And Zeranols

With the development of economy,people pay more and more attention to food safety and the development of drug residue detection technology has also been paid great attention to.The operation is simple and the result is accurate green environmental protection is the direction of future development.A new selective adsorbent for MEPS was made on the basis of glass beads bound with m Abs and a novel IA-MEPS-HPLC-FLD method for the detection of QNs in milk has been developed.The syringe was filled with 0.2 g microbeads bounded with a QN monoclonal antibody using glutaraldehyde and the specificity and column capacity of the prepared IA-MEPS were investigated.And the relevant parameters of IA-MEPS were optimized.Finally,when extracting QNs,the extraction time is 15 min,the extraction rate is 3.5 m L/min,the elution time is 5 min,the eluent is methanol-and phosphate-buffered saline(9 ∶ 1,v/v),and the eluent volume is 600 μL.The extraction time of extraction ZER is 15 min,the extraction rate is 3.5 m L/min,the elution time is 5 min,the eluant is pure methanol,and the eluent volume is 600 μL.The column capacity of QNs is between 0.051～0.458 ng/mg,and the column capacity of ZER is 0.284～0.429 ng/mg.It can meet the needs of residual analysis.0.2 g microbeads bounded with a QN monoclonal antibody using glutaraldehyde,and the relevant parameters of IA-MEPS were optimized.Milk samples were extracted at a flow rate of 3.5 m L/min,600 μL of methanol-and phosphate-buffered saline(9∶1,v/v)was used for elution,and 200 μL of mobile phase was used for reconstitution after the sample was dried with nitrogen.Then,the sample was detected by LC-FLD.The limit of detection of the method ranged from 0.05 to 0.1 ng/g for eight QN compounds,the limit of quantification ranged from 0.15 to 0.3 ng/g,and the intra-and inter-day precision were 3.2%～14.6% and 9.1%～15.8%,respectively.The syringe was filled with 0.2 g microbeads bounded with a ZER monoclonal antibody using glutaraldehyde,and the relevant parameters of IA-MEPS were optimized.Milk samples were extracted at a flow rate of 3.5 m L/min,600 μL of methanol was used for elution,and 200 μL of mobile phase was used for reconstitution after the sample was dried with nitrogen.Then,the sample was detected by LC-MS/MS.The limit of detection of the method ranged from 0.05 ng/g for six ZER compounds,the limit of quantification ranged from 0.2 ng/g,and the intra-and inter-day precision were 5.28%～17.64% and 7.04%～18.75%,respectively.