HPLC Analysis Of Macrolide Antibiotic Residues In Animal Derived Food

Macrolide antibiotics(MALs) is a kind of chemical structure and antibacterial activity similar to the basic antibiotic group,belong to the spectrum antibiotics. MALs widely used in animal bacteria and mycoplasma infection of the chemical treatment,and it is also important to promote the growth of the animal,and it occupied an important position in animal durgs and feed additives.However,as excessive or inappropriate use of such antibiotics can cause veterinary durg residues,MALs enter the body through the food chain,which will pose a serious hazard to human health.Like other veterinary durgs,detection and monitoring of MALs in animal food residue have attached great importance to many countries.Currently the EU and China have made limited to MALs.This experimental to target detection of SPI,KIT,TYL,TILM,ERM,OLE,aiming at the research of MALs residue in meat,following aspects.1)A comfirmative method was developed with high performance liquid chromatography to detect macrolide antibiotics.By examining column,temperature and mobile phase composition,optimizing the conditions for the chromatography.Diode array detector was used,at 204nm,232nm,287nm wavelength test. With the SPI,KIT,TYL,TILM in the detection limit of 0.016-0.041mg/kg,quantification limit 0.053-0.135mg/kg,the method is sensitive .2)The conditions for the extract,extraction method,solid-phase extraction columns,eluate and eluent were optimized.The treatment involves extraction of the analytes with methanol and clean-up by SPE with a Bond Elut SCX cartridge(500mg,3mL).Pig liver and chicken samples tested with HPLC. The recovery of spiked samples was good,and confirming with liquid chromatography-electrospray mass spectrometry.3)A method with high performance liquid chromatographyto-electrospray mass spectrometry to detect residues of six macrolide antibiotics in meat food was developed.Roxithromycin as internal standard,ESI ion source,positive ion scan mode,and M+H were chosen for the monitoring of plasma,a mobile phase of formic acid-acetonitrile gradient system.The method has higher sensitivity than liquid chromatography.The recovery of spiked chicken liver sample is 73.5%-92.3%,the relative standard deviation is lower than 8.2%, the recovery of spiked cattle sample is 78.5%-94.2%,the relative standard deviation is lower than 9.1%.Batches of chicken liver sample,chicken samples and cattle samples on sales of market were determined.The quantification limit is 0.005-0.030mg/kg,which can provide technical support for inspection and monitoring of MALs residue.According to the research,HPLC,LC-ESI-MS methods were established to separate and detect MALs,and the sample treatment were optimized.It is also providing a strong basis for the detection of MALs. The detectability and quantification limit of the method acquire the requirement of the actual residual monitoring.Applied with the analytical method erected,the residues of MALs in the marketing samples are detected successfully and satisfying results are obtained.